CN102302548B - Preparation method for compound salvia tablets - Google Patents
Preparation method for compound salvia tablets Download PDFInfo
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- CN102302548B CN102302548B CN 201110247792 CN201110247792A CN102302548B CN 102302548 B CN102302548 B CN 102302548B CN 201110247792 CN201110247792 CN 201110247792 CN 201110247792 A CN201110247792 A CN 201110247792A CN 102302548 B CN102302548 B CN 102302548B
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Abstract
The invention discloses a preparation method for compound salvia tablets. In the preparation method, active ingredients of salvia are extracted by using the diaphragm filter-press circular extraction separation integrated technology, so a process can be simplified, the production period is shortened substantially, the production energy consumption is reduced, environmental protection and the utilization of waste residues are facilitated, the used amount of ethanol serving as an extraction solvent is reduced, and the recovery rate of the active ingredients is increased greatly.
Description
Technical field
The invention belongs to pharmaceutical field, relate to a kind of preparation method of Chinese medicine preparation.
Background technology
Record of Chinese Pharmacopoeia version in 2010: FUFANG DANSHEN PIAN has blood circulation promoting and blood stasis dispelling, and the effect of regulating QI to relieve pain is for the thoracic obstruction of caused by energy stagnation and blood stasis, uncomfortable in chest, pareordia twinge that disease is seen; Angina pectoris is seen above-mentioned patient.Its prescription is Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g.Its preparation method is that Radix Salviae Miltiorrhizae is added 95% alcohol heating reflux 1.5 hours, and extracting solution filters, and filtrate recycling ethanol also is concentrated into an amount of, standby; Medicinal residues add 50% alcohol heating reflux 1.5 hours, and extracting solution filters, and filtrate recycling ethanol also is concentrated into an amount of, standby; Medicinal residues decoct with water 2 hours, and decocting liquid filters, and filtrate is concentrated in right amount; Radix Notoginseng powder is broken into fine powder, makes granule, drying with above-mentioned concentrated solution and an amount of adjuvant; The Borneolum Syntheticum porphyrize with above-mentioned granule mixing, is pressed into 333, and the bag film-coat perhaps is pressed into 1000, sugar coating or film-coat, namely.Adopt circumfluence method and decocting method to extract the effective ingredient of Radix Salviae Miltiorrhizae in the said method respectively, thereby exist the losses of degrading in process of production such as technology is loaded down with trivial details, extraction time long, extraction temperature height, energy consumption height, thermal sensitivity composition Tanshinone I Ia seriously to make product not meet problems such as quality regulation.
Summary of the invention
In view of this; the object of the present invention is to provide a kind of method of utilizing membrane filter pressing circulation extraction isolation integral technology to prepare FUFANG DANSHEN PIAN; not only can simplify technological process; significantly shorten the production cycle; reduce energy consumption; be beneficial to environmental conservation and waste residue utilization, and can reduce the consumption that extracts etoh solvent, and greatly improve the response rate of effective ingredient.
For achieving the above object, the invention provides following technical scheme:
The preparation method of FUFANG DANSHEN PIAN, made by following raw materials by weight proportions: 8 parts of 450 parts of Radix Salviae Miltiorrhizaes, 141 parts of Radix Notoginseng and Borneolum Syntheticums, preparation method may further comprise the steps:
A. the extraction of Radix Salviae Miltiorrhizae
A1. the Radix Salviae Miltiorrhizae powder with recipe quantity is broken into coarse powder, and is standby;
A2. in material-compound tank, add 75-90% ethanol; Three-way valve is switched to the material-compound tank position, 75-90% ethanol in the material-compound tank is pumped into diaphragm filter press, when passing back into material-compound tank to pressing filtering liquid, under stirring condition, in material-compound tank, add step a1 gained medicated powder, finish, carry out the membrane filter pressing circulation first time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, again three-way valve is switched to the material-compound tank position, in material-compound tank, add 50% ethanol, carry out the membrane filter pressing circulation second time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. in material-compound tank, add water, be heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, the water in the material-compound tank is pumped into diaphragm filter press, under 50-90 ℃ condition, carry out the membrane filter pressing circulation and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, be designated as extracting solution B;
B. preparation
B1. the extracting solution A with step a2 gained reclaims ethanol and concentrated, gets concentrated solution A;
B2. the extracting solution B with step a3 gained concentrates, and gets concentrated solution B;
B3. the Radix Notoginseng powder with recipe quantity is broken into fine powder, makes granule, drying with the concentrated solution A of step b1 gained, concentrated solution B and the adjuvant of step b2 gained; With the Borneolum Syntheticum porphyrize of recipe quantity, with above-mentioned dried granule mixing, tabletting, sugar coating or film-coat namely get FUFANG DANSHEN PIAN.
