CN102247476B - Method for preparing nine immortal extract - Google Patents
Method for preparing nine immortal extract Download PDFInfo
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- CN102247476B CN102247476B CN2011102477628A CN201110247762A CN102247476B CN 102247476 B CN102247476 B CN 102247476B CN 2011102477628 A CN2011102477628 A CN 2011102477628A CN 201110247762 A CN201110247762 A CN 201110247762A CN 102247476 B CN102247476 B CN 102247476B
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Abstract
The invention discloses a method for preparing nine immortal extract. Active ingredients of prescription drugs are extracted by adopting a diaphragm filter pressing circular extraction and separation integrated technology, thus a technological process is simplified, production period is greatly shortened, energy consumption is reduced, environmental protection and waste residue utilization can be conveniently realized, and recovery rate of the active ingredients can be greatly improved.
Description
Technical field
The invention belongs to pharmaceutical field, relate to a kind of method for preparing of Chinese medicine preparation.
Background technology
State Food and Drug Administration's standard (trying) WS-11376 (ZD-1376)-2002 record: Notopterygii Bolus of Nine Ingredients have induce sweat, the effect of cold expelling, dehumidifying, be used for affection of exogenous wind-cold and hold under the arm and wetly cause fever with aversion to cold lossless, headache and heavy, limb aching pain.Its prescription by Rhizoma Et Radix Notopterygii 300g, windproof 300g, Rhizoma Atractylodis 300g, Herba Asari 100g, Rhizoma Chuanxiong 200g, Radix Angelicae Dahuricae 200g, Radix Scutellariae 200g, Radix Glycyrrhizae 200g and Radix Rehmanniae 200g totally nine the flavor medicines form, process 1000g altogether.Its preparation method is with Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari, Rhizoma Chuanxiong distillating extracting oil, and the medicinal liquid after distillation device is in addition preserved, and adds the Radix Angelicae Dahuricae after the medicinal residues drying and is ground into fine powder, sieves; Fine powder is subsequent use, the medicinal liquid decocte with water after the three flavor adding distillations such as residue coarse powder and all the other Radix Scutellariaes three times, each 1 hour, collecting decoction; Filter, filtrating is concentrated into the clear paste that relative density is 1.03-1.05 (70 ℃), with the general ball of above-mentioned fine powder, drying; Put coldly, spray into volatile oil, mixing promptly gets.Adopt decocting method to extract the effective ingredient of part medical material in the said method, have long, shortcomings such as the extraction temperature is high, energy consumption is high, the thermal sensitivity composition is prone to loss, the effective ingredient response rate is low, post processing trouble of extraction time.
Summary of the invention
In view of this; The object of the present invention is to provide a kind of method of utilizing membrane filter pressing circulation extraction isolation integral technology to prepare Notopterygii Bolus of Nine Ingredients; 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 present invention provides following technical scheme:
The method for preparing of Notopterygii Bolus of Nine Ingredients; Process by following raw materials by weight proportions: 200 parts of 300 parts of Rhizoma Et Radix Notopterygiis, windproof 300 parts, 300 parts of Rhizoma Atractylodis, 100 parts of Herba Asaris, 200 parts of Rhizoma Chuanxiongs, 200 parts of the Radixs Angelicae Dahuricae, 200 parts of Radix Scutellariaes, 200 parts in Radix Glycyrrhizae and Radix Rehmanniae, method for preparing may further comprise the steps:
A. the extraction of Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong
A1. Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong are mixed, be ground into coarse powder, subsequent use;
A2. the medicated powder with step a1 gained extracts volatile oil with steam distillation, and the aqueous solution after medicinal residues and the distillation is 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 finishes, will be preheated to 60-90 ℃ water again and pump into diaphragm filter press 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; Aqueous solution after the distillation of twice pressing filtering liquid, pressed liquor and step a2 gained is merged, be designated as extracting solution A;
A4. the medicinal residues after step a3 being handled are dry, mix with the Radix Angelicae Dahuricae, pulverize, and sieve, and collect fine powder and remaining coarse powder respectively, and are subsequent use;
B. the extraction of Radix Scutellariae, Radix Glycyrrhizae and Radix Rehmanniae
B1. Radix Scutellariae, Radix Glycyrrhizae and Radix Rehmanniae are mixed, be ground into coarse powder, subsequent use;
B2. the coarse powder with step a4 gained mixes with Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae coarse powder of step b1 gained, and is subsequent use;
B3. in material-compound tank, add the extracting solution A and the water of step a3 gained, 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 pressing filtering liquid passes back into material-compound tank, under stirring condition, in material-compound tank, add the medicated powder of step b2 gained; Finish; Under 50-90 ℃ condition, carry out the membrane filter pressing circulation extraction first 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, 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 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 B;
C. preparation
C1. the extracting solution B concentrating under reduced pressure with step b3 gained becomes 70 ℃ of relative densities to be the clear paste of 1.03-1.05, and is subsequent use;
C2. with the clear paste of step c1 gained and the general ball of fine powder of step a4 gained, drying is put coldly, sprays into the volatile oil of step a2 gained, and mixing promptly gets Notopterygii Bolus of Nine Ingredients.
Preferably, said step a3 adds earlier to be equivalent to step a1 gained medicated powder weight 2-4 water doubly in medicinal residues, 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 step a1 gained medicated powder weight 1-3 doubly be preheated to 75-85 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Said step b3 is the extracting solution A that adds earlier step a3 gained, adds 6-9 that the water ad pond om is equivalent to step b2 gained medicated powder weight more doubly, under 55-65 ℃ condition, carries out the membrane filter pressing circulation extraction first time, and extraction time is 30-40 minute; Add and be equivalent to step b2 gained medicated powder weight 3-5 water doubly, under 55-65 ℃ condition, carry out the membrane filter pressing circulation extraction second time, extraction time is 10-20 minute.
Preferred, said step a3 adds earlier the water that is equivalent to 4 times of step a1 gained medicated powder 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 step a1 gained medicated powder weight be preheated to 80 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Said step b3 is the extracting solution A that adds earlier step a3 gained, adds the water ad pond om again and is equivalent to 7.5 times of step b2 gained medicated powder weight, under 65 ℃ condition, carries out the membrane filter pressing circulation extraction first time, and extraction time is 35 minutes; Add the water that is equivalent to 3.5 times of step b2 gained medicated powder weight again, under 65 ℃ condition, carry out the membrane filter pressing circulation extraction second time, extraction time is 20 minutes.
Membrane filter pressing circulation extraction isolation integral technology of the present invention; Be that the discharging opening of material-compound tank is communicated with the charging aperture of diaphragm filter press through pump (like membrane pump etc.), the liquid outlet of diaphragm filter press is communicated with the import of the 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 and carries out membrane filter pressing, and the pressing filtering liquid that comes out from diaphragm filter press 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, remakes to extracting solvent to be pumped to diaphragm filter press and to carry out membrane filter pressing and constantly circulate, thereby realizes the membrane filter pressing circulation extraction of medical material; 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, will 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, become coarse powder as extracting material pulverizing medicinal materials usually, the soft medical material (like 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 extraction; 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 actual for 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 into and circulate in the material-compound tank, 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, extracting temperature and can be controlled at 50-90 ℃ with water; Measure the result and combine bibliographical information according to the polarized light microscopy method; Mostly starch gelatinization temperature in the plant tissue is 70-71 ℃, for fear of occurring because of starch gelatinization blocks cell inclusion (being mostly 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 be controlled at below 70 ℃, preferred 55-65 ℃.And when adopting organic solvent extraction, the boiling point height of looking organic solvent can not heat (promptly 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 can last 1 time extracting solution 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 next group material extraction 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 thoroughly 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, because the process of extracting volatile oil with the water azeotropic reaches several hours; During the water soluble ingredient of medical material fully is soluble in the aqueous phase in the process of extracting volatile oil; Do not carry out decocting so generally need medicinal residues and other medical material not merged, and practice thrift follow-up concentrated energy consumption simultaneously for the response rate that guarantees effective ingredient, can be behind extraction volatile oil; The water of doubly measuring with 2-4 is heated to 60-90 ℃ of membrane filter pressing and passes through the wash slag; Wash 1-2 time thoroughly, the aqueous solution after gained passes through washing liquid and distills 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 (like 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 (like 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.
Beneficial effect of the present invention is: the response rate of effective ingredient has been improved in (1): the present invention adopts the membrane filter pressing circulating extraction method to substitute the effective ingredient that decocting method extracts the prescription medical material; This method system adopts the pressure-driven of 0.5-0.6Mpa; Circulation extraction is piled up in hundreds of the powder beds on the eluting face, has the effect of pressurized column chromatography or pressurization percolation, and extraction efficiency significantly improves; The extraction temperature reduces; Thermal sensitivity composition loss reduces, and the response rate of index components significantly increases, and is increased to 9.14mg/g like content of baicalin by the 7.05mg/g of existing method; And the filter cloth aperture of adopting because of diaphragm filter press is far below be used for the isolating filter screen of medicinal residues and decocting liquid aperture at present, and gained extracting solution clarity is good, and naked eyes visible particle thing can not get 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 prescription medical material of same weight, adopt decocting method to need 3 hours, and adopt the membrane filter pressing circulating extraction method to be no more than 1 hour, extraction time shortens more than 60%; And the inventive method has realized the integrated of circulation extraction and solid-liquid separation, does not have the worry of the existing follow-up solid-liquid separation of decocting method.(3) energy savings: with 1m
3Water is heated to 55-65 ℃ from 20 ℃ and needs raw coal 18.4-21.7kg, needs raw coal 37.6kg and be heated to 98 ℃, and 42-51% on year-on-year basis lowers consumption; The extraction time of prescription medical material foreshortened to 1 hour by 3 hours, and the extraction energy consumption is reduced greatly.(4) be beneficial to environmental conservation and waste residue utilization: the medicinal residues after the technical finesse of membrane filter pressing circulation extraction isolation integral are the nearly powdered form block of doing; Water content is few; Not only be convenient to transhipment, can not pollute, and be convenient to later use to environment; 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 is the preferred corollary apparatus figure of membrane filter pressing circulation extraction isolation integral technology.
The specific embodiment
In order to make the object of the invention, technical scheme and advantage clearer, will combine accompanying drawing that the preferred embodiments of the present invention are carried out detailed description below.
The preferred corollary apparatus figure of membrane filter pressing circulation extraction isolation integral technology is as shown in Figure 1; The discharging opening of material-compound tank is communicated with the charging aperture of diaphragm filter press through membrane pump; The liquid outlet of diaphragm filter press is communicated with the import of the charging aperture and the filtrate tank of material-compound tank respectively with three-way valve, and when three-way valve switched to the material-compound tank position, the liquid outlet of diaphragm filter press was 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 gets into the filtrate tank storage, constitutes the membrane filter pressing solid-liquid separation system.
Embodiment 1
Prescription: Rhizoma Et Radix Notopterygii 6kg, windproof 6kg, Rhizoma Atractