CN1751675B - Method for preparing compound injection of traditional Chinese medicine - Google Patents
Method for preparing compound injection of traditional Chinese medicine Download PDFInfo
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- CN1751675B CN1751675B CN 200410072057 CN200410072057A CN1751675B CN 1751675 B CN1751675 B CN 1751675B CN 200410072057 CN200410072057 CN 200410072057 CN 200410072057 A CN200410072057 A CN 200410072057A CN 1751675 B CN1751675 B CN 1751675B
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Landscapes
- Medicines Containing Plant Substances (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
A process for preparing Chinese-medicinal compound injection is disclosed, which includes such steps as extracting liquid medicine, clarifying and ultrafiltering, then preparing an injection, wherein the pressure of the ultrafiltering is 0.1 to 0.5 Mpa at the liquid inlet mouth, and the pressure of the ultrafiltering at the liquid outlet mouth is 0.25 to 0.5 Mpa lower than that at the liquid inlet mouth; the temperature of the feed liquid is 15 DEG to 50 DEG, and the pH of the feed liquid is 5 to 9; ultrafiltering 1-2 times while the feed liquid stoste is concentrated between 1/15 and 1/5, filling water or rare alcoholic solution; and adopting periodicity pressure oscillation and periodicity flowed fluctuation alone or in combination in the process of the ultrafiltering; intermittently filling inertial gas in order to improve ultrafiltering efficiency. The process of the present invention has the characterized of great removement of impurity and retainment of active ingredients, and strong operability, as well as solves the problem of poor operability of industrialization production ultrafiltration porcess.
Description
Technical field
The present invention relates to a kind of method for preparing of Chinese medicine preparation, particularly the method for preparing of Chinese medicine compound injection.
Background technology
Chinese medicine generally is the injection of processing after the effective site in extracting single medicinal material, is mixed with injection again after perhaps the single medicinal material in the Chinese medicine compound being extracted effective site separately.This is the complicated component because of Chinese medicine compound, and the extraction of single medicinal material is comparatively simple.But; According to traditional Chinese medical theory, what herbal mixture was particular about is compatibility, and the effect of compatibility not only is embodied in each interaction between component after being absorbed by the body in body tissue; And be embodied in the composition that the composition between different Chinese medicines occurs change in frying in shallow oil altogether like polymerization, decomposition, hydrolysis etc.; Even produce new active component, therefore, extract respectively and may cause the different of drug effect with the united extraction herbal mixture.See that from technology the medicine of respectively distinguishing the flavor of that united extraction generally also extracts more respectively in the herbal mixture is simply many.In addition, Chinese medicine must carry out strictness control to impurity, must just can process injection through further refining after single or herbal mixture extract, and process for purification adopts resin method such as macroporous adsorbent resin etc. at present mostly.Though macroporous adsorbent resin is a kind of effective process for purification refine active constituent-enriched, that remove impurity, the toxicity problem of its porogen and degradation product has hindered its application.On November 28th, 2000; National drug is evaluated central tissue and has been held " symposium of macroporous adsorbent resin separating and purifying technology ", and meeting points out that Chinese medicine employing purification by macroporous resin should be prudent; Competent foundation need be provided, guarantee safety and effectiveness through the resin purification medicine; The injection purification is used macroporous resin, should select organic residue amount the lowest in the similar resin for use, or adopts injection resin dedicated.It is thus clear that; If in the technology of Chinese medicine, use macroporous adsorbent resin; Then must formulate resin separately and use preceding processing method and detection method porogen, degradation product; Formulate the quality control standard of benzene, toluene etc., just might pass through the new drug reviewing of State Food and Drug Administration.Like this, not only the control difficulty of the source of resin, quality, regeneration and degree of stability strengthens, and cost also significantly rises.Avoid the use of macroporous adsorbent resin and become one of difficult point among the Chinese medicine preparation technology.
Hyperfiltration technique is a kind of membrane separation technique, and its ultimate principle is to utilize fenestra selectivity sieve performance, with separation, purification and condensed matter.Because hyperfiltration process is physical method, having not must repeated heating, does not have " phase " to change, the probability of destroying effective ingredient than other universal method for few, characteristics such as technological process is short, thus its be applied to extract in the research of pharmaceutically active ingredient become increasingly active.Though hyperfiltration technique is applied to the production of Chinese medicine preparation its unique advantage is arranged; But its degree of applying is still very limited; Mainly be a lot of because influence the factor of ultrafiltration effect, the for example selection of membrane module, the cleaning method after the definite and ultrafilter of technological parameter uses etc.; At present relevant hyperfiltration technique be applied to Chinese medicine preparation particularly the report of injection aspect derive from laboratory research mostly, the feasibility of suitability for industrialized production and concrete process condition thereof are not proposed.Seek the ultrafiltration technology operating condition that is fit to the Chinese medicine suitability for industrialized production and become the target that people make great efforts.
Summary of the invention
The method for preparing that the purpose of this invention is to provide a kind of Chinese medicine compound injection, this method can be dispeled impurity largely and keep effective ingredient, and be workable, solved the difficult problem of suitability for industrialized production ultrafiltration technology condition poor operability.
The method for preparing of Chinese medicine compound injection of the present invention realizes through following technical step:
(1) the Chinese medicine medical material is processed extracting solution through extraction;
(2) predefecation is handled;
(3) ultrafiltration;
(4) ultrafiltrate concentrates, and processes injection.
In the above-mentioned technical step (1); Said Chinese medicine medical material through extracting the flavour of a drug of hyperfiltration treatment, is generally 2～15 flavor medicines in needs, is preferably 2～10 flavor medicines; The best is 2～5 flavor medicines; Both can kinds of traditional Chinese medicines medical material united extraction, also can there be some flavour of a drug to extract separately, but have two flavor Chinese medicines united extraction together at least.Said warp extracts processes extracting solution; Available water or organic solvent or both mix Chinese medicine extracted and process it and get liquid; Wherein organic solvent can be used the general conventional organic solvent of using, preferred alcohol organic solvent, and 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); Said 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, obtain supernatant, adsorption clarification 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 Combined application, 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 technical step of the present invention (3); The used ultrafilter membrane of ultrafiltration can be cellulose diacetate film (CA), three cellulose acetate membrane (CTA), cyanoethyl cellulose film (CN-CA), PS 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 ultrafilter membrane that dynamically forms, and the Modified Membrane of above-mentioned film.Be preferably cellulose diacetate film (CA), three cellulose acetate membrane (CTA), PS 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 following:
(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 in membrane channels, produce pulsating flow or non-stationary flow, 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 the method for alternately recoil is used in the ultrafiltration module parallel connection; 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 filtrating; 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, i.e. 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 technical step of the present invention (4), after ultrafiltrate concentrated, be prepared into injection by conventional method again, for example can lyophilization or spray-dired method process injectable powder, also can directly filtrating be processed aqueous injection without drying steps.
The method for preparing of Chinese medicine compound injection of the present invention has following advantage:
(1) on process, has very strong operability;
(2) this method is not used macroporous adsorbent resin, has not only avoided using the toxicity problem of macroporous adsorbent resin technology, and more superior or close with it than using macroporous adsorbent resin technology on effective ingredient enrichment and impurity-eliminating effect;
(3) can dispel the impurity in the Chinese medicine largely;
(4) can keep effective ingredient dramatically, effective.
The specific embodiment
Below in conjunction with embodiment the present invention is done further elaboration.These embodiment only are used to the purpose of giving an example, rather than limit the present invention by any way.
Embodiment one
Raw material: Radix Salviae Miltiorrhizae 300g, Cortex Moutan 150g
Adjuvant: mannitol 30g
Radix Salviae Miltiorrhizae and Cortex Moutan are ground into coarse powder, the decocte 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.Get the supernatant of medicinal liquid behind the precipitate with ethanol, it is that 50000 three cellulose acetate membrane carries out ultrafiltration that this liquid is used molecular cut off, in the ultrafiltrate of gained, adds mannitol, dissolving, and solution is processed aqueous injection.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment two
Raw material: Radix Salviae Miltiorrhizae 410g, Radix Notoginseng 80g, Borneolum Syntheticum 2.6g
Adjuvant: mannitol 25g
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.Get the supernatant of medicinal liquid behind the precipitate with ethanol, it is that 40000 PS membrane carries out ultrafiltration that this liquid is used molecular cut off, in the ultrafiltrate of gained, adds mannitol, dissolving, and the solution lyophilization adds Borneolum Syntheticum, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment three
Raw material: Radix Salviae Miltiorrhizae 350g, Rhizoma Chuanxiong 160g, Styrax 5.2g
Adjuvant: dextran 30g
Rhizoma Chuanxiong extracts volatile oil, adds 0.5% HP-aqueous solution in the Rhizoma Chuanxiong volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; Residue and Radix Salviae Miltiorrhizae that Rhizoma Chuanxiong extracts behind the volatile oil add 5 times of water gagings, 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.Filtrating merges with the Rhizoma Chuanxiong clathrate, and using molecular cut off is that 20000 sulfonated polysulfone membrane carries out ultrafiltration, in the ultrafiltrate of gained, adds dextran, dissolving, and solution spray is dry, adds Styrax, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment four
Raw material: Radix Salviae Miltiorrhizae 350g, Rhizoma Chuanxiong 160g, Borneolum Syntheticum 2.6g
Adjuvant: mannitol 25g, sodium thiosulfate 2g
Rhizoma Chuanxiong extracts volatile oil, adds 0.5% HP-aqueous solution in the Rhizoma Chuanxiong volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; 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.Filtrating merges with the Rhizoma Chuanxiong clathrate, and using molecular cut off is that 30000 the mystery sulfone film that gathers carries out ultrafiltration, in the ultrafiltrate of gained, adds mannitol and sodium thiosulfate, dissolving, and the solution lyophilization adds Borneolum Syntheticum, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
The active constituent content of Test Example 1 different process method relatively
(1) process:
Among water extraction: the embodiment four 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; Filtrating is concentrated into the extractum that relative density is 1.36 (55 ℃).
Among decoction and alcohol sedimentation technique: the embodiment three without the method for ultrafiltration, Radix Salviae Miltiorrhizae, the Rhizoma Chuanxiong that is about to coarse pulverization extracts residue behind the volatile oil to extraction pot, adds 5 times of water gagings, decocts 2 hours; Filter, filtering residue carries out the second time and extracts, and adds 4 times of water gagings, fries in shallow oil 1 hour; 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; Filtrating is concentrated into the extractum that relative density is 1.36 (55 ℃).
3. water is carried resin method: the residue behind the Radix Salviae Miltiorrhizae of the coarse pulverization of learning from else's experience, the Rhizoma Chuanxiong extraction volatile oil adds 5 times of water gagings to extraction pot, decocted 2 hours, filters, 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; Filtrating is concentrated into relative density and is about 0.9 extractum.After extractum adds the suitable quantity of water dissolving, last D
101Macroporous adsorbent resin to neutral, is abandoned water liquid with deionized water rinsing, continues to use 95% ethanol elution, collects eluent; Eluent is concentrated into the extractum that relative density is 1.36 (55 ℃).
4. water is put forward ultrafiltration: water is put forward the method for ultrafiltration among the embodiment four, 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 four) treatment angina pectoris
1 data and method
1.1 case is selected among the 100 routine angina pectoris patients, male 53 examples, and women 47 examples, 35～55 years old 35 age example, 56～70 years old 65 example, 51.3 years old mean age, the course of disease 2.5 years, wherein with hyperpietic's 39 examples, type ii diabetes 6 examples.All patients all meet name and the standard of WTO about the ischemic heart desease diagnosis, wherein stable angina pectoris 46 examples, UA 54 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 medicine of the present invention, and consumption is to add 200mg (being equivalent to contain crude drug amount 30g), intravenous drip once a day, totally 14 days in every 500ml liquid.Matched group gives FUFANG DANSHEN ZHUSHEYE, and consumption is to add 15ml (every milliliter contains crude drug amount 2g), intravenous drip once a day, totally 14 days in every 500ml liquid.
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, basic identical before resting electrocardiogram and the treatment.
2 results
2.1 treatment group and matched group curative effect are relatively seen table 2, table 3.
Table 2 Drug therapy angina pectoris symptom of the present invention curative effect and matched group are relatively
| Group | The example number | Produce effects | Take a turn for the better | Invalid | Total effective rate |
| Treatment group matched group | 5050 | 34(68) 19(38) | 11(22) 18(36) | 5(10) 13(26) | (90) (74) |
Table 3 Drug therapy angina pectoris of the present invention ECG curative effect and matched group are relatively
| Group | The example number | Produce effects | Take a turn for the better | Invalid | Total effective rate |
| Treatment group matched group | 50 50 | 13(22) 7(14) | 24(44) 20(40) | 13(34) 23(46) | (66) (54) |
Embodiment five
Raw material: Radix Salviae Miltiorrhizae 500g, Radix Notoginseng 100g, Styrax 3.5g
Adjuvant: lactose 30g
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.It is that 20000 sulfonated polyether sulfone film carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds lactose, dissolving, and the solution lyophilization adds Styrax, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment six
Raw material: Radix Salviae Miltiorrhizae 450g, Radix Paeoniae Rubra 141g, Borneolum Syntheticum 8g.
Adjuvant: sorbitol 15g
With 60% ethanol heating extraction Radix Salviae Miltiorrhizae and Radix Paeoniae Rubra 2 times, each 2 hours, merge extractive liquid, was obtained supernatant behind the high speed centrifugation.It is that 30000 polysulfonamides film carries out ultrafiltration that supernatant is used molecular cut off, in the ultrafiltrate of gained, adds sorbitol, dissolving, and the solution lyophilization adds Borneolum Syntheticum, and mixing is processed injectable powder.
The ultrafiltration mode adopts dead-end filtration, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment seven
Raw material: Radix Salviae Miltiorrhizae 200g, Radix Notoginseng 200g, Lignum Dalbergiae Odoriferae oil 1.75ml
Raw material: glucose 30g, Glycine sodium 3g
Add 0.3% HP-aqueous solution in the Lignum Dalbergiae Odoriferae oil, stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use.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.Merge supernatant and inclusion complex in solution, using molecular cut off is that 40000 polyacrylonitrile film carries out ultrafiltration, in the ultrafiltrate of gained, adds glucose and Glycine sodium, dissolving, and solution spray is dry, processes injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment eight
Raw material: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g, Flos Carthami 50g
Adjuvant: sodium chloride 23g
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 filtrating.It is that 10000 cyanoethyl cellulose film carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds sodium chloride, dissolving, and the solution lyophilization adds Borneolum Syntheticum, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment nine
Raw material: Radix Salviae Miltiorrhizae 110g, Radix Notoginseng 30g, Radix Astragali 430g, Lignum Dalbergiae Odoriferae 100g
Adjuvant: dextran 26g
Get Lignum Dalbergiae Odoriferae, add 5 times of water gagings, reflux, extract, 5 hours is collected volatile oil, adds 0.3% HP-aqueous solution in the volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use.Will be through the Radix Astragali, Radix Salviae Miltiorrhizae, the Radix Notoginseng of pulverizing, decocte with water 2 times adds 7 times of water gagings at every turn, and each 2 hours, merge decoction liquor, filter, filtrating is concentrated into 900ml, adds 95% ethanol, makes determining alcohol reach 70%, leaves standstill 24 hours, filters.It is that 20000 PS membrane carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds dextran, dissolving, and solution is processed aqueous injection.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment ten
Raw material: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g, Radix Codonopsis 100g
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 filtrating.It is that 50000 polysulfonamides film carries out ultrafiltration that filtrating is used molecular cut off, with the ultrafiltrate lyophilization of gained, adds Borneolum Syntheticum, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 11
Raw material: Rhizoma Chuanxiong 300g, Radix Puerariae 350g, Styrax 10g
Adjuvant: sorbitol 35g, disodiumedetate 3g
Rhizoma Chuanxiong extracts volatile oil, adds 0.3% HP-aqueous solution in the volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; Rhizoma Chuanxiong extracts residue and Radix Puerariae behind the volatile oil with 70% alcohol reflux 2 times, 2 hours for the first time, 1 hour second time, merge extractive liquid,, filtration.It is that 20000 polyvinylidene fluoride film carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds sorbitol and disodiumedetate, dissolving, and the solution lyophilization adds Styrax, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition is: the inlet pressure of ultrafiltration is 0.2MPa, 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 temperature is 40 ℃, when feed liquid stock solution is concentrated 1/12, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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 0.5MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Embodiment 12
Raw material: Semen Ziziphi Spinosae (stir-fry) 250g, Radix Salviae Miltiorrhizae 50g, Fructus Schisandrae Chinensis (processed with vinegar) 50g
Adjuvant: mannitol 15g
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.It is that 10000 polyimide film carries out ultrafiltration that supernatant uses molecular cut off, in the ultrafiltrate of gained, adds mannitol, dissolving, and solution spray is dry, processes injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 13
Raw material: Radix Notoginseng 100g, Flos Carthami 100g, Rhizoma Chuanxiong 200g
Adjuvant: glucose 20g
Radix Notoginseng and Rhizoma Chuanxiong power are broken into coarse powder, and decocte with water 2 hours filters, and filtrating is deposited in addition, medicinal residues and Flos Carthami decocte with water secondary, and each 1 hour, merge three times decocting liquid, carry out coarse filtration with tiffany.It is that 70000 cellulose membrane carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds glucose, dissolving, and solution is processed aqueous injection.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 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 1/8, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 14
Raw material: Fructus Trichosanthis 360g, Rhizoma Cyperi 180g, Herba Epimedii 180g
Adjuvant: dextran 25g
Fructus Trichosanthis, Rhizoma Cyperi, Herba Epimedii are ground into coarse powder, and the decocte with water secondary 2 hours for the first time, 1.5 hours for the second time, filters merging filtrate.It is that 8000 phenolphthalein side group polyarylsulfone (PAS) film carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds dextran, dissolving, and solution spray is dry, processes injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 0.1MPa.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 7.0.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.When the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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 12, and cleaning pressure is 0.05MPa.After cleaning with chemical, the flushing of reuse water is near neutral.