Preferably, described step a2 adds earlier to be equivalent to Radix Salviae Miltiorrhizae weight 6-9 75% ethanol doubly, carries out membrane filter pressing circulation extraction first time, and extraction time is 30-50 minute; Add and be equivalent to Radix Salviae Miltiorrhizae weight 3-5 50% ethanol doubly, carry out the membrane filter pressing circulation second time and extract, extraction time is 10-30 minute;
Described step a3 adds earlier to be equivalent to Radix Salviae Miltiorrhizae weight 4-6 water doubly, carries out the membrane filter pressing circulation and extract under 55-65 ℃ condition, and extraction time is 30-50 minute.
Preferred, described step a2 adds 75% ethanol that is equivalent to 7.5 times of Radix Salviae Miltiorrhizae weight earlier, carries out the membrane filter pressing circulation first time and extracts, and extraction time is 40 minutes; Add 50% ethanol that is equivalent to 4 times of Radix Salviae Miltiorrhizae weight again, carry out the membrane filter pressing circulation second time and extract, extraction time is 20 minutes;
Described step a3 adds the water that is equivalent to 5 times of Radix Salviae Miltiorrhizae weight earlier, carries out the membrane filter pressing circulation and extract under 65 ℃ condition, and extraction time is 35 minutes.
Preferably, described step b1 is with extracting solution A ultrafiltration membrance filter, and permeate carries out nanofiltration dehydration, dealcoholysis again, merges the concentrated solution of ultrafiltration and nanofiltration gained, concentrated solution A, the permeate of nanofiltration is measured behind the ethanol content preparation liquid as next group tanshinol extraction solvent;
Described step b2 is with extracting solution B ultrafiltration membrance filter, and permeate carries out the nanofiltration dehydration again, merges the concentrated solution of ultrafiltration and nanofiltration gained, gets concentrated solution B.
The aperture of ultrafilter membrane can be decided according to the grading curve of feed liquid, is to the maximum suitable with membrane aperture less than particle diameter and the flux of smallest particles.In the present invention, the preferred aperture of ultrafiltration is the ceramic membrane of 50-200nm, and more preferably the aperture is the hollow fiber ceramic membrane of 100-200nm.The preferred molecular cut off of nanofiltration is the daltonian NF membrane of 100-300, and more preferably molecular cut off is the daltonian NF90-8040 type of 100-150 NF membrane, and this NF membrane not only molecular cut off is little, and the flux height.
Preferably, also comprise step a2 ＇ between described step a2 and the a3: three-way valve is switched to the material-compound tank position, in material-compound tank, add water, carry out the membrane filter pressing circulation and wash thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, measure ethanol content, as the preparation liquid of next group tanshinol extraction solvent.
Preferred, described step a2 ＇ adds to be equivalent to Radix Salviae Miltiorrhizae weight 2-4 water doubly, and the membrane filter pressing circulation was washed 3-7 minute thoroughly.
The isolation integral technology is extracted in membrane filter pressing circulation of the present invention, be that the discharging opening of material-compound tank is communicated with the charging aperture of diaphragm filter press by pump (as membrane pump etc.), the liquid outlet of diaphragm filter press is communicated with the import of charging aperture and the filtrate tank of material-compound tank respectively with three-way valve.When three-way valve switches to the material-compound tank position, the liquid outlet of diaphragm filter press is communicated with the charging aperture of material-compound tank, constitute membrane filter pressing circulation extraction system, slip in the material-compound tank is pumped to diaphragm filter press to carry out the pressing filtering liquid that membrane filter pressing comes out from diaphragm filter press and passes back into (medicated powder then is deposited on the filter cloth surface of each filter pressing chamber of diaphragm filter press equably) the material-compound tank, be re-used as and extract solvent and be pumped to diaphragm filter press and carry out membrane filter pressing and constantly circulate, thereby the membrane filter pressing circulation that realizes medical material is extracted; When three-way valve switches to the filtrate tank position, the liquid outlet of diaphragm filter press is communicated with the import of filtrate tank, constitute the membrane filter pressing solid-liquid separation system, after the membrane filter pressing circulation extraction of medical material finishes, to send into the filtrate tank storage from pressing filtering liquid and pressed liquor that diaphragm filter press comes out, thereby herbal extract is well separated with medicinal residues.
About extracting the problem of material, usually pulverizing medicinal materials is become coarse powder as extracting material, the soft medical material (as Radix Rehmanniae Preparata, Fructus Jujubae etc.) that difficulty is ground into coarse powder can add the water that 2-4 doubly measures and be ground into slip as extracting material with feed grinder or tissue mashing machine.
About the problem of charging sequence, when the medical material fibre-bearing more after a little while, can be in material-compound tank directly add medicated powder and extract solvent, under stirring condition, carry out the membrane filter pressing circulation and extract; When the medical material fibre rich, then should adopt the outer circulation method of feeding in raw material, to stop that medicated powder stops up in material-compound tank discharging opening and feeding pipe and phenomenon that the stock circulation is obstructed.The reinforced method of so-called outer circulation is will extract required whole solvents earlier first to add in the material-compound tank, three-way valve is switched to the material-compound tank position, solvent is pumped into diaphragm filter press, (can observe from the manhole of material-compound tank) when passing back into material-compound tank when observing pressing filtering liquid (this moment is actual to be solvent), under stirring condition, progressively drop into medicated powder again, the gained feed liquid is pumped to diaphragm filter press thereupon carries out the membrane filter pressing pressing filtering liquid and passes back in the material-compound tank and circulate, and medicated powder then is deposited on the filter cloth surface of each filter pressing chamber of diaphragm filter press equably.
About extracting the problem of temperature, when being solvent with water, extracting temperature can control at 50-90 ℃, according to polarized light microscopy method measurement result and in conjunction with bibliographical information, starch gelatinization temperature in the plant tissue mostly is 70-71 ℃, for fear of occurring because starch gelatinization blocks cell inclusion (mostly being effective ingredient) stripping or stops up phenomenons such as filter cloth, the medical material of rich in starch is carried out water when carrying, extract temperature and should control below 70 ℃, preferred 55-65 ℃.And when adopting organic solvent extraction, the boiling point height of looking organic solvent can not heat (namely at room temperature extracting) or suitably heating.
About the problem of extraction time and extraction time, can require according to the response rate of index components and economy requirement suitable adjustment extraction time and extraction time.For the extraction of general medicinal material coarse powder, but selective extraction 2 times extracted 30-40 minute for the 1st time, extracted 10-20 minute for the 2nd time; Higher for price of medicinal material, require the higher kind of the index components response rate, extraction time can suitably increase, as extracts 4 times, extracts the 2-4 time extraction 10-20 minute 40-60 minute the 1st time; Also last 1 time extracting solution can be carried out recycled as the solvent of extraction first of next group material.When serving as when extracting solvent with alcohol-water mixed solution, carry out membrane filter pressing and wash and squeeze medicinal residues thoroughly in the extraction back available water that finishes, after gained pressing filtering liquid and pressed liquor are measured pure content, can be used as the next group material and extract preparing solvent liquid and carry out recycled.Carry out membrane filter pressing when washing thoroughly at water, also can close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, water is fully soaked overflow the top filtering layer, to strengthen washing effect.
Need to extract earlier volatile oil about part medical material in the compound preparation prescription, medicinal residues merge the problem of carrying out decocting with other medical material again, reach a few hours owing to extract the process of volatile oil with the water azeotropic, during the water soluble ingredient of medical material fully is soluble in the aqueous phase in the process of extracting volatile oil, so generally do not need medicinal residues and the merging of other medical material are carried out decocting, and save follow-up concentrated energy consumption simultaneously for the response rate that guarantees effective ingredient, can be after extracting volatile oil, the water of doubly measuring with 2-4 is heated to the 60-90 ℃ of saturating wash slag of membrane filter pressing, wash 1-2 time thoroughly, aqueous solution after the saturating washing liquid of gained and the distillation merges, as the extraction solvent of water first of other medical material.
About the problem of diaphragm filter press, filter cloth should be selected polypropylene multifilament filter cloth for use, and its Air permenbility selection principle is: less (as 3-10L/m with the appropriate to the occasion Air permenbility of selecting for use of organic solvent extraction
2.s) filter cloth is big (as 50-1200L/m with the appropriate to the occasion Air permenbility of selecting for use of water extraction
2.s) filter cloth.Membrane filter plate should select polypropylene etc. to meet the plastic material of medicinal requirements.The feed liquid pipeline should be selected the plastic conduit of 304 above rustless steels or non-PVC for use.
In the present invention, percentage ratio means the ratio of weight with " % " symbolic representation; But the percentage ratio of solution except as otherwise herein provided, means and contains the some grams of solute among the solution 100ml; The percentage ratio of ethanol means percent by volume, contains the some milliliters of ethanol among the ie in solution 100ml.
Beneficial effect of the present invention is: (1) has improved the response rate of effective ingredient: the present invention adopts the membrane filter pressing circulating extraction method to substitute the effective ingredient of circumfluence method and decocting method extraction Radix Salviae Miltiorrhizae, this method system adopts the pressure-driven of 0.5-0.6Mpa, circulation is extracted and is piled up in hundreds of the powder beds on the eluting face, effect with pressurized column chromatography or pressurization percolation, extraction efficiency significantly improves, the extraction temperature reduces, the loss of thermal sensitivity composition reduces, the response rate of index components significantly improves, for example, the content of the index components Tanshinone I Ia that thermal sensitivity is high reaches the 0.41mg/ sheet, what be higher than drug standard regulation far away is not less than the 0.20mg/ sheet, and the content of Tanshinone I Ia only is the 0.17mg/ sheet in the product that existing method makes; And the filter cloth aperture of adopting because of diaphragm filter press is far below being used for the filter screen aperture that medicinal residues separate with decocting liquid at present, and gained extracting solution clarity is good, and naked eyes visible particle thing can not enter in the finished product, has also correspondingly improved the content of active ingredient in the finished product.(2) reduced the consumption that extracts etoh solvent: the inventive method can substitute 95% ethanol, the 50% ethanol extracted twice Radix Salviae Miltiorrhizae of existing method with 75% ethanol, 50% ethanol extracted twice, and the ethanol consumption reduces, but the content of index components increases on the contrary.(3) simplified technological process, shortened the production cycle: the present invention replaces the lengthy and tedious technology that existing 95% ethanol, twice reflux, extract, of 50% ethanol and medicinal residues decocting extract with 75% ethanol, the continuous membrane filter pressing circulation extracting process of 50% second alcohol and water, not only simplified technological process, realized the extraction isolation integral, and extraction time foreshortened to about 1 hour by 5 hours, extraction time shortens more than 80%.(4) energy savings: with 1m
3Water is heated to 55-65 ℃ from 20 ℃ and needs raw coal 18.4-21.7kg, needs raw coal 37.6kg and be heated to 98 ℃, and 42-51% on year-on-year basis lowers consumption; The extraction time of prescription medical material foreshortened to about 1 hour by 5 hours, and the extraction energy consumption is reduced greatly.(5) be beneficial to environmental conservation and waste residue utilization: the medicinal residues after the isolation integral technical finesse is extracted in the membrane filter pressing circulation are the nearly powdered form block of doing; water content is few; not only be convenient to transhipment; can not pollute to environment; and be convenient to the later use of waste residue; as insert in the coal dust burning with reduce the coal consumption, biofermentation is made feedstuff, dry distilling is made as the charcoal piece and makes heating or domestic fuel etc.(6) on the basis of improving extracting method, the present invention also further improves the method for concentration of extracting solution, adopts nanofiltration to concentrate the traditional decompression heating of replacement and concentrates, simultaneously, in order to improve the nanofiltration concentrating efficiency, the present invention carries out the ultrafiltration pre-separation earlier before carrying out nanofiltration.Small-molecule substance in bod, total organic carbon, 7 kinds of essential amino acids (being the soluble small molecular material about molecular weight 75-150) and the Chinese medicine index components of the permeate of nanofiltration and concentrated solution is carried out quantitative analysis to be found, loss in the nanofiltration permeate can be ignored substantially, only runs off 0.3% as the bod CODcr that weighs total amount of organic.Adopt the nanofiltration method for concentration, can further reduce the degraded loss of thermal sensitivity composition Tanshinone I Ia etc.
Description of drawings
Fig. 1 extracts the preferred corollary apparatus figure of isolation integral technology for the membrane filter pressing circulation.
The specific embodiment
In order to make the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing the preferred embodiments of the present invention are described in detail.
The preferred corollary apparatus figure of membrane filter pressing circulation extraction isolation integral technology as shown in Figure 1, the discharging opening of material-compound tank is communicated with the charging aperture of diaphragm filter press by membrane pump, the liquid outlet of diaphragm filter press is communicated with the import of charging aperture and the filtrate tank of material-compound tank respectively with three-way valve, when three-way valve switches to the material-compound tank position, the liquid outlet of diaphragm filter press is communicated with the charging aperture of material-compound tank, the pressing filtering liquid that comes out from diaphragm filter press passes back into material-compound tank, constitutes membrane filter pressing circulation extraction system; When three-way valve switched to the filtrate tank position, the liquid outlet of diaphragm filter press was communicated with the import of filtrate tank, and the pressing filtering liquid that comes out from diaphragm filter press enters the filtrate tank storage, constitutes the membrane filter pressing solid-liquid separation system.
Embodiment 1
Prescription: Radix Salviae Miltiorrhizae 9kg, Radix Notoginseng 2.82kg, Borneolum Syntheticum 160g
Preparation method may further comprise the steps:
A. the extraction of Radix Salviae Miltiorrhizae
A1. the Radix Salviae Miltiorrhizae powder with recipe quantity is broken into coarse powder, and is standby;
A2. in material-compound tank, add 75% ethanol that is equivalent to 7.5 times of Radix Salviae Miltiorrhizae weight; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, 75% ethanol in the material-compound tank is pumped into diaphragm filter press (adopt 5-8 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, at the uniform velocity add step a gained medicated powder in material-compound tank, finish, the membrane filter pressing circulation was extracted 40 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position again, add 50% ethanol that is equivalent to 4 times of Radix Salviae Miltiorrhizae weight in material-compound tank, the membrane filter pressing circulation was extracted 20 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. three-way valve is switched to the material-compound tank position, in material-compound tank, add the water that is equivalent to 3 times of Radix Salviae Miltiorrhizae weight, close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, water in the material-compound tank is pumped into diaphragm filter press, the membrane filter pressing circulation was washed 5 minutes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, measure ethanol content, as the preparation liquid of next group tanshinol extraction solvent;
A4. three-way valve is switched to the material-compound tank position, add 65 ℃ the water of being preheated to that is equivalent to 5 times of Radix Salviae Miltiorrhizae weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 35 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge pressing filtering liquid and pressed liquor, be designated as extracting solution B;
B. preparation
B1. be that the hollow fiber ceramic membrane of 100nm carries out ultrafiltration with the extracting solution A of step a2 gained with the aperture, permeate uses DK8040F type NF membrane (molecular cut off is 150-300 dalton) to carry out nanofiltration again, running temperature is no more than 45 ℃, operating pressure is 1.3-1.5Mpa, when penetration speed be lower than initial velocity 80% the time stop nanofiltration, merge the concentrated solution of ultrafiltration and nanofiltration gained, get concentrated solution A, the permeate of nanofiltration is measured behind the ethanol content preparation liquid as next group tanshinol extraction solvent;
B2. the extracting solution B with step a4 gained carries out ultrafiltration according to the described method of step b1, and permeate carries out nanofiltration again, merges the concentrated solution of ultrafiltration and nanofiltration gained, gets concentrated solution B, and the permeate of nanofiltration discards;
B3. the Radix Notoginseng powder with recipe quantity is broken into fine powder, makes granule, drying with the concentrated solution A of step b1 gained, concentrated solution B and the adjuvant of step b2 gained; With the Borneolum Syntheticum porphyrize of recipe quantity, with above-mentioned dried granule mixing, tabletting, sugar coating or film-coat namely get FUFANG DANSHEN PIAN.
Embodiment 2
Prescription: Radix Salviae Miltiorrhizae 9kg, Radix Notoginseng 2.82kg, Borneolum Syntheticum 160g
Preparation method may further comprise the steps:
A. the extraction of Radix Salviae Miltiorrhizae
A1. the Radix Salviae Miltiorrhizae powder with recipe quantity is broken into coarse powder, and is standby;
A2. in material-compound tank, add 75% ethanol that is equivalent to 6 times of Radix Salviae Miltiorrhizae weight; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, 75% ethanol in the material-compound tank is pumped into diaphragm filter press (adopt 5-8 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, at the uniform velocity add step a gained medicated powder in material-compound tank, finish, the membrane filter pressing circulation was extracted 50 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position again, add 50% ethanol that is equivalent to 5 times of Radix Salviae Miltiorrhizae weight in material-compound tank, the membrane filter pressing circulation was extracted 10 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. three-way valve is switched to the material-compound tank position, in material-compound tank, add the water that is equivalent to 2 times of Radix Salviae Miltiorrhizae weight, close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, water in the material-compound tank is pumped into diaphragm filter press, the membrane filter pressing circulation was washed 3 minutes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, measure ethanol content, as the preparation liquid of next group tanshinol extraction solvent;
A4. three-way valve is switched to the material-compound tank position, add 55 ℃ the water of being preheated to that is equivalent to 6 times of Radix Salviae Miltiorrhizae weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 50 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge pressing filtering liquid and pressed liquor, be designated as extracting solution B;
B. preparation
B1. be that the hollow fiber ceramic membrane of 100nm carries out ultrafiltration with the extracting solution A of step a2 gained with the aperture, permeate uses NF90-4040 type NF membrane (molecular cut off is 100-150 dalton) to carry out nanofiltration again, running temperature is no more than 45 ℃, operating pressure is 1.3-1.5Mpa, when penetration speed be lower than initial velocity 80% the time stop nanofiltration, merge the concentrated solution of ultrafiltration and nanofiltration gained, get concentrated solution A, the permeate of nanofiltration is measured behind the ethanol content preparation liquid as next group tanshinol extraction solvent;
B2. the extracting solution B with step a4 gained carries out ultrafiltration according to the described method of step b1, and permeate carries out nanofiltration again, merges the concentrated solution of ultrafiltration and nanofiltration gained, gets concentrated solution B, and the permeate of nanofiltration discards;
B3. the Radix Notoginseng powder with recipe quantity is broken into fine powder, makes granule, drying with the concentrated solution A of step b1 gained, concentrated solution B and the adjuvant of step b2 gained; With the Borneolum Syntheticum porphyrize of recipe quantity, with above-mentioned dried granule mixing, tabletting, sugar coating or film-coat namely get FUFANG DANSHEN PIAN.
Embodiment 3
Prescription: Radix Salviae Miltiorrhizae 9kg, Radix Notoginseng 2.82kg, Borneolum Syntheticum 160g
Preparation method may further comprise the steps:
A. the extraction of Radix Salviae Miltiorrhizae
A1. the Radix Salviae Miltiorrhizae powder with recipe quantity is broken into coarse powder, and is standby;
A2. in material-compound tank, add 75% ethanol that is equivalent to 9 times of Radix Salviae Miltiorrhizae weight; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, 75% ethanol in the material-compound tank is pumped into diaphragm filter press (adopt 5-8 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, at the uniform velocity add step a gained medicated powder in material-compound tank, finish, the membrane filter pressing circulation was extracted 30 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position again, add 50% ethanol that is equivalent to 3 times of Radix Salviae Miltiorrhizae weight in material-compound tank, the membrane filter pressing circulation was extracted 30 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. three-way valve is switched to the material-compound tank position, in material-compound tank, add the water that is equivalent to 4 times of Radix Salviae Miltiorrhizae weight, close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, water in the material-compound tank is pumped into diaphragm filter press, the membrane filter pressing circulation was washed 7 minutes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, measure ethanol content, as the preparation liquid of next group tanshinol extraction solvent;
A4. three-way valve is switched to the material-compound tank position, add 60 ℃ the water of being preheated to that is equivalent to 4 times of Radix Salviae Miltiorrhizae weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 30 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge pressing filtering liquid and pressed liquor, be designated as extracting solution B;
B. preparation
B1. the extracting solution A decompression recycling ethanol with step a2 gained also concentrates, and gets concentrated solution A;
B2. the extracting solution B with step a4 gained concentrates, and gets concentrated solution B;
B3. the Radix Notoginseng powder with recipe quantity is broken into fine powder, makes granule, drying with the concentrated solution A of step b1 gained, concentrated solution B and the adjuvant of step b2 gained; With the Borneolum Syntheticum porphyrize of recipe quantity, with above-mentioned dried granule mixing, tabletting, sugar coating or film-coat namely get FUFANG DANSHEN PIAN.
Employing is with a collection of medicinal raw material, adopt the described method of embodiment 1-3 and existing method (Chinese Pharmacopoeia one one of version in 2010 is recorded method) to compare experiment respectively, and products obtained therefrom carried out quality inspection, the result shows: the product that adopts the described method of embodiment 1-3 to make all meets the requirement of quality standard, and the response rate of index components is higher.Wherein, the cost-effectiveness of embodiment 1 described method is than best, the content of the high index components Tanshinone I Ia of thermal sensitivity reaches the 0.41mg/ sheet in the products obtained therefrom, what be higher than drug standard regulation far away is not less than the 0.20mg/ sheet, and the content of Tanshinone I Ia only is the 0.17mg/ sheet in the product that existing method makes, and does not meet the regulation of quality standard.Embodiment 1-2 compares with embodiment 3, adopts nanofiltration to concentrate to replace traditional decompression heating to concentrate, and can further reduce the degraded loss of thermal sensitivity composition Tanshinone I Ia etc.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (7)
1. the preparation method of FUFANG DANSHEN PIAN, made by following raw materials by weight proportions: 8 parts of 450 parts of Radix Salviae Miltiorrhizaes, 141 parts of Radix Notoginseng and Borneolum Syntheticums is characterized in that preparation method may further comprise the steps:
A. the extraction of Radix Salviae Miltiorrhizae
A1. Radix Salviae Miltiorrhizae powder is broken into coarse powder, standby;
A2. adding concentration of volume percent in the material-compound tank is the ethanol of 75-90%; Three-way valve is switched to the material-compound tank position, be that the ethanol of 75-90% pumps into diaphragm filter press with the concentration of volume percent in the material-compound tank, when passing back into material-compound tank to pressing filtering liquid, under stirring condition, in material-compound tank, add step a1 gained medicated powder, finish, carry out the membrane filter pressing circulation first time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, again three-way valve is switched to the material-compound tank position, add concentration of volume percent in the material-compound tank and be 50% ethanol, carry out membrane filter pressing circulation extraction second time, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. in material-compound tank, add water, be heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, the water in the material-compound tank is pumped into diaphragm filter press, under 50-90 ℃ condition, carry out the membrane filter pressing circulation and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, be designated as extracting solution B;
B. preparation
B1. the extracting solution A with step a2 gained reclaims ethanol and concentrated, gets concentrated solution A;
B2. the extracting solution B with step a3 gained concentrates, and gets concentrated solution B;
B3. the Radix Notoginseng powder with recipe quantity is broken into fine powder, makes granule, drying with the concentrated solution A of step b1 gained, concentrated solution B and the adjuvant of step b2 gained; With the Borneolum Syntheticum porphyrize of recipe quantity, with above-mentioned dried granule mixing, tabletting, sugar coating or film-coat namely get FUFANG DANSHEN PIAN.
2. the preparation method of FUFANG DANSHEN PIAN according to claim 1, it is characterized in that, described step a2 adds earlier that to be equivalent to Radix Salviae Miltiorrhizae weight 6-9 concentration of volume percent doubly be 75% ethanol, carries out membrane filter pressing circulation extraction first time, and extraction time is 30-50 minute; Adding and being equivalent to Radix Salviae Miltiorrhizae weight 3-5 concentration of volume percent doubly is 50% ethanol, carries out membrane filter pressing circulation extraction second time, and extraction time is 10-30 minute;
Described step a3 adds earlier to be equivalent to Radix Salviae Miltiorrhizae weight 4-6 water doubly, carries out the membrane filter pressing circulation and extract under 55-65 ℃ condition, and extraction time is 30-50 minute.
3. the preparation method of FUFANG DANSHEN PIAN according to claim 2, it is characterized in that, described step a2 is that to add earlier the concentration of volume percent that is equivalent to 7.5 times of Radix Salviae Miltiorrhizae weight be 75% ethanol, carries out membrane filter pressing circulation extraction first time, and extraction time is 40 minutes; Add the concentration of volume percent be equivalent to 4 times of Radix Salviae Miltiorrhizae weight again and be 50% ethanol, carry out membrane filter pressing circulation extraction second time, extraction time is 20 minutes;
Described step a3 adds the water that is equivalent to 5 times of Radix Salviae Miltiorrhizae weight earlier, carries out the membrane filter pressing circulation and extract under 65 ℃ condition, and extraction time is 35 minutes.
4. the preparation method of FUFANG DANSHEN PIAN according to claim 1, it is characterized in that, described step b1 is with extracting solution A ultrafiltration membrance filter, permeate carries out nanofiltration again, the concentrated solution that merges ultrafiltration and nanofiltration gained, concentrated solution A, the permeate of nanofiltration is measured behind the ethanol content preparation liquid as next group tanshinol extraction solvent;
Described step b2 is with extracting solution B ultrafiltration membrance filter, and permeate carries out nanofiltration again, merges the concentrated solution of ultrafiltration and nanofiltration gained, gets concentrated solution B.
5. the preparation method of FUFANG DANSHEN PIAN according to claim 4 is characterized in that, ultrafiltration employing aperture is the ceramic membrane of 50-200nm among described step b1 and the b2, and it is the daltonian NF membrane of 100-300 that molecular cut off is adopted in nanofiltration.
6. according to the preparation method of the described FUFANG DANSHEN PIAN of the arbitrary claim of claim 1 to 5, it is characterized in that, also comprise step a2 ＇ between described step a2 and the a3: three-way valve is switched to the material-compound tank position, in material-compound tank, add water, carrying out the membrane filter pressing circulation washes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, measure ethanol content, as the preparation liquid of next group tanshinol extraction solvent.
7. the preparation method of FUFANG DANSHEN PIAN according to claim 6 is characterized in that, described step a2 ＇ adds to be equivalent to Radix Salviae Miltiorrhizae weight 2-4 water doubly, and the membrane filter pressing circulation was washed 3-7 minute thoroughly.
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