CN102293884B - Preparation method of anti-diarrheal medicinal composition - Google Patents
Preparation method of anti-diarrheal medicinal composition Download PDFInfo
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Abstract
The invention discloses a preparation method of an anti-diarrheal medicinal composition. According to the preparation method disclosed by the invention, effective components in medicinal materials in a prescription are extracted by adopting a diaphragm filter press circulation, extraction and separation integrated technology instead of an ultrasonic treatment method or a decocting method, thus a process flow can be simplified, the production period is greatly shortened, the energy consumption is reduced, environmental protection and utilization of waste residue are facilitated, and the recovery rate of the effective components can be greatly improved.
Description
Technical field
The invention belongs to pharmaceutical field, relate to a kind of preparation method of Chinese medicine preparation.
Background technology
Chinese patent ZL95117485.1 discloses a kind of antidiarrheal pharmaceutical composition.Crude drug by the following weight proportioning is made: Rhizoma Atractylodis Macrocephalae 200-350 part, Poria 200-350 part, Polyporus 300-400 part, Rhizoma Pinelliae 200-300 part, Pericarpium Citri Reticulatae 200-350 part, Cortex Cinnamomi 100-250 part, Radix Scutellariae 200-350 part, Rhizoma Osmundae 300-400 part, Radix Sanguisorbae 500-600 part.The preferred weight proportioning is 502.5 parts of 268 parts of the Rhizoma Atractylodis Macrocephalaes, 234.5 parts in Poria, 301.5 parts of Polyporus, 201 parts of the Rhizoma Pinelliaes, 234.5 parts of Pericarpium Citri Reticulataes, 167.5 parts of Cortex Cinnamomis, 268 parts of Radix Scutellariaes, 335 parts of Rhizoma Osmundae and Radix Sanguisorbaes.The preparation method of its oral liquid formulation is: get Poria, Polyporus adds water temperature and soaks twice, is respectively 3 hours and 2 hours, add water is 10 times of amounts of crude drug at every turn, merges warm macerating liquid, filters, and filtrate is concentrated into 50 ℃ of relative density 1.02-1.03, and is for subsequent use; Other gets the Rhizoma Atractylodis Macrocephalae, Pericarpium Citri Reticulatae, Cortex Cinnamomi and adds 8 times of amounts of water, extracts volatile oil with the way of distillation, and extraction time, until volatile oil no longer increases, the medicinal residues after the distillation added 4 times in water more than 5 hours, decocts half an hour, and decocting liquid in addition device is collected; All the other 4 flavors are fried in shallow oil three times, and wherein Radix Scutellariae boils rear time, adds 8 times in water at every turn, decocts 1 hour at every turn, decocting liquid after collecting decoction and the distillation filters, and filtrate is concentrated into 80 ℃ of relative density 1.16-1.19, lets cool, adding ethanol is 60-75% to containing determining alcohol, and hold over night filters, and decompression filtrate recycling ethanol is to nothing alcohol flavor, add above-mentioned warm macerating liquid, volatile oil and tween 80, adjust pH are 5.0-6.5, add water to 1000ml, leave standstill, filter, fill, sterilization, and get final product.Adopt warm macerating method, decocting method to extract the effective ingredient of prescription medical material in the above-mentioned preparation method, have long, high, the shortcomings such as energy consumption is high, the thermal sensitivity composition easily loses, the effective ingredient response rate is low, post processing trouble of extraction temperature of extraction time.
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 above-mentioned antidiarrheal pharmaceutical composition; not only can simplification of flowsheet; significantly shorten the production cycle; energy efficient; be beneficial to environmental conservation and waste residue utilization, and can greatly improve the response rate of effective ingredient.
