CN102293898B - Preparation method of rhizoma dioscoreae nipponicae bone spur tablet - Google Patents
Preparation method of rhizoma dioscoreae nipponicae bone spur tablet Download PDFInfo
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Abstract
The invention discloses a preparation method of a rhizoma dioscoreae nipponicae bone spur tablet. 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 a percolation 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, the consumption of ethanol as an extraction solvent can be reduced, 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
Record of Chinese Pharmacopoeia version in 2010: the Dioscorea nipponica bony spur tablet has the effect of reinforcing the kidney to strengthen the bone, promoting blood circulation and stopping pain, and clinical in the osteoarthritis due to the blood stasis due to renal deficiency, disease is seen arthralgia.Its prescription is Rhizoma Dioscoreae Nipponicae 270g, Herba Epimedii 324g, Rhizoma Cibotii 432g, Radix Cyathulae 432g, Radix Rehmanniae Preparata 270g, Fructus Lycii 162g.Its preparation method is that Rhizoma Dioscoreae Nipponicae is pulverized, and it is standby to get the 180g fine powder; Residue Rhizoma Dioscoreae Nipponicae powder is made solvent with 70% ethanol, carries out percolation, collects percolate 600ml, and reclaiming ethanol and being concentrated into relative density is 1.20-1.25(70 ℃); The five tastes such as all the other Herba Epimedii decoct with water three times, and collecting decoction filters, and it is 1.20-1.25(70 ℃ that filtrate is concentrated into relative density), merge with Dioscorea nipponica Mak. Ningpo Yam Rhizome extract, be concentrated in right amount, with Rhizoma Dioscoreae Nipponicae fine powder mixing, make granule, drying is pressed into 1000, namely.Adopt percolation and decocting method to extract the effective ingredient of prescription medical material in the said method respectively, have that technology is loaded down with trivial details, extraction time long, extract the temperature height, energy consumption height, thermal sensitivity composition easily lose, shortcomings such as 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 the Dioscorea nipponica bony spur tablet; not only can simplify technological process; 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 Dioscorea nipponica bony spur tablet, made by following raw materials by weight proportions: 162 parts of 270 parts of Rhizoma Dioscoreae Nipponicae, 324 parts of Herba Epimedii, 432 parts of Rhizoma Cibotii, 432 parts of Radix Cyathulaes, 270 parts of Radix Rehmanniae Preparata and Fructus Lycii may further comprise the steps:
A. the extraction of Rhizoma Dioscoreae Nipponicae
A1. the Rhizoma Dioscoreae Nipponicae with proportional quantity 1/3rd is ground into coarse powder, and is standby;
A2. in material-compound tank, add 60-70% ethanol; Three-way valve is switched to the material-compound tank position, 60-70% ethanol in the material-compound tank is pumped into diaphragm filter press, when passing back into material-compound tank to pressing filtering liquid, under stirring condition, in material-compound tank, add step a1 gained medicated powder, finish, carry out the membrane filter pressing circulation first time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, again three-way valve is switched to the material-compound tank position, in material-compound tank, add 60-70% ethanol, carry out the membrane filter pressing circulation second time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
B. the extraction of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii
B1. Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae and Fructus Lycii are mixed, be ground into coarse powder, standby; Radix Rehmanniae Preparata is added water, be ground into slip, standby;
B2. in material-compound tank, add water, 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 b1 gained medicated powder and Radix Rehmanniae Preparata slip, 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 finishes, again three-way valve is switched to the material-compound tank position, in material-compound tank, add water, 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 finishes, again three-way valve is switched to the material-compound tank position, in material-compound tank, add water, under 50-90 ℃ condition, carry out membrane filter pressing circulation for the third time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge three pressing filtering liquids and pressed liquor, be designated as extracting solution B;
C. preparation
The Rhizoma Dioscoreae Nipponicae of proportional quantity 2/3rds is ground into fine powder, standby; The extracting solution A of step a2 gained is reclaimed ethanol and is concentrated into 70 ℃ of relative densities the thick paste that is 1.20-1.25; With the extracting solution B of the step b2 gained thick paste that to be concentrated into 70 ℃ of relative densities be 1.20-1.25; Above-mentioned two kinds of thick pastes are merged, concentrate, with Rhizoma Dioscoreae Nipponicae fine powder mixing, make granule again, drying, tabletting namely gets the Dioscorea nipponica bony spur tablet.
Preferably, described step a2 adds earlier to be equivalent to Rhizoma Dioscoreae Nipponicae coarse powder weight 5-7 60% ethanol doubly, carries out the membrane filter pressing circulation first time and extracts, and extraction time is 30-40 minute; Add and be equivalent to Rhizoma Dioscoreae Nipponicae coarse powder weight 2-4 60% ethanol doubly, carry out the membrane filter pressing circulation second time and extract, extraction time is 10-20 minute;
Described step b1 adds the Radix Rehmanniae Preparata of recipe quantity to be equivalent to its weight 3-5 water doubly, is ground into slip, and is standby;
Described step b2 adds earlier to be equivalent to Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii 5 flavor medical material gross weight 6-8 water doubly, the added water yield when wherein deducting Radix Rehmanniae Preparata 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 above-mentioned 5 flavor medical material 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; Add and be equivalent to above-mentioned 5 flavor medical material gross weight 2-4 water doubly, carry out membrane filter pressing circulation for the third time and extract under 55-65 ℃ condition, extraction time is 10-20 minute.
Preferred, described step a2 adds 60% ethanol that is equivalent to 5 times of Rhizoma Dioscoreae Nipponicae coarse powder weight earlier, carries out the membrane filter pressing circulation first time and extracts, and extraction time is 30 minutes; Add 60% ethanol that is equivalent to 3 times of Rhizoma Dioscoreae Nipponicae coarse powder weight again, carry out the membrane filter pressing circulation second time and extract, extraction time is 15 minutes;
Described step b1 is the water that the Radix Rehmanniae Preparata adding of recipe quantity is equivalent to 4 times of its weight, is ground into slip, and is standby;
Described step b2 adds earlier the water that is equivalent to 7 times of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii 5 flavor medical material gross weights, the added water yield when wherein deducting Radix Rehmanniae Preparata slurrying, carry out the membrane filter pressing circulation first time and extract under 65 ℃ condition, extraction time is 30 minutes; Add the water that is equivalent to 4 times of above-mentioned 5 flavor medical material gross weights again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 15 minutes; Add the water that is equivalent to 3 times of above-mentioned 5 flavor medical material gross weights again, carry out membrane filter pressing circulation for the third time and extract under 65 ℃ condition, extraction time is 10 minutes.
Preferably, also comprise step a3 after the described step a2: three-way valve is switched to the material-compound tank position, in material-compound tank, add water, carry out the membrane filter pressing circulation and wash thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, measure ethanol content, extract preparing solvent liquid as the next group Rhizoma Dioscoreae Nipponicae.
Preferred, described step a3 adds to be equivalent to Rhizoma Dioscoreae Nipponicae coarse powder weight 2-3 water doubly, and the membrane filter pressing circulation was washed 3-7 minute thoroughly.
The isolation integral technology is extracted in membrane filter pressing circulation of the present invention, be that the discharging opening of material-compound tank is communicated with the charging aperture of diaphragm filter press by pump (as membrane pump etc.), the liquid outlet of diaphragm filter press is communicated with the import of charging aperture and the filtrate tank of material-compound tank respectively with three-way valve.When three-way valve switches to the material-compound tank position, the liquid outlet of diaphragm filter press is communicated with the charging aperture of material-compound tank, constitute membrane filter pressing circulation extraction system, slip in the material-compound tank is pumped to diaphragm filter press to carry out the pressing filtering liquid that membrane filter pressing comes out from diaphragm filter press and passes back into (medicated powder then is deposited on the filter cloth surface of each filter pressing chamber of diaphragm filter press equably) the material-compound tank, be re-used as and extract solvent and be pumped to diaphragm filter press and carry out membrane filter pressing and constantly circulate, thereby the membrane filter pressing circulation that realizes medical material is extracted; When three-way valve switches to the filtrate tank position, the liquid outlet of diaphragm filter press is communicated with the import of filtrate tank, constitute the membrane filter pressing solid-liquid separation system, after the membrane filter pressing circulation extraction of medical material finishes, to send into the filtrate tank storage from pressing filtering liquid and pressed liquor that diaphragm filter press comes out, thereby herbal extract is well separated with medicinal residues.
About extracting the problem of material, usually pulverizing medicinal materials is become coarse powder as extracting material, the soft medical material (as Radix Rehmanniae Preparata, Fructus Jujubae etc.) that difficulty is ground into coarse powder can add the water that 2-4 doubly measures and be ground into slip as extracting material with feed grinder or tissue mashing machine.
About the problem of charging sequence, when the medical material fibre-bearing more after a little while, can be in material-compound tank directly add medicated powder and extract solvent, under stirring condition, carry out the membrane filter pressing circulation and extract; When the medical material fibre rich, then should adopt the outer circulation method of feeding in raw material, to stop that medicated powder stops up in material-compound tank discharging opening and feeding pipe and phenomenon that the stock circulation is obstructed.The reinforced method of so-called outer circulation is will extract required whole solvents earlier first to add in the material-compound tank, three-way valve is switched to the material-compound tank position, solvent is pumped into diaphragm filter press, (can observe from the manhole of material-compound tank) when passing back into material-compound tank when observing pressing filtering liquid (this moment is actual to be solvent), under stirring condition, progressively drop into medicated powder again, the gained feed liquid is pumped to diaphragm filter press thereupon carries out the membrane filter pressing pressing filtering liquid and passes back in the material-compound tank and circulate, and medicated powder then is deposited on the filter cloth surface of each filter pressing chamber of diaphragm filter press equably.
About extracting the problem of temperature, when being solvent with water, extracting temperature can control at 50-90 ℃, according to polarized light microscopy method measurement result and in conjunction with bibliographical information, starch gelatinization temperature in the plant tissue mostly is 70-71 ℃, for fear of occurring because starch gelatinization blocks cell inclusion (mostly being effective ingredient) stripping or stops up phenomenons such as filter cloth, the medical material of rich in starch is carried out water when carrying, extract temperature and should control below 70 ℃, preferred 55-65 ℃.And when adopting organic solvent extraction, the boiling point height of looking organic solvent can not heat (namely at room temperature extracting) or suitably heating.
About the problem of extraction time and extraction time, can require according to the response rate of index components and economy requirement suitable adjustment extraction time and extraction time.For the extraction of general medicinal material coarse powder, but selective extraction 2 times extracted 30-40 minute for the 1st time, extracted 10-20 minute for the 2nd time; Higher for price of medicinal material, require the higher kind of the index components response rate, extraction time can suitably increase, as extracts 4 times, extracts the 2-4 time extraction 10-20 minute 40-60 minute the 1st time; Also last 1 time extracting solution can be carried out recycled as the solvent of extraction first of next group material.When serving as when extracting solvent with alcohol-water mixed solution, carry out membrane filter pressing and wash and squeeze medicinal residues thoroughly in the extraction back available water that finishes, after gained pressing filtering liquid and pressed liquor are measured pure content, can be used as the next group material and extract preparing solvent liquid and carry out recycled.Carry out membrane filter pressing when washing thoroughly at water, also can close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, water is fully soaked overflow the top filtering layer, to strengthen washing effect.
Need to extract earlier volatile oil about part medical material in the compound preparation prescription, medicinal residues merge the problem of carrying out decocting with other medical material again, reach a few hours owing to extract the process of volatile oil with the water azeotropic, during the water soluble ingredient of medical material fully is soluble in the aqueous phase in the process of extracting volatile oil, so generally do not need medicinal residues and the merging of other medical material are carried out decocting, and save follow-up concentrated energy consumption simultaneously for the response rate that guarantees effective ingredient, can be after extracting volatile oil, the water of doubly measuring with 2-4 is heated to the 60-90 ℃ of saturating wash slag of membrane filter pressing, wash 1-2 time thoroughly, aqueous solution after the saturating washing liquid of gained and the distillation merges, as the extraction solvent of water first of other medical material.
About the problem of diaphragm filter press, filter cloth should be selected polypropylene multifilament filter cloth for use, and its Air permenbility selection principle is: less (as 3-10L/m with the appropriate to the occasion Air permenbility of selecting for use of organic solvent extraction
2.s) filter cloth is big (as 50-1200L/m with the appropriate to the occasion Air permenbility of selecting for use of water extraction
2.s) filter cloth.Membrane filter plate should select polypropylene etc. to meet the plastic material of medicinal requirements.The feed liquid pipeline should be selected the plastic conduit of 304 above rustless steels or non-PVC for use.
In the present invention, percentage ratio means the ratio of weight with " % " symbolic representation; But the percentage ratio of solution except as otherwise herein provided, means and contains the some grams of solute among the solution 100ml; The percentage ratio of ethanol means percent by volume, contains the some milliliters of ethanol among the ie in solution 100ml.
Beneficial effect of the present invention is: (1) has improved the response rate of effective ingredient: the present invention adopts the membrane filter pressing circulating extraction method to substitute the effective ingredient of percolation and decocting method extraction prescription medical material, this method system adopts the pressure-driven of 0.5-0.6Mpa, circulation is extracted and is piled up in hundreds of the powder beds on the eluting face, effect with pressurized column chromatography or pressurization percolation, extraction efficiency significantly improves, the extraction temperature reduces, the loss of thermal sensitivity composition reduces, the response rate of index components significantly improves, for example, Herba Epimedii index components content Determination of Icariin improves about 27% than decocting method, the response rate of Rhizoma Dioscoreae Nipponicae index components dioscin improves about 32% than percolation; And the filter cloth aperture of adopting because of diaphragm filter press is far below being used for the filter screen aperture that medicinal residues separate with decocting liquid at present, and gained extracting solution clarity is good, and naked eyes visible particle thing can not enter in the finished product, has also correspondingly improved the content of active ingredient in the finished product.(2) reduced the consumption that extracts etoh solvent: the inventive method can substitute 70% ethanol extraction Rhizoma Dioscoreae Nipponicae of existing method with 60% ethanol, and the ethanol consumption reduces, but the content of index components increases on the contrary.(3) simplified technological process, shortened the production cycle: extract the prescription medical material of same weight, adopt existing percolation or decocting method to be not less than 5 hours, and adopt the membrane filter pressing circulating extraction method to be no more than 1.5 hours, extraction time shortens more than 70%; 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.(4) energy savings: with 1m
3Water is heated to 55-65 ℃ from 20 ℃ and needs raw coal 18.4-21.7kg, needs raw coal 37.6kg and be heated to 98 ℃, and 42-51% on year-on-year basis lowers consumption; The extraction time of prescription medical material foreshortened to 1.5 hours by 5 hours, and the extraction energy consumption is reduced greatly.(5) be beneficial to environmental conservation and waste residue utilization: the medicinal residues after the isolation integral technical finesse is extracted in the membrane filter pressing circulation are the nearly powdered form block of doing; water content is few; not only be convenient to transhipment; can not pollute to environment; and be convenient to the later use of waste residue; as insert in the coal dust burning with reduce the coal consumption, biofermentation is made feedstuff, dry distilling is made as the charcoal piece and makes heating or domestic fuel etc.
Description of drawings
Fig. 1 extracts the preferred corollary apparatus figure of isolation integral technology for the membrane filter pressing circulation.
The specific embodiment
In order to make the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing the preferred embodiments of the present invention are described in detail.
The preferred corollary apparatus figure of membrane filter pressing circulation extraction isolation integral technology as shown in Figure 1, the discharging opening of material-compound tank is communicated with the charging aperture of diaphragm filter press by membrane pump, the liquid outlet of diaphragm filter press is communicated with the import of charging aperture and the filtrate tank of material-compound tank respectively with three-way valve, when three-way valve switches to the material-compound tank position, the liquid outlet of diaphragm filter press is communicated with the charging aperture of material-compound tank, the pressing filtering liquid that comes out from diaphragm filter press passes back into material-compound tank, constitutes membrane filter pressing circulation extraction system; When three-way valve switched to the filtrate tank position, the liquid outlet of diaphragm filter press was communicated with the import of filtrate tank, and the pressing filtering liquid that comes out from diaphragm filter press enters the filtrate tank storage, constitutes the membrane filter pressing solid-liquid separation system.
Embodiment 1
Prescription: Rhizoma Dioscoreae Nipponicae 2.7kg, Herba Epimedii 3.24kg, Rhizoma Cibotii 4.32kg, Radix Cyathulae 4.32kg, Radix Rehmanniae Preparata 2.7kg, Fructus Lycii 1.62kg
Preparation method may further comprise the steps:
A. the extraction of Rhizoma Dioscoreae Nipponicae
A1. the Rhizoma Dioscoreae Nipponicae with recipe quantity 1/3rd is ground into coarse powder, and is standby;
A2. in material-compound tank, add 60% ethanol that is equivalent to 5 times of Rhizoma Dioscoreae Nipponicae coarse powder weight; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, 60% ethanol in the material-compound tank is pumped into diaphragm filter press (adopt 5-8 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, at the uniform velocity add step a1 gained medicated powder in material-compound tank, finish, the membrane filter pressing circulation was extracted 30 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position again, add 60% ethanol that is equivalent to 3 times of Rhizoma Dioscoreae Nipponicae coarse powder weight in material-compound tank, the membrane filter pressing circulation 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 finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. three-way valve is switched to the material-compound tank position, in material-compound tank, add the water that is equivalent to 3 times of Rhizoma Dioscoreae Nipponicae coarse powder weight, close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, the membrane filter pressing circulation was washed 5 minutes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge pressing filtering liquid and pressed liquor, measure ethanol content, extract preparing solvent liquid as the next group Rhizoma Dioscoreae Nipponicae;
B. the extraction of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii
B1. Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae and the Fructus Lycii with recipe quantity mixes, and is ground into coarse powder, and be standby; The Radix Rehmanniae Preparata of recipe quantity is added the water that is equivalent to 4 times of its weight, be ground into slip, standby;
B2. add the water (the added water yield during slurrying of deduction Radix Rehmanniae Preparata) that is equivalent to 7 times of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii 5 flavor medical material gross weights in the material-compound tank, 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 and Radix Rehmanniae Preparata slip, finish, 65 ℃ 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 finishes, three-way valve is switched to the material-compound tank position again, add 65 ℃ the water of being preheated to that is equivalent to 4 times of above-mentioned 5 flavor medical material 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 finishes, 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 above-mentioned 5 flavor medical material 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 finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge three pressing filtering liquids and pressed liquor, be designated as extracting solution B;
C. preparation
The Rhizoma Dioscoreae Nipponicae of recipe quantity 2/3rds is ground into fine powder, standby; The extracting solution A of step a2 gained is reclaimed ethanol and is concentrated into 70 ℃ of relative densities the thick paste that is 1.20-1.25; With the extracting solution B of the step b2 gained thick paste that to be concentrated into 70 ℃ of relative densities be 1.20-1.25; Above-mentioned two kinds of thick pastes are merged, concentrate, with Rhizoma Dioscoreae Nipponicae fine powder mixing, make granule again, drying is pressed into 10000, namely gets the Dioscorea nipponica bony spur tablet.
Embodiment 2
Prescription: Rhizoma Dioscoreae Nipponicae 2.7kg, Herba Epimedii 3.24kg, Rhizoma Cibotii 4.32kg, Radix Cyathulae 4.32kg, Radix Rehmanniae Preparata 2.7kg, Fructus Lycii 1.62kg
Preparation method may further comprise the steps:
A. the extraction of Rhizoma Dioscoreae Nipponicae
A1. the Rhizoma Dioscoreae Nipponicae with recipe quantity 1/3rd is ground into coarse powder, and is standby;
A2. in material-compound tank, add 60% ethanol that is equivalent to 6 times of Rhizoma Dioscoreae Nipponicae coarse powder weight; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, 60% ethanol in the material-compound tank is pumped into diaphragm filter press (adopt 5-8 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, at the uniform velocity add step a1 gained medicated powder in material-compound tank, finish, the membrane filter pressing circulation was extracted 40 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position again, add 60% ethanol that is equivalent to 4 times of Rhizoma Dioscoreae Nipponicae coarse powder weight in material-compound tank, the membrane filter pressing circulation 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 finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. three-way valve is switched to the material-compound tank position, in material-compound tank, add the water that is equivalent to 2 times of Rhizoma Dioscoreae Nipponicae coarse powder weight, close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, the membrane filter pressing circulation was washed 3 minutes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge pressing filtering liquid and pressed liquor, measure ethanol content, extract preparing solvent liquid as the next group Rhizoma Dioscoreae Nipponicae;
B. the extraction of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii
B1. Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae and the Fructus Lycii with recipe quantity mixes, and is ground into coarse powder, and be standby; The Radix Rehmanniae Preparata of recipe quantity is added the water that is equivalent to 3 times of its weight, be ground into slip, standby;
B2. add the water (the added water yield during slurrying of deduction Radix Rehmanniae Preparata) that is equivalent to 6 times of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii 5 flavor medical material gross weights in the material-compound tank, 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 and Radix Rehmanniae Preparata slip, finish, 60 ℃ 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 finishes, three-way valve is switched to the material-compound tank position again, add 60 ℃ the water of being preheated to that is equivalent to 5 times of above-mentioned 5 flavor medical material 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 finishes, three-way valve is switched to the material-compound tank position again, add 60 ℃ the water of being preheated to that is equivalent to 4 times of above-mentioned 5 flavor medical material 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 finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge three pressing filtering liquids and pressed liquor, be designated as extracting solution B;
C. preparation
The Rhizoma Dioscoreae Nipponicae of recipe quantity 2/3rds is ground into fine powder, standby; The extracting solution A of step a2 gained is reclaimed ethanol and is concentrated into 70 ℃ of relative densities the thick paste that is 1.20-1.25; With the extracting solution B of the step b2 gained thick paste that to be concentrated into 70 ℃ of relative densities be 1.20-1.25; Above-mentioned two kinds of thick pastes are merged, concentrate, with Rhizoma Dioscoreae Nipponicae fine powder mixing, make granule again, drying is pressed into 10000, namely gets the Dioscorea nipponica bony spur tablet.
Embodiment 3
Prescription: Rhizoma Dioscoreae Nipponicae 2.7kg, Herba Epimedii 3.24kg, Rhizoma Cibotii 4.32kg, Radix Cyathulae 4.32kg, Radix Rehmanniae Preparata 2.7kg, Fructus Lycii 1.62kg
Preparation method may further comprise the steps:
A. the extraction of Rhizoma Dioscoreae Nipponicae
A1. the Rhizoma Dioscoreae Nipponicae with recipe quantity 1/3rd is ground into coarse powder, and is standby;
A2. in material-compound tank, add 60% ethanol that is equivalent to 7 times of Rhizoma Dioscoreae Nipponicae coarse powder weight; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, 60% ethanol in the material-compound tank is pumped into diaphragm filter press (adopt 5-8 L/m
2.s polypropylene multifilament filter cloth), when passing back into material-compound tank to pressing filtering liquid, at the uniform velocity add step a1 gained medicated powder in material-compound tank, finish, the membrane filter pressing circulation was extracted 35 minutes, afterwards three-way valve was switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position again, add 60% ethanol that is equivalent to 2 times of Rhizoma Dioscoreae Nipponicae coarse powder weight in material-compound tank, the membrane filter pressing circulation 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 finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
A3. three-way valve is switched to the material-compound tank position, in material-compound tank, add the water that is equivalent to 3 times of Rhizoma Dioscoreae Nipponicae coarse powder weight, close two liquid valves that are in low level in four jiaos of liquid valves of diaphragm filter press, the membrane filter pressing circulation was washed 7 minutes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge pressing filtering liquid and pressed liquor, measure ethanol content, extract preparing solvent liquid as the next group Rhizoma Dioscoreae Nipponicae;
B. the extraction of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii
B1. Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae and the Fructus Lycii with recipe quantity mixes, and is ground into coarse powder, and be standby; The Radix Rehmanniae Preparata of recipe quantity is added the water that is equivalent to 2 times of its weight, be ground into slip, standby;
B2. add the water (the added water yield during slurrying of deduction Radix Rehmanniae Preparata) that is equivalent to 8 times of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii 5 flavor medical material gross weights in the material-compound tank, 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 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 finishes, three-way valve is switched to the material-compound tank position again, add 55 ℃ the water of being preheated to that is equivalent to 3 times of above-mentioned 5 flavor medical material 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 finishes, three-way valve is switched to the material-compound tank position again, add 55 ℃ the water of being preheated to that is equivalent to 2 times of above-mentioned 5 flavor medical material 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 finishes, start the squeezing program of diaphragm filter press, collect pressed liquor, last release is opened plate, slag dumping; Merge three pressing filtering liquids and pressed liquor, be designated as extracting solution B;
C. preparation
The Rhizoma Dioscoreae Nipponicae of recipe quantity 2/3rds is ground into fine powder, standby; The extracting solution A of step a2 gained is reclaimed ethanol and is concentrated into 70 ℃ of relative densities the thick paste that is 1.20-1.25; With the extracting solution B of the step b2 gained thick paste that to be concentrated into 70 ℃ of relative densities be 1.20-1.25; Above-mentioned two kinds of thick pastes are merged, concentrate, with Rhizoma Dioscoreae Nipponicae fine powder mixing, make granule again, drying is pressed into 10000, namely gets the Dioscorea nipponica bony spur tablet.
Employing is with a collection of medicinal raw material, adopt the described method of embodiment 1-3 and existing method (Chinese Pharmacopoeia one one of version in 2010 is recorded method) to compare experiment respectively, and products obtained therefrom carried out quality inspection, the result shows: the product that adopts the described method of embodiment 1-3 to make all meets the requirement of quality standard, and the response rate of index components is higher.Wherein, the cost-effectiveness of embodiment 1 described method is than best, and the index components content Determination of Icariin improves approximately 27% in the products obtained therefrom than decocting method, and the content of dioscin improves about 32% than percolation.
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 (5)
1. the preparation method of Dioscorea nipponica bony spur tablet, made by following raw materials by weight proportions: 162 parts of 270 parts of Rhizoma Dioscoreae Nipponicae, 324 parts of Herba Epimedii, 432 parts of Rhizoma Cibotii, 432 parts of Radix Cyathulaes, 270 parts of Radix Rehmanniae Preparata and Fructus Lycii, it is characterized in that, may further comprise the steps:
A. the extraction of Rhizoma Dioscoreae Nipponicae
A1. the Rhizoma Dioscoreae Nipponicae with proportional quantity 1/3rd is ground into coarse powder, and is standby;
A2. adding concentration of volume percent in the material-compound tank is the ethanol of 60-70%; Three-way valve is switched to the material-compound tank position, be that the ethanol of 60-70% pumps into diaphragm filter press with the concentration of volume percent in the material-compound tank, when passing back into material-compound tank to pressing filtering liquid, under stirring condition, in material-compound tank, add step a1 gained medicated powder, finish, carry out the membrane filter pressing circulation first time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position, adding concentration of volume percent in the material-compound tank is the ethanol of 60-70% again, carries out membrane filter pressing circulation extraction second time, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge twice pressing filtering liquid and pressed liquor, be designated as extracting solution A;
B. the extraction of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii
B1. Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae and Fructus Lycii are mixed, be ground into coarse powder, standby; Radix Rehmanniae Preparata is added water, be ground into slip, standby;
B2. in material-compound tank, add water, 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 b1 gained medicated powder and Radix Rehmanniae Preparata slip, 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 finishes, again three-way valve is switched to the material-compound tank position, in material-compound tank, add water, 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 finishes, again three-way valve is switched to the material-compound tank position, in material-compound tank, add water, under 50-90 ℃ condition, carry out membrane filter pressing circulation for the third time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge three pressing filtering liquids and pressed liquor, be designated as extracting solution B;
C. preparation
The Rhizoma Dioscoreae Nipponicae of proportional quantity 2/3rds is ground into fine powder, standby; The extracting solution A of step a2 gained is reclaimed ethanol and is concentrated into 70 ℃ of relative densities the thick paste that is 1.20-1.25; With the extracting solution B of the step b2 gained thick paste that to be concentrated into 70 ℃ of relative densities be 1.20-1.25; Above-mentioned two kinds of thick pastes are merged, concentrate, with Rhizoma Dioscoreae Nipponicae fine powder mixing, make granule again, drying, tabletting namely gets the Dioscorea nipponica bony spur tablet.
2. the preparation method of Dioscorea nipponica bony spur tablet according to claim 1, it is characterized in that, described step a2 adds earlier that to be equivalent to Rhizoma Dioscoreae Nipponicae coarse powder weight 5-7 concentration of volume percent doubly be 60% ethanol, carries out membrane filter pressing circulation extraction first time, and extraction time is 30-40 minute; Adding and being equivalent to Rhizoma Dioscoreae Nipponicae coarse powder weight 2-4 concentration of volume percent doubly is 60% ethanol, carries out membrane filter pressing circulation extraction second time, and extraction time is 10-20 minute;
Described step b1 adds the Radix Rehmanniae Preparata of recipe quantity to be equivalent to its weight 3-5 water doubly, is ground into slip, and is standby;
Described step b2 adds earlier to be equivalent to Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii 5 flavor medical material gross weight 6-8 water doubly, the added water yield when wherein deducting Radix Rehmanniae Preparata 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 above-mentioned 5 flavor medical material 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; Add and be equivalent to above-mentioned 5 flavor medical material gross weight 2-4 water doubly, carry out membrane filter pressing circulation for the third time and extract under 55-65 ℃ condition, extraction time is 10-20 minute.
3. the preparation method of Dioscorea nipponica bony spur tablet according to claim 2, it is characterized in that, described step a2 is that to add earlier the concentration of volume percent that is equivalent to 5 times of Rhizoma Dioscoreae Nipponicae coarse powder weight be 60% ethanol, carries out membrane filter pressing circulation extraction first time, and extraction time is 30 minutes; Add the concentration of volume percent be equivalent to 3 times of Rhizoma Dioscoreae Nipponicae coarse powder weight again and be 60% ethanol, carry out membrane filter pressing circulation extraction second time, extraction time is 15 minutes;
Described step b1 is the water that the Radix Rehmanniae Preparata adding of recipe quantity is equivalent to 4 times of its weight, is ground into slip, and is standby;
Described step b2 adds earlier the water that is equivalent to 7 times of Herba Epimedii, Rhizoma Cibotii, Radix Cyathulae, Radix Rehmanniae Preparata and Fructus Lycii 5 flavor medical material gross weights, the added water yield when wherein deducting Radix Rehmanniae Preparata slurrying, carry out the membrane filter pressing circulation first time and extract under 65 ℃ condition, extraction time is 30 minutes; Add the water that is equivalent to 4 times of above-mentioned 5 flavor medical material gross weights again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 15 minutes; Add the water that is equivalent to 3 times of above-mentioned 5 flavor medical material gross weights again, carry out membrane filter pressing circulation for the third time and extract under 65 ℃ condition, extraction time is 10 minutes.
4. according to the preparation method of the described Dioscorea nipponica bony spur tablet of the arbitrary claim of claim 1 to 3, it is characterized in that, also comprise step a3 after the described step a2: three-way valve is switched to the material-compound tank position, in material-compound tank, add water, carrying out the membrane filter pressing circulation washes thoroughly, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge pressing filtering liquid and pressed liquor, measure ethanol content, extract preparing solvent liquid as the next group Rhizoma Dioscoreae Nipponicae.
5. the preparation method of Dioscorea nipponica bony spur tablet according to claim 4 is characterized in that, described step a3 adds to be equivalent to Rhizoma Dioscoreae Nipponicae coarse powder weight 2-3 water doubly, and the membrane filter pressing circulation was washed 3-7 minute thoroughly.
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| 国家药典委员.穿龙骨刺片.《中华人民共和国药典2010年版第一部》.2010,第965页[处方][制法]项下. * |
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