Embodiment 15
Raw material: Radix Salviae Miltiorrhizae 500g, Rhizoma Chuanxiong 500g, Radix Puerariae 500g
Adjuvant: gelatin hydrolysate 35g
Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, powder of Radix Puerariae are broken into coarse powder, the decocte with water secondary, and 1.5 hours for the first time, 1 hour collecting decoction for the second time, extracting solution filters with gauze.It is that methyl methacrylate-acrylonitrile copolymer film of 9000 carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds gelatin hydrolysate, dissolving, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 16
Raw material: Radix Ophiopogonis 300g, Radix Paeoniae Rubra 300g, Radix Glehniae 300g, Radix Notoginseng 200g.
Adjuvant: lactose 30g
Radix Ophiopogonis, Radix Glehniae, Radix Notoginseng decocte with water three times, first and second time each 2 hours, 1 hour for the third time, collecting decoction filtered, and filtrating is concentrated into an amount of, adds ethanol and makes that to contain the alcohol amount be 65%, leaves standstill, and filters filtrate for later use; Radix Paeoniae Rubra decocte with water three times, first and second time each 2 hours, 1 hour for the third time, collecting decoction; Filter, filtrating is concentrated into an amount of, regulates pH value to 8 with 1% sodium hydroxide solution, and it is an amount of to add 2% gelatin solution; Make deposition fully, filter, filtrating is concentrated into an amount of, adds ethanol and makes that to contain the alcohol amount be 65%; Leave standstill, filter filtrate for later use.Merge above-mentioned filtrating, it is that polyacrylonitrile-cellulose diacetate film of 20000 carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds lactose, dissolving, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 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 5.Backwashing pressure is 1.5MPa, and backwashing period is that 0.5 hour, backwashing time are 1 minute.When the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 17
Raw material: Radix Astragali 350g, Ramulus Cinnamomi 150g, Radix Salviae Miltiorrhizae 250g, Radix Puerariae 250g
Adjuvant: mannitol 35g, sodium thiosulfate 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 decocte with water three times, each 2 hours, collecting decoction; Filter, filtrating merges with above-mentioned aqueous solution, filters; It is that 10000 cellulose diacetate film carries out ultrafiltration that filtrating is used molecular cut off; In the ultrafiltrate of gained, add mannitol and sodium thiosulfate, dissolving, solution is processed infusion solution.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 18
Raw material: Fructus Crataegi 270g, Radix Salviae Miltiorrhizae 200g, Radix Puerariae 300g, Radix Notoginseng 90g, Radix Aucklandiae 50g
Raw material: mannitol 30g
Fructus Crataegi, Radix Salviae Miltiorrhizae, Radix Puerariae, Radix Notoginseng, Radix Aucklandiae powder are broken into coarse powder, decocte 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; It is that 20000 cellulose diacetate film carries out ultrafiltration that supernatant uses molecular cut off, in the ultrafiltrate of gained, adds mannitol, dissolving, and solution lyophilization or spray drying are processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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 processed granule 1000g, promptly gets in the batch (-type) fluid bed.
Embodiment 19
Raw material: Radix Salviae Miltiorrhizae 300g, Radix Angelicae Sinensis 150g, Fructus Aurantii 150g, Radix Notoginseng 200g, Rhizoma Zingiberis Recens 300g
Adjuvant: glucose 25g
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.It is that 70000 three cellulose acetate membrane carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds glucose, dissolving, and solution spray is dry, processes injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 20
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: glucose 23g, cysteine hydrochloride 5g
Radix Paeoniae Rubra, Radix Salviae Miltiorrhizae decocte with water twice, 2 hours for the first time, 1 hour for the second time, decocting liquid filtered, and merging filtrate is subsequent use.Cataclasm Lignum Dalbergiae Odoriferae and Rhizoma Chuanxiong extract volatile oil, add 0.3% HP-aqueous solution in the volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; Its residue decocte with water 2 hours, decocting liquid filters, and is subsequent use.Flos Carthami adds water temperature and soaks twice, and 2 hours for the first time, 1 hour for the second time, merge immersion, filter, subsequent use; Above-mentioned each filtrating is merged, and using molecular cut off is that 20000 sulfonated polysulfone membrane carries out ultrafiltration, in the ultrafiltrate of gained, adds glucose and cysteine hydrochloride, dissolving, and solution is processed aqueous injection.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 21
Raw material: Radix Salviae Miltiorrhizae 200g, Radix Paeoniae Alba 2000g, Radix Et Caulis Acanthopanacis Senticosi 1000g, Radix Curcumae 300g, Fructus Crataegi 2000g
Adjuvant: mannitol 60g
Fructus Crataegi is extracted secondary with alcohol heating reflux, and each 2 hours, merge extractive liquid,, subsequent use; Radix Salviae Miltiorrhizae, the Radix Paeoniae Alba, Radix Et Caulis Acanthopanacis Senticosi, Radix Curcumae decocte with water secondary, each 2 hours, collecting decoction filtered, and filtrating is concentrated into relative density to 1.20, and add ethanol and make pure content reach 70%, hold over night, the leaching supernatant merges with above-mentioned hawthorn extract, filters.It is that 10000 polysulfonamides film carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds mannitol, dissolving, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 22
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: sorbitol 25g
Rhizoma Chuanxiong extracts volatile oil, and the aqueous solution after distillation device is in addition collected; Add 0.3% HP-aqueous solution in the volatile oil, stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; Its medicinal residues and Flos Carthami, Radix Salviae Miltiorrhizae, Rhizoma Alismatis, Radix Notoginseng, the decocte with water secondary, 3 hours for the first time, 2 hours collecting decoctions filtered for the second time.Merge above-mentioned solution, dissolve in Radix Et Caulis Acanthopanacis Senticosi extractum powder, it is that 30000 poly (ether sulfone) film carries out ultrafiltration that solution uses molecular cut off, in the ultrafiltrate of gained, adds sorbitol, dissolving, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 23
Raw material: Radix Salviae Miltiorrhizae 250g, Radix Notoginseng 200g, Borneolum Syntheticum 5g, TENGHEHUAN 1000g, Radix Aucklandiae 200g, Styrax 5g
Adjuvant: dextran 35g
Radix Salviae Miltiorrhizae, Radix Notoginseng, TENGHEHUAN, Radix Aucklandiae powder are broken into coarse powder, and the decocte with water secondary each 2 hours, filters merging filtrate.It is that 50000 polyvinylidene fluoride film carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds dextran, dissolving, and the solution lyophilization adds Borneolum Syntheticum and Styrax, and mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 24
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: mannitol 40g
More than seven flavors, decocte with water three times, each 1 hour, collecting decoction filtered.Filtrating 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, in the ultrafiltrate of gained, adds mannitol, dissolving, and solution spray is dry, processes injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 25
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 40g
More than seven flavors, decocte with water three times, each 1 hour, collecting decoction adds the flocculate with chitosan clarifier, leaves standstill 24 hours, and was centrifugal, gets supernatant.It is that 30000 sulfonated polyether sulfone film carries out ultrafiltration that supernatant uses molecular cut off, in the ultrafiltrate of gained, adds lactose, dissolving, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 26
Raw material: Radix Codonopsis 150g, Radix Astragali 150g, Flos Carthami 100g, Radix Angelicae Sinensis 100g, Rhizoma Chuanxiong 100g, triangular 100g, Pollen Typhae 100g
Adjuvant: sodium chloride 30g, sodium thiosulfate 3g
Get Pollen Typhae and wrap with cloth bag, same Radix Codonopsis, the Radix Astragali, return, Rhizoma Chuanxiong, Rhizoma Sparganii decocte with water secondary, 2 hours for the first time, decoct 1.5 hours for the second time after, add Flos Carthami again and decocted 30 minutes, merging filtrate filters with gauze.It is that 60000 cellulose diacetate film carries out ultrafiltration that filtrating is used molecular cut off, in the ultrafiltrate of gained, adds sodium chloride and sodium thiosulfate, dissolving, and solution is processed infusion solution.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 0.1MPa.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 1/15, 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 27
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: mannitol 40g
Rhizoma Chuanxiong, Flos Carthami, Lignum Dalbergiae Odoriferae extract volatile oil respectively, add 0.3% HP-aqueous solution in the volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; Its residue and Radix Salviae Miltiorrhizae, Flos Sophorae, Radix Notoginseng, Radix Paeoniae Rubra, decocte with water three times, 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, collecting decoction filtered.Filtrating merges with inclusion complex in solution, and using molecular cut off is that 50000 three cellulose acetate membrane carries out ultrafiltration, in the ultrafiltrate of gained, adds mannitol, dissolves, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 28
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: mannitol 45g
More than seven flavors, decocte with water three times, 3 hours for the first time, second and third time each 1 hour, collecting decoction filters, filtrating 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.It is that 30000 polyvinylidene fluoride film carries out ultrafiltration that supernatant uses molecular cut off, in the ultrafiltrate of gained, adds mannitol, dissolving, and solution spray is dry, processes injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 29
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: dextran 35g, glycine 3g
More than eight flavors, add 70% ethanol ultrasonic extraction 2 times, each 1 hour, merge extractive liquid, filtered.Filtrating is carried out two-stage ultrafiltering, and the first order is that molecular cut off is 70000 PS membrane, and the second level is that molecular cut off is 10000 cellulose diacetate film, in the ultrafiltrate of gained, adds dextran and glycine, dissolving, and solution is processed infusion solution.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 30
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, Catergen 0g
Adjuvant: mannitol 45g
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 decocte with water three times, each 1.5 hours, collecting decoction filtered; The ratio that filtrating 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; Placed 48 hours, and filtered, filtrating merges with above-mentioned Radix Puerariae extracting solution.Filtrating is dissolved in aluminum clofibrate and vitamin, and the reuse molecular cut off is that 20000 PS membrane carries out ultrafiltration, in the ultrafiltrate of gained, adds mannitol, dissolving, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
The embodiment hentriaconta-
Raw material: Rhizoma Chuanxiong 100g, Rhizoma Ligustici 60g, Herba Asari 30g, Radix Angelicae Dahuricae 100g, Radix Salviae Miltiorrhizae 100g, Radix Puerariae 100g, Ramulus Uncariae Cum Uncis 100g
Adjuvant: gelatin hydrolysate 25g
Rhizoma Chuanxiong, Herba Asari extract volatile oil, add 0.3% HP-aqueous solution in the volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; Its residue and Rhizoma Ligustici, the Radix Angelicae Dahuricae, Radix Salviae Miltiorrhizae, Radix Puerariae, Ramulus Uncariae Cum Uncis decocte with water three times, 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, collecting decoction filtered.Filtrating merges with inclusion complex in solution, and using molecular cut off is that 20000 cellulose diacetate film carries out ultrafiltration, in the ultrafiltrate of gained, adds gelatin hydrolysate, dissolves, and injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 32
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: mannitol 45g, sodium dihydrogen phosphate 3g
More than ten flavor decocte with water secondaries, filter, merging filtrate is concentrated in right amount, adds ethanol and makes that to contain the alcohol amount be 70%, leaves standstill 24 hours, filters.Filtrating is carried out two-stage ultrafiltering; First order use molecular cut off is 70000 cellulose diacetate film, and second level use molecular cut off is 10000 cellulose diacetate film, in the ultrafiltrate of gained, adds mannitol and sodium dihydrogen phosphate; Dissolving, solution is processed aqueous injection.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 33
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, cortex trichosanthis 80g, Radix Polygalae (Radix Glycyrrhizae system) 60g, Lignum Dalbergiae Odoriferae 60g, Rhizoma Acori Graminei 60g, Radix Glycyrrhizae (processed with honey) 60g
Adjuvant: glucose 35g, sodium chloride 35g
Flos Carthami is with 75 ℃ of warm water immersion secondaries, and each 2 hours, merge immersion, immersion is subsequent use; Lignum Dalbergiae Odoriferae and Rhizoma Chuanxiong extract volatile oil, add 0.3% HP-aqueous solution in the volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; 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 decocte with water secondary, each 3 hours, merge with above-mentioned Flos Carthami immersion, filter.Merge above-mentioned solution, carry out two-stage ultrafiltering, first order use molecular cut off is 80000 polyvinylidene fluoride film; Second level use molecular cut off is 10000 cellulose diacetate film; In the ultrafiltrate of gained, add glucose and sodium chloride, dissolving, solution is processed infusion solution.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 34
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: dextran 30g, sodium pyrosulfite 5g
Get Radix Puerariae, Radix Salviae Miltiorrhizae, heating and refluxing extraction secondary in 70% ethanol each 1 hour, merges ethanol extract; With the medicinal residues behind the ethanol extraction and the Radix Astragali etc. ten decocte with water secondary simply, 2 hours for the first time, 1.5 hours for the second time, collecting decoction; Filter, filtrating 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.Filtrating is carried out two-stage ultrafiltering, and first order use molecular cut off is 70000 sulfonated polysulfone membrane, and second level use molecular cut off is 10000 cellulose diacetate film; In the ultrafiltrate of gained, add dextran and sodium pyrosulfite; Dissolving, injectable powder is processed in the solution lyophilization.
The ultrafiltration mode adopts cross flow filter, and its process 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.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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 35
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: mannitol 45g, methionine 5g, vitamin C 4g
Ten five tastes such as above Radix Salviae Miltiorrhizae, decocte with water three times, 3 hours for the first time, 2 hours for the second time, 1 hour for the third time, collecting decoction filtered.Filtrating is carried out three grades of ultrafiltration; First order use molecular cut off is 80000 cellulose diacetate film; Second level use molecular cut off is 20000 cellulose diacetate film, and third level use molecular cut off is 6000 sulfonated polysulfone membrane, in the ultrafiltrate of gained, adds mannitol, methionine and vitamin C; Dissolving, solution is processed infusion solution.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Embodiment 36
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: mannitol 45g, Glycine sodium 10g
Radix Salviae Miltiorrhizae, Radix Paeoniae Rubra, Rhizoma Acori Graminei, Radix Curcumae, Radix Ginseng, Radix Notoginseng, Caulis Spatholobi, Radix Ophiopogonis, Semen Persicae decocte with water secondary, 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 be with 70% alcohol reflux secondary, and 3 hours for the first time, 2 hours for the second time, merging filtrate, filtrate for later use.The Radix Aucklandiae, Lignum Dalbergiae Odoriferae extract volatile oil, add 0.3% HP-aqueous solution in the volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use.Above each filtrating of merging, filtrating is carried out three grades of ultrafiltration, and first order use molecular cut off is 70000 cellulose diacetate film; Second level use molecular cut off is 20000 cellulose diacetate film, and third level use molecular cut off is 8000 polysulfonamides film, in the ultrafiltrate of gained, adds mannitol and Glycine sodium; Dissolving, the solution lyophilization adds Borneolum Syntheticum; Mixing is processed injectable powder.
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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 the method for alternately recoil was used in ultrafiltration module parallel connection, wherein a cover or a few cover carried out normal ultrafiltration and distribute the recoil ultrafilter membrane of another set of or several grip assemblies of part filtrating, 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.
Claims (1)
1. the method for preparing of a compound Chinese medicinal preparation is characterized in that:
Raw material: Radix Salviae Miltiorrhizae 350g, Rhizoma Chuanxiong 160g, Borneolum Syntheticum 2.6g
Adjuvant: mannitol 25g, sodium thiosulfate 2g
Rhizoma Chuanxiong extracts volatile oil, adds 0.5% HP-aqueous solution in the Rhizoma Chuanxiong volatile oil, and stirring and dissolving filters, and processes inclusion complex in solution, and is subsequent use; 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; Filtrating merges with the Rhizoma Chuanxiong clathrate, and using molecular cut off is that 30000 the mystery sulfone film that gathers carries out ultrafiltration, in the ultrafiltrate of gained, adds mannitol and sodium thiosulfate, dissolving, and the solution lyophilization adds Borneolum Syntheticum, and mixing is processed injectable powder;
The ultrafiltration mode adopts cross flow filter, and its process condition 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 in membrane channels, produce pulsating flow or non-stationary flow; 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.
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| CN 200410072057 CN1751675B (en) | 2004-09-22 | 2004-09-22 | Method for preparing compound injection of traditional Chinese medicine |
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| CN 200410072057 CN1751675B (en) | 2004-09-22 | 2004-09-22 | Method for preparing compound injection of traditional Chinese medicine |
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| CN1751675B true CN1751675B (en) | 2012-04-18 |
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