For achieving the above object, the invention provides following technical scheme:
The preparation method of umbellate pore fungus and poria cocos antidiarrhea oral liquid, crude drug by the following weight proportioning is made: Rhizoma Atractylodis Macrocephalae 200-350 part, Poria 200-350 part, Polyporus 300-400 part, Rhizoma Pinelliae 200-300 part, Pericarpium Citri Reticulatae 200-350 part, Cortex Cinnamomi 100-250 part, Radix Scutellariae 200-350 part, Rhizoma Osmundae 300-400 part, Radix Sanguisorbae 500-600 part, and preparation method may further comprise the steps:
A. the extraction of the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae
A1. the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae are mixed, be ground into coarse powder, for subsequent use;
A2. with the medicated powder extraction by steam distillation volatile oil of step a1 gained, the aqueous solution after medicinal residues and the distillation is for subsequent use;
A3. in the medicinal residues of step a2 gained, add water, be heated with stirring to 60-95 ℃, slip is pumped into diaphragm filter press carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, will be preheated to again 60-95 ℃ water and pumps into diaphragm filter press and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor; Aqueous solution after the distillation of twice pressing filtering liquid, pressed liquor and step a2 gained is merged, be designated as extracting solution A;
B. the extraction of the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae
B1. the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae are mixed, be ground into coarse powder, for subsequent use;
B2. the extracting solution A and the water that add step a3 gained in the material-compound tank are heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, water 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 b1 gained medicated powder, finish, under 50-90 ℃ condition, 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 is complete, again three-way valve is switched to the material-compound tank position, in material-compound tank, add entry, under 50-90 ℃ condition, 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 is complete, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. the extraction of Poria and Polyporus
C1. Poria and Polyporus are mixed, be ground into coarse powder, for subsequent use;
C2. in material-compound tank, add entry, be heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, water 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 c1 gained medicated powder, finish, under 50-90 ℃ condition, 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 is complete, again three-way valve is switched to the material-compound tank position, in material-compound tank, add entry, under 50-90 ℃ condition, 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 is complete, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution C;
D. preparation
D1. the extracting solution C of step c2 gained is concentrated, for subsequent use;
D2. the extracting solution B of step b2 gained is concentrated, let cool, adding ethanol is 60-75% to containing pure concentration of volume percent, leave standstill, filter, filtrate recycling ethanol adds the concentrate of steps d 1 gained, volatile oil and the pharmaceutically acceptable adjuvant of step a2 gained, adopt practice of pharmacy to make pharmaceutical preparation, and get final product.
Preferably, described step a3 adds in the medicinal residues first to be equivalent to step a1 gained medicated powder weight 2-4 water doubly, is heated with stirring to 75-95 ℃, insulated and stirred 5-15 minute, with slip pump into diaphragm filter press carry out the membrane filter pressing To be equivalent to again step a1 gained medicated powder weight 1-3 doubly be preheated to 75-95 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds first the described extracting solution A of step a3, and adds 6-8 that the water ad pond om is equivalent to step b1 gained medicated powder weight doubly, carries out membrane filter pressing circulation extraction first time under 55-65 ℃ condition, and extraction time is 20-40 minute; Add and be equivalent to step b1 gained medicated powder weight 2-4 water doubly, carry out the membrane filter pressing circulation second time and extract under 55-65 ℃ condition, extraction time is 10-20 minute;
Described step c2 adds first to be equivalent to step c1 gained medicated powder weight 6-8 water doubly, carries out the membrane filter pressing circulation first time and extract under 55-65 ℃ condition, and extraction time is 30-40 minute; Add and be equivalent to step c1 gained medicated powder weight 2-5 water doubly, carry out the membrane filter pressing circulation second time and extract under 55-65 ℃ condition, extraction time is 10-20 minute.
Preferred, described step a3 first adds the water that is equivalent to 2 times of step a1 gained medicated powder weight in medicinal residues, be heated with stirring to 80 ℃, insulated and stirred 5 minutes, with slip pump into diaphragm filter press carry out the membrane filter pressing To be equivalent to again 1 times of step a1 gained medicated powder weight be preheated to 80 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds first the described extracting solution A of step a3, and adds the water ad pond om and be equivalent to 7 times of step b1 gained medicated powder weight, carries out the membrane filter pressing circulation first time and extract under 65 ℃ condition, and extraction time is 25 minutes; Add the water that is equivalent to 3 times of step b1 gained medicated powder weight again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 10 minutes;
Described step c2 adds first the water that is equivalent to 7 times of step c1 gained medicated powder weight, carries out the membrane filter pressing circulation first time and extract under 65 ℃ condition, and extraction time is 35 minutes; Add the water that is equivalent to 3.5 times of step c1 gained medicated powder weight again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 15 minutes.
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 (such as membrane pump etc.), the liquid outlet of diaphragm filter press is communicated with respectively the import of charging aperture and the filtrate tank of material-compound tank 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, consist of membrane filter pressing circulation extraction system, slip in the material-compound tank is pumped to diaphragm filter press to carry out membrane filter pressing 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 from diaphragm filter press pressing filtering liquid out, 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, consist of the membrane filter pressing solid-liquid separation system, after the membrane filter pressing circulation extraction of medical material is complete, to send into the filtrate tank storage from diaphragm filter press pressing filtering liquid and pressed liquor 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 (such 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 is less, can in material-compound tank, directly adds 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 first first required whole solvents 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 again medicated powder, 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, during take water as solvent, extract temperature and can be controlled 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 the phenomenons such as filter cloth, when the medical material of rich in starch is carried out water extraction, extract temperature and should be controlled at below 70 ℃, preferred 55-65 ℃.And when adopting organic solvent extraction, can not heat (namely at room temperature extracting) or suitably heating depending on the boiling point height of organic solvent.
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 first extraction solvent of next group material.When take alcohol-water mixed solution as the extraction solvent, carry out membrane filter pressing in the complete rear available water of extraction and thoroughly wash and squeeze medicinal residues, after gained pressing filtering liquid and pressed liquor were measured pure content, the preparation liquid that can be used as next group material extraction solvent carried out recycled.Carry out membrane filter pressing when thoroughly washing 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 extract first 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 simultaneously follow-up concentrated energy consumption 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, thoroughly wash 1-2 time, aqueous solution after the saturating washing liquid of gained and the distillation merges, as the first water extraction solvent of other medical material.
About the problem of diaphragm filter press, filter cloth should be selected polypropylene multifilament filter cloth, and its Air permenbility selection principle is: less (such as 3-10L/m with the appropriate to the occasion Air permenbility of selecting of organic solvent extraction
2.s) filter cloth is large (such as 50-1200L/m with the appropriate to the occasion Air permenbility of selecting 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.
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 warm macerating method and decocting method extraction prescription medical material, the party's genealogy of law 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, content such as baicalin improves 10-14% than existing method, and the content of 75% ethanol ethanol-soluble extractives improves 9-15% than existing method; And the filter cloth aperture of adopting because of diaphragm filter press is far below being used at present the aperture of filter screen that medicinal residues separate with decocting liquid, 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) simplified technological process, shortened the production cycle: Poria and the Polyporus of extracting same weight, adopt the warm macerating method to need 5 hours, extract the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and the Radix Sanguisorbae of same weight, adopt decocting method to need 3 hours, all be no more than 1 hour and adopt the membrane filter pressing circulating extraction method to extract above-mentioned medical material, extraction time shortens more than 60%; And the inventive method can realize the integrated of extraction and solid-liquid separation that circulate, and does not have the worry of the existing follow-up solid-liquid separation of decocting method.(3) 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 1 hour by 2 hours, and the extraction energy consumption is reduced greatly.(4) 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 give 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.(5) require the Rhizoma Atractylodis Macrocephalae in the existing method, the medicinal residues that Cortex Cinnamomi and Pericarpium Citri Reticulatae extract behind the volatile oil decoct with water half an hour, reach a few hours owing to extract the process of volatile oil with the water azeotropic, during the water soluble ingredient of above-mentioned medical material fully is soluble in the aqueous phase in the process of extracting volatile oil, so the medicinal residues that the inventive method no longer will be extracted behind the volatile oil decoct with water, and only with hot water medicinal residues are washed thoroughly, aqueous solution after washing liquid and the distillation merges thoroughly, as the Rhizoma Pinelliae, Radix Scutellariae, the first extraction solvent of Rhizoma Osmundae and Radix Sanguisorbae is applied mechanically, when guaranteeing the effective ingredient response rate, reduce and extract solvent load, reduce follow-up concentrated energy consumption.
Description of drawings
Fig. 1 is the preferred corollary apparatus figure that the isolation integral technology is extracted in 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 respectively the import of charging aperture and the filtrate tank of material-compound tank 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, pass back into material-compound tank from diaphragm filter press pressing filtering liquid out, consist of 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, entered filtrate tank from diaphragm filter press pressing filtering liquid out and stored, and consisted of the membrane filter pressing solid-liquid separation system.
Embodiment 1
Prescription: Rhizoma Atractylodis Macrocephalae 5.36kg, Poria 4.69kg, Polyporus 6.03kg, Rhizoma Pinelliae 4.02kg, Pericarpium Citri Reticulatae 4.69kg, Cortex Cinnamomi 3.35kg, Radix Scutellariae 5.36kg, Rhizoma Osmundae 6.7kg, Radix Sanguisorbae 10.05kg
Preparation method: may further comprise the steps:
A. the extraction of the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae
A1. the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae are mixed, be ground into coarse powder, for subsequent use;
A2. step a1 gained medicated powder is put in the multi-function extractor, extracted volatile oil with straight-through steam distillation method, the aqueous solution after the distillation in addition device is collected, and is for subsequent use;
A3. add the water that is equivalent to 2 times of step a1 gained medicated powder weight to being equipped with in the multi-function extractor that extracts medicinal residues behind the volatile oil, be heated with stirring to 80 ℃, insulated and stirred 5 minutes pumps into diaphragm filter press with slip and (adopts 80 ± 10 L/m
2.s polypropylene multifilament filter cloth) carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, add again 90 ℃ the water of being preheated to that is equivalent to 1 times of step a1 gained medicated powder weight in the multi-function extractor, pump into diaphragm filter press and carry out membrane filter pressing, collect pressing filtering liquid; Start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Aqueous solution after the distillation of pressing filtering liquid, pressed liquor and step a2 gained is merged, be designated as extracting solution A;
B. the extraction of the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae
B1. the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae are mixed, be ground into coarse powder, for subsequent use;
B2. add the extracting solution A of step a3 gained in the material-compound tank, and add the water ad pond om and be equivalent to 7 times of step b1 gained medicated powder weight, be heated to 65 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, in material-compound tank, at the uniform velocity add step b1 gained medicated powder, finish, 65 ℃ of membrane filter pressing circulations were extracted 25 minutes, afterwards three-way valve were switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing is complete, three-way valve is switched to the material-compound tank position again, add 65 ℃ the water of being preheated to that is equivalent to 3 times of step b1 gained medicated powder weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 10 minutes, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. the extraction of Poria and Polyporus
C1. Poria and Polyporus are mixed, be ground into coarse powder, for subsequent use;
C2. in material-compound tank, add the water that is equivalent to 7 times of step c1 gained medicated powder weight, be heated to 65 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, in material-compound tank, at the uniform velocity add step c1 gained medicated powder, finish, 65 ℃ of membrane filter pressing circulations were extracted 35 minutes, afterwards three-way valve were switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing is complete, again three-way valve is switched to the material-compound tank position, add 65 ℃ the water of being preheated to that is equivalent to 3.5 times of step b1 gained medicated powder weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 15 minutes, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution C;
D. preparation
D1. the clear paste that the extracting solution C of step c2 gained to be concentrated into 50 ℃ of relative densities be 1.02-1.03, for subsequent use;
D2. the extracting solution B of step b2 gained being concentrated into 80 ℃ of relative densities is 1.16-1.19, lets cool, and adding ethanol is 60-75% to containing pure concentration of volume percent, hold over night filters, and decompression filtrate recycling ethanol is to distinguishing the flavor of without alcohol, add the clear paste of steps d 1 gained, volatile oil and the tween 80 200ml of step a2 gained, adjust pH is 5.0-6.5, adds water to 20L, leaves standstill, filter, fill, sterilization, and get final product.
Embodiment 2
Prescription: Rhizoma Atractylodis Macrocephalae 5.36kg, Poria 4.69kg, Polyporus 6.03kg, Rhizoma Pinelliae 4.02kg, Pericarpium Citri Reticulatae 4.69kg, Cortex Cinnamomi 3.35kg, Radix Scutellariae 5.36kg, Rhizoma Osmundae 6.7kg, Radix Sanguisorbae 10.05kg
Preparation method: may further comprise the steps:
A. the extraction of the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae
A1. the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae are mixed, be ground into coarse powder, for subsequent use;
A2. step a1 gained medicated powder is put in the multi-function extractor, extracted volatile oil with straight-through steam distillation method, the aqueous solution after the distillation in addition device is collected, and is for subsequent use;
A3. add the water that is equivalent to 4 times of step a1 gained medicated powder weight to being equipped with in the multi-function extractor that extracts medicinal residues behind the volatile oil, be heated with stirring to 75 ℃, insulated and stirred 15 minutes pumps into diaphragm filter press with slip and (adopts 80 ± 10 L/m
2.s polypropylene multifilament filter cloth) carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, add again 75 ℃ the water of being preheated to that is equivalent to 3 times of step a1 gained medicated powder weight in the multi-function extractor, pump into diaphragm filter press and carry out membrane filter pressing, collect pressing filtering liquid; Start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Aqueous solution after the distillation of pressing filtering liquid, pressed liquor and step a2 gained is merged, be designated as extracting solution A;
B. the extraction of the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae
B1. the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae are mixed, be ground into coarse powder, for subsequent use;
B2. add the extracting solution A of step a3 gained in the material-compound tank, and add the water ad pond om and be equivalent to 8 times of step b1 gained medicated powder weight, be heated to 55 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, in material-compound tank, at the uniform velocity add step b1 gained medicated powder, finish, 55 ℃ of membrane filter pressing circulations were extracted 40 minutes, afterwards three-way valve were switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing is complete, three-way valve is switched to the material-compound tank position again, add 55 ℃ the water of being preheated to that is equivalent to 4 times of step b1 gained medicated powder weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 20 minutes, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. the extraction of Poria and Polyporus
C1. Poria and Polyporus are mixed, be ground into coarse powder, for subsequent use;
C2. in material-compound tank, add the water that is equivalent to 6 times of step c1 gained medicated powder weight, be heated to 60 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, in material-compound tank, at the uniform velocity add step c1 gained medicated powder, finish, 60 ℃ of membrane filter pressing circulations were extracted 30 minutes, afterwards three-way valve were switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing is complete, three-way valve is switched to the material-compound tank position again, add 60 ℃ the water of being preheated to that is equivalent to 2 times of step b1 gained medicated powder weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 10 minutes, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution C;
D. preparation
D1. the clear paste that the extracting solution C of step c2 gained to be concentrated into 50 ℃ of relative densities be 1.02-1.03, for subsequent use;
D2. the extracting solution B of step b2 gained being concentrated into 80 ℃ of relative densities is 1.16-1.19, lets cool, and adding ethanol is 60-75% to containing pure concentration of volume percent, hold over night filters, and decompression filtrate recycling ethanol is to distinguishing the flavor of without alcohol, add the clear paste of steps d 1 gained, volatile oil and the tween 80 200ml of step a2 gained, adjust pH is 5.0-6.5, adds water to 20L, leaves standstill, filter, fill, sterilization, and get final product.
Embodiment 3
Prescription: Rhizoma Atractylodis Macrocephalae 5.36kg, Poria 4.69kg, Polyporus 6.03kg, Rhizoma Pinelliae 4.02kg, Pericarpium Citri Reticulatae 4.69kg, Cortex Cinnamomi 3.35kg, Radix Scutellariae 5.36kg, Rhizoma Osmundae 6.7kg, Radix Sanguisorbae 10.05kg
Preparation method: may further comprise the steps:
A. the extraction of the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae
A1. the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae are mixed, be ground into coarse powder, for subsequent use;
A2. step a1 gained medicated powder is put in the multi-function extractor, extracted volatile oil with straight-through steam distillation method, the aqueous solution after the distillation in addition device is collected, and is for subsequent use;
A3. add the water that is equivalent to 3 times of step a1 gained medicated powder weight to being equipped with in the multi-function extractor that extracts medicinal residues behind the volatile oil, be heated with stirring to 95 ℃, insulated and stirred 10 minutes pumps into diaphragm filter press with slip and (adopts 80 ± 10 L/m
2.s polypropylene multifilament filter cloth) carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, add again 95 ℃ the water of being preheated to that is equivalent to 2 times of step a1 gained medicated powder weight in the multi-function extractor, pump into diaphragm filter press and carry out membrane filter pressing, collect pressing filtering liquid; Start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Aqueous solution after the distillation of pressing filtering liquid, pressed liquor and step a2 gained is merged, be designated as extracting solution A;
B. the extraction of the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae
B1. the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae are mixed, be ground into coarse powder, for subsequent use;
B2. add the extracting solution A of step a3 gained in the material-compound tank, and add the water ad pond om and be equivalent to 6 times of step b1 gained medicated powder weight, be heated to 60 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, in material-compound tank, at the uniform velocity add step b1 gained medicated powder, finish, 60 ℃ of membrane filter pressing circulations were extracted 30 minutes, afterwards three-way valve were switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing is complete, three-way valve is switched to the material-compound tank position again, add 60 ℃ the water of being preheated to that is equivalent to 2 times of step b1 gained medicated powder weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 10 minutes, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. the extraction of Poria and Polyporus
C1. Poria and Polyporus are mixed, be ground into coarse powder, for subsequent use;
C2. in material-compound tank, add the water that is equivalent to 8 times of step c1 gained medicated powder weight, be heated to 55 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, in material-compound tank, at the uniform velocity add step c1 gained medicated powder, finish, 55 ℃ of membrane filter pressing circulations were extracted 40 minutes, afterwards three-way valve were switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing is complete, three-way valve is switched to the material-compound tank position again, add 55 ℃ the water of being preheated to that is equivalent to 5 times of step b1 gained medicated powder weight in the material-compound tank, the circulation of insulation membrane filter pressing was extracted 20 minutes, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution C;
D. preparation
D1. the clear paste that the extracting solution C of step c2 gained to be concentrated into 50 ℃ of relative densities be 1.02-1.03, for subsequent use;
D2. the extracting solution B of step b2 gained being concentrated into 80 ℃ of relative densities is 1.16-1.19, lets cool, and adding ethanol is 60-75% to containing pure concentration of volume percent, hold over night filters, and decompression filtrate recycling ethanol is to distinguishing the flavor of without alcohol, add the clear paste of steps d 1 gained, volatile oil and the tween 80 200ml of step a2 gained, adjust pH is 5.0-6.5, adds water to 20L, leaves standstill, filter, fill, sterilization, and get final product.
Employing is with a collection of medicinal raw material, adopt respectively the described method of embodiment 1-3 and existing method (the open method of Chinese patent ZL95117485.1) to compare test, and the gained finished product carried out quality inspection, the result shows: the product that adopts the described method of embodiment 1-3 to make, the content of baicalin improves 10-14% than existing method, the content of 75% ethanol ethanol-soluble extractives improves 9-15% than existing method, the existing method of thick paste weight ratio before the precipitate with ethanol reduces 16-21%, the amount of alcohol that is equivalent to expend reduces, but the content of various index components increases on the contrary.Wherein, the cost-effectiveness of embodiment 1 described method is than best, and the content of baicalin improves 14%, 75% ethanol ethanol-soluble extractives than existing method content improves 15% than existing method, and the existing method of the thick paste weight ratio before the precipitate with ethanol reduces by 20%.
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 (3)
1. the preparation method of antidiarrheal pharmaceutical composition, crude drug by the following weight proportioning is made: Rhizoma Atractylodis Macrocephalae 200-350 part, Poria 200-350 part, Polyporus 300-400 part, Rhizoma Pinelliae 200-300 part, Pericarpium Citri Reticulatae 200-350 part, Cortex Cinnamomi 100-250 part, Radix Scutellariae 200-350 part, Rhizoma Osmundae 300-400 part, Radix Sanguisorbae 500-600 part, it is characterized in that preparation method may further comprise the steps:
A. the extraction of the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae
A1. the Rhizoma Atractylodis Macrocephalae, Cortex Cinnamomi and Pericarpium Citri Reticulatae are mixed, be ground into coarse powder, for subsequent use;
A2. with the medicated powder extraction by steam distillation volatile oil of step a1 gained, the aqueous solution after medicinal residues and the distillation is for subsequent use;
A3. in the medicinal residues of step a2 gained, add water, be heated with stirring to 60-95 ℃, slip is pumped into diaphragm filter press carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, will be preheated to again 60-95 ℃ water and pumps into diaphragm filter press and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing is complete, start the squeezing program of diaphragm filter press, collect pressed liquor; Aqueous solution after the distillation of twice pressing filtering liquid, pressed liquor and step a2 gained is merged, be designated as extracting solution A;
B. the extraction of the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae
B1. the Rhizoma Pinelliae, Radix Scutellariae, Rhizoma Osmundae and Radix Sanguisorbae are mixed, be ground into coarse powder, for subsequent use;
B2. the extracting solution A and the water that add step a3 gained in the material-compound tank are heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, water 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 b1 gained medicated powder, finish, under 50-90 ℃ condition, 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 is complete, again three-way valve is switched to the material-compound tank position, in material-compound tank, add entry, under 50-90 ℃ condition, 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 is complete, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. the extraction of Poria and Polyporus
C1. Poria and Polyporus are mixed, be ground into coarse powder, for subsequent use;
C2. in material-compound tank, add entry, be heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, water 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 c1 gained medicated powder, finish, under 50-90 ℃ condition, 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 is complete, again three-way valve is switched to the material-compound tank position, in material-compound tank, add entry, under 50-90 ℃ condition, 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 is complete, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution C;
D. preparation
D1. the extracting solution C of step c2 gained is concentrated, for subsequent use;
D2. the extracting solution B of step b2 gained is concentrated, let cool, adding ethanol is 60-75% to containing pure concentration of volume percent, leave standstill, filter, filtrate recycling ethanol adds the concentrate of steps d 1 gained, volatile oil and the pharmaceutically acceptable adjuvant of step a2 gained, adopt practice of pharmacy to make pharmaceutical preparation, and get final product.
2. the preparation method of antidiarrheal pharmaceutical composition according to claim 1, it is characterized in that, described step a3 adds in the medicinal residues first to be equivalent to step a1 gained medicated powder weight 2-4 water doubly, be heated with stirring to 75-95 ℃, insulated and stirred 5-15 minute, slip is pumped into diaphragm filter press carry out membrane filter pressing To be equivalent to again step a1 gained medicated powder weight 1-3 doubly be preheated to 75-95 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds first the described extracting solution A of step a3, and adds 6-8 that the water ad pond om is equivalent to step b1 gained medicated powder weight doubly, carries out membrane filter pressing circulation extraction first time under 55-65 ℃ condition, and extraction time is 20-40 minute; Add and be equivalent to step b1 gained medicated powder weight 2-4 water doubly, carry out the membrane filter pressing circulation second time and extract under 55-65 ℃ condition, extraction time is 10-20 minute;
Described step c2 adds first to be equivalent to step c1 gained medicated powder weight 6-8 water doubly, carries out the membrane filter pressing circulation first time and extract under 55-65 ℃ condition, and extraction time is 30-40 minute; Add and be equivalent to step c1 gained medicated powder weight 2-5 water doubly, carry out the membrane filter pressing circulation second time and extract under 55-65 ℃ condition, extraction time is 10-20 minute.
3. the preparation method of antidiarrheal pharmaceutical composition according to claim 2, it is characterized in that described step a3 adds the water that is equivalent to 2 times of step a1 gained medicated powder weight first in medicinal residues, be heated with stirring to 80 ℃, insulated and stirred 5 minutes pumps into diaphragm filter press with slip and carries out membrane filter pressing To be equivalent to again 1 times of step a1 gained medicated powder weight be preheated to 80 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds first the described extracting solution A of step a3, and adds the water ad pond om and be equivalent to 7 times of step b1 gained medicated powder weight, carries out the membrane filter pressing circulation first time and extract under 65 ℃ condition, and extraction time is 25 minutes; Add the water that is equivalent to 3 times of step b1 gained medicated powder weight again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 10 minutes;
Described step c2 adds first the water that is equivalent to 7 times of step c1 gained medicated powder weight, carries out the membrane filter pressing circulation first time and extract under 65 ℃ condition, and extraction time is 35 minutes; Add the water that is equivalent to 3.5 times of step c1 gained medicated powder weight again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 15 minutes.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150906A (en) * | 1995-11-22 | 1997-06-04 | 四川涪陵制药厂 | Umbellate pore fungus and poria cocos antidiarrhea oral liquid and its production technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150906A (en) * | 1995-11-22 | 1997-06-04 | 四川涪陵制药厂 | Umbellate pore fungus and poria cocos antidiarrhea oral liquid and its production technology |
Non-Patent Citations (2)
| Title |
|---|
| 严晓梁.双苓止泻口服液煎煮提取的工艺研究.《实用医院临床杂志》.1994,第48-49页. * |
| 陈彪等.隔膜压滤工艺在甘草流浸膏生产上的应用研究.《2008年成渝药学学术年会论文集》.2008,第117-118页. * |
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