CN102293897B - Preparation method of Liuweidihuang pills - Google Patents
Preparation method of Liuweidihuang pills Download PDFInfo
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- CN102293897B CN102293897B CN 201110247764 CN201110247764A CN102293897B CN 102293897 B CN102293897 B CN 102293897B CN 201110247764 CN201110247764 CN 201110247764 CN 201110247764 A CN201110247764 A CN 201110247764A CN 102293897 B CN102293897 B CN 102293897B
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Abstract
The invention discloses a preparation method of Liuweidihuang pills. The preparation method adopts a diaphragm press filtration cycle extraction separation integrated technology to extract active ingredients of prescription drugs. The preparation method simplifies a process flow, shortens greatly a production period, saves energy consumption, is beneficial for environmental protection and dreg utilization, and improves greatly an active ingredient recovery rate.
Description
Technical field
The invention belongs to pharmaceutical field, relate to a kind of preparation method of Chinese medicine preparation.
Background technology
The Sanitation Ministry medicine standard WS3-B-2102-96 record: LIUWEI DIHUANG WAN (concentrated pill) has the effect of enriching yin and nourishing kidney, is used for damage of kidney-YIN, dizziness and tinnitus, soreness of the waist and knees, osteopyrexia and fever, night sweat seminal emission, quenches one's thirst.Its prescription is total to the Six-element medicine by Radix Rehmanniae Preparata 160g, Fructus Corni (processed) 80g, Cortex Moutan 60g, Rhizoma Dioscoreae 80g, Poria 60g and Rhizoma Alismatis 60g and forms.Its preparation method is that Cortex Moutan is extracted paeonol; Medicinal residues and Fructus Corni 27g, Radix Rehmanniae Preparata, Poria, Rhizoma Alismatis decoct with water secondary, and each 2 hours, collecting decoction filtered, and filtrate is concentrated into the thick paste that relative density is 1.35-1.40; Rhizoma Dioscoreae is broken into fine powder with the residue powder of Fructus Corni, sieves mixing; With above thick paste, fine powder, paeonol mixing, pill, drying, polishing, and get final product.Adopt decocting method to extract the effective ingredient of prescription medical material in the said method, exist extraction time long, extract that temperature is 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.
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 LIUWEI DIHUANG WAN (concentrated pill); 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 LIUWEI DIHUANG WAN, made by the crude drug of following weight proportioning: 60 parts of 160 parts of Radix Rehmanniae Preparata, 80 parts of Fructus Corni (processed)s, 60 parts of Cortex Moutans, 80 parts of Rhizoma Dioscoreaes, 60 parts in Poria and Rhizoma Alismatis, preparation method may further comprise the steps:
A. the extraction of Cortex Moutan
A1. Cortex Moutan is 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 60-90 ℃, 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 60-90 ℃ 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 Fructus Corni (processed), Radix Rehmanniae Preparata, Poria and Rhizoma Alismatis
B1. Poria, Rhizoma Alismatis are mixed with the Fructus Corni (processed) of proportional quantity 1/3rd, be ground into coarse powder, for subsequent use; Radix Rehmanniae Preparata is broken into slip with pigment, 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, the medicated powder and the Radix Rehmanniae Preparata slip that under stirring condition, add step b1 gained in the material-compound tank, 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. preparation
C1. the extracting solution B with step b2 gained is concentrated into the thick paste that relative density is 1.35-1.40, and is for subsequent use;
C2. the Fructus Corni (processed) of Rhizoma Dioscoreae with proportional quantity 2/3rds mixed, be ground into fine powder, for subsequent use;
C3. with the thick paste of step c1 gained, the fine powder of step c2 gained and the volatile oil mixing of step a2 gained, pill, drying, polishing namely gets LIUWEI DIHUANG WAN.
Preferably, described step a3 adds in the medicinal residues first to be equivalent to Cortex Moutan weight 2-4 water doubly, is heated with stirring to 75-85 ℃, insulated and stirred 5-15 minute, with slip pump into diaphragm filter press carry out the membrane filter pressing To be equivalent to again Cortex Moutan weight 1-3 doubly be preheated to 75-85 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 is the extracting solution A that adds first step a3 gained, and add 6-9 that the water ad pond om is equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight doubly, wherein deduct Radix Rehmanniae Preparata added water yield (6-9 of the gross weight of the water that adds during the slurrying of extracting solution A+ Radix Rehmanniae Preparata+add water=step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight doubly) when slurrying, carry out the membrane filter pressing circulation first time and extract under 55-65 ℃ condition, extraction time is 30-40 minute; Add and be equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight 3-5 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 3 times of Cortex Moutan weight in medicinal residues, be heated with stirring to 80 ℃, insulated and stirred 10 minutes, with slip pump into diaphragm filter press carry out the membrane filter pressing To be equivalent to again 2 times of Cortex Moutan weight be preheated to 80 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 is the extracting solution A that adds first step a3 gained, and add the water ad pond om and be equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight 7.5 times, wherein deduct Radix Rehmanniae Preparata added water yield when slurrying, carry out the membrane filter pressing circulation first time and extract under 65 ℃ condition, extraction time is 35 minutes; Add the water be equivalent to step b1 gained medicated powder and 3.5 times of Radix Rehmanniae Preparata gross weights again, carry out the membrane filter pressing extraction that circulates second time 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 extracting 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, therefore 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 that decocting method extracts the 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, and the content of index components such as extractum (solid content), 50% methanolic extract and loganin all significantly increases; 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: extract the medical material of same weight, adopt decocting method to need 4 hours, and adopt the membrane filter pressing circulating extraction method to be no more than 1 hour, extraction time shortens more than 75%; And the inventive method has realized the integrated of circulation extraction and solid-liquid separation, do not have the worry of the existing follow-up solid-liquid separation of decocting method, and because the filter cloth of diaphragm filter press is ultimate attainment close, the clarity of gained extracting solution is good.(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 1.5 hours by 4 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 later use; 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 in the existing method Cortex Moutan is extracted medicinal residues and Fructus Corni behind the volatile oil, Radix Rehmanniae Preparata, Poria, Rhizoma Alismatis decocts with water, reach a few hours owing to extracting the process of volatile oil with the water azeotropic, during the water soluble ingredient of Cortex Moutan fully is soluble in the aqueous phase in the process of extracting volatile oil, therefore the inventive method no longer will be extracted medicinal residues and Fructus Corni behind the volatile oil, Radix Rehmanniae Preparata, Poria, Rhizoma Alismatis is fried in shallow oil altogether, and only with hot water medicinal residues are washed thoroughly, aqueous solution after washing liquid and the distillation merges thoroughly, as Fructus Corni, Radix Rehmanniae Preparata, Poria, the first extraction solvent of Rhizoma Alismatis is applied mechanically, and extracts solvent load to save, 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: Radix Rehmanniae Preparata 8kg, Fructus Corni (processed) 4kg, Cortex Moutan 3kg, Rhizoma Dioscoreae 4kg, Poria 3kg, Rhizoma Alismatis 3kg
Preparation method may further comprise the steps:
A. the extraction of Cortex Moutan
A1. the Cortex Moutan with recipe quantity is ground into coarse powder, and is 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 Cortex Moutan weight in the multi-function extractor that the Cortex Moutan medicinal residues are housed, 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 80 ℃ the water of being preheated to that is equivalent to 2 times of Cortex Moutan 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 Fructus Corni (processed), Radix Rehmanniae Preparata, Poria and Rhizoma Alismatis
B1. the Fructus Corni (processed) of recipe quantity 1/3rd and Poria, the Rhizoma Alismatis of recipe quantity are mixed, be ground into coarse powder, for subsequent use; The Radix Rehmanniae Preparata of recipe quantity is added the water of 3 times of weight, be ground into slip with the claw-disc type pulverizer, for subsequent use;
B2. add the extracting solution A of step a3 gained in the material-compound tank and add 7.5 times (noting therefrom deducting Radix Rehmanniae Preparata added water yield when slurrying) that the water ad pond om is equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight, be heated to 65 ℃ and be incubated; 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 and Radix Rehmanniae Preparata slip, 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 and Radix Rehmanniae Preparata gross weights 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 B;
C. preparation
C1. the extracting solution B with step b2 gained is concentrated into the thick paste that relative density is 1.35-1.40, and is for subsequent use;
C2. the Fructus Corni (processed) of recipe quantity 2/3rds and the Rhizoma Dioscoreae of recipe quantity are mixed, be ground into fine powder, for subsequent use;
C3. with the thick paste of step c1 gained, the fine powder of step c2 gained and the volatile oil mixing of step a2 gained, pill, drying, polishing namely gets LIUWEI DIHUANG WAN (concentrated pill).
Embodiment 2
Prescription: Radix Rehmanniae Preparata 8kg, Fructus Corni (processed) 4kg, Cortex Moutan 3kg, Rhizoma Dioscoreae 4kg, Poria 3kg, Rhizoma Alismatis 3kg
Preparation method may further comprise the steps:
A. the extraction of Cortex Moutan
A1. the Cortex Moutan with recipe quantity is ground into coarse powder, and is 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 Cortex Moutan weight in the multi-function extractor that the Cortex Moutan medicinal residues are housed, be heated with stirring to 85 ℃, 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 85 ℃ the water of being preheated to that is equivalent to 1 times of Cortex Moutan 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 Fructus Corni (processed), Radix Rehmanniae Preparata, Poria and Rhizoma Alismatis
B1. the Fructus Corni (processed) of recipe quantity 1/3rd and Poria, the Rhizoma Alismatis of recipe quantity are mixed, be ground into coarse powder, for subsequent use; The Radix Rehmanniae Preparata of recipe quantity is added the water of 2 times of weight, be ground into slip with the claw-disc type pulverizer, for subsequent use;
B2. add the extracting solution A of step a3 gained in the material-compound tank and add 6 times (noting therefrom deducting Radix Rehmanniae Preparata added water yield when slurrying) that the water ad pond om is equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight, be heated to 55 ℃ and be incubated; 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 and Radix Rehmanniae Preparata slip, 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, again three-way valve is switched to the material-compound tank position, add 55 ℃ the water of being preheated to that is equivalent to 5 times of step b1 gained medicated powder and Radix Rehmanniae Preparata gross weights 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. preparation
C1. the extracting solution B with step b2 gained is concentrated into the thick paste that relative density is 1.35-1.40, and is for subsequent use;
C2. the Fructus Corni (processed) of recipe quantity 2/3rds and the Rhizoma Dioscoreae of recipe quantity are mixed, be ground into fine powder, for subsequent use;
C3. with the thick paste of step c1 gained, the fine powder of step c2 gained and the volatile oil mixing of step a2 gained, pill, drying, polishing namely gets LIUWEI DIHUANG WAN (concentrated pill).
Embodiment 3
Prescription: Radix Rehmanniae Preparata 8kg, Fructus Corni (processed) 4kg, Cortex Moutan 3kg, Rhizoma Dioscoreae 4kg, Poria 3kg, Rhizoma Alismatis 3kg
Preparation method may further comprise the steps:
A. the extraction of Cortex Moutan
A1. the Cortex Moutan with recipe quantity is ground into coarse powder, and is 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 Cortex Moutan weight in the multi-function extractor that the Cortex Moutan medicinal residues are housed, 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 Cortex Moutan 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 Fructus Corni (processed), Radix Rehmanniae Preparata, Poria and Rhizoma Alismatis
B1. the Fructus Corni (processed) of recipe quantity 1/3rd and Poria, the Rhizoma Alismatis of recipe quantity are mixed, be ground into coarse powder, for subsequent use; The Radix Rehmanniae Preparata of recipe quantity is added the water of 4 times of weight, be ground into slip with the claw-disc type pulverizer, for subsequent use;
B2. add the extracting solution A of step a3 gained in the material-compound tank and add 9 times (noting therefrom deducting Radix Rehmanniae Preparata added water yield when slurrying) that the water ad pond om is equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight, be heated to 60 ℃ and be incubated; 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 and Radix Rehmanniae Preparata slip, 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, again three-way valve is switched to the material-compound tank position, add 60 ℃ the water of being preheated to that is equivalent to 3 times of step b1 gained medicated powder and Radix Rehmanniae Preparata gross weights 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. preparation
C1. the extracting solution B with step b2 gained is concentrated into the thick paste that relative density is 1.35-1.40, and is for subsequent use;
C2. the Fructus Corni (processed) of recipe quantity 2/3rds and the Rhizoma Dioscoreae of recipe quantity are mixed, be ground into fine powder, for subsequent use;
C3. with the thick paste of step c1 gained, the fine powder of step c2 gained and the volatile oil mixing of step a2 gained, pill, drying, polishing namely gets LIUWEI DIHUANG WAN (concentrated pill).
Employing is with a collection of medicinal raw material, adopt respectively the described method of embodiment 1-3 and existing method (the Sanitation Ministry medicine standard WS3-B-2102-96 records method) to compare experiment, 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 content of index components is higher.Wherein, the cost-effectiveness of embodiment 1 described method is than best, and the content of each index components sees the following form in the products obtained therefrom.
As seen from table: 1, compare with existing method, the content of extractum (solid content), 50% methanolic extract and the loganin of the inventive method extracted twice gained has improved respectively 13.57%, 16.0% and 12.55%, the amount that wherein comprises 50% methanolic extract of hydrophilic effective ingredient and lipotropy effective ingredient increases obviously, illustrates that the inventive method can improve the response rate of effective ingredient greatly; 2, the content of three indexs (extractum, 50% methanolic extract and loganin) is than the 2nd high 3.5-4 of extracting solution doubly in the 1st extracting solution of the inventive method gained, and the content of three indexs illustrates that only than the 2nd the high 20-36% of extracting solution the extraction efficiency of the inventive method is higher in existing the 1st extracting solution of method gained.
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 LIUWEI DIHUANG WAN, made by the crude drug of following weight proportioning: 60 parts of 160 parts of Radix Rehmanniae Preparata, 80 parts of Fructus Corni (processed)s, 60 parts of Cortex Moutans, 80 parts of Rhizoma Dioscoreaes, 60 parts in Poria and Rhizoma Alismatis, it is characterized in that, preparation method may further comprise the steps:
A. the extraction of Cortex Moutan
A1. Cortex Moutan is 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 60-90 ℃, 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 60-90 ℃ 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 Fructus Corni (processed), Radix Rehmanniae Preparata, Poria and Rhizoma Alismatis
B1. Poria, Rhizoma Alismatis are mixed with the Fructus Corni (processed) of proportional quantity 1/3rd, be ground into coarse powder, for subsequent use; Radix Rehmanniae Preparata is broken into slip with pigment, 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, the medicated powder and the Radix Rehmanniae Preparata slip that under stirring condition, add step b1 gained in the material-compound tank, 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. preparation
C1. the extracting solution B with step b2 gained is concentrated into the thick paste that relative density is 1.35-1.40, and is for subsequent use;
C2. the Fructus Corni (processed) of Rhizoma Dioscoreae with proportional quantity 2/3rds mixed, be ground into fine powder, for subsequent use;
C3. with the thick paste of step c1 gained, the fine powder of step c2 gained and the volatile oil mixing of step a2 gained, pill, drying, polishing namely gets LIUWEI DIHUANG WAN.
2. the preparation method of LIUWEI DIHUANG WAN according to claim 1, it is characterized in that, described step a3 adds in the medicinal residues first to be equivalent to Cortex Moutan weight 2-4 water doubly, is heated with stirring to 75-85 ℃, insulated and stirred 5-15 minute, slip is pumped into diaphragm filter press carry out membrane filter pressing To be equivalent to again Cortex Moutan weight 1-3 doubly be preheated to 75-85 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 is the extracting solution A that adds first step a3 gained, and add 6-9 that the water ad pond om is equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight doubly, wherein deduct Radix Rehmanniae Preparata added water yield when slurrying, carry out the membrane filter pressing circulation first time and extract under 55-65 ℃ condition, extraction time is 30-40 minute; Add and be equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight 3-5 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 LIUWEI DIHUANG WAN according to claim 2, it is characterized in that, described step a3 adds the water that is equivalent to 3 times of Cortex Moutan weight first in medicinal residues, be heated with stirring to 80 ℃, insulated and stirred 10 minutes pumps into diaphragm filter press with slip and carries out membrane filter pressing To be equivalent to again 2 times of Cortex Moutan weight be preheated to 80 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 is the extracting solution A that adds first step a3 gained, and add the water ad pond om and be equivalent to step b1 gained medicated powder and Radix Rehmanniae Preparata gross weight 7.5 times, wherein deduct Radix Rehmanniae Preparata added water yield when slurrying, carry out the membrane filter pressing circulation first time and extract under 65 ℃ condition, extraction time is 35 minutes; Add the water be equivalent to step b1 gained medicated powder and 3.5 times of Radix Rehmanniae Preparata gross weights again, carry out the membrane filter pressing extraction that circulates second time under 65 ℃ condition, extraction time is 15 minutes.
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| CN101129642A (en) * | 2007-07-16 | 2008-02-27 | 太极集团重庆中药二厂 | Method of preparing concentrated pill of six ingredients with rehmannia |
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| CN101129642A (en) * | 2007-07-16 | 2008-02-27 | 太极集团重庆中药二厂 | Method of preparing concentrated pill of six ingredients with rehmannia |
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| 中华人民共和国卫生部药典委员会编.六味地黄丸（浓缩丸）.《中华人民共和国卫生部药品标准中药成方制剂第十一册》.1996,第36页. * |
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| CN103349042A (en) * | 2013-06-08 | 2013-10-16 | 涡阳县丰华面业有限公司 | Rehmannia health care flour and preparation method thereof |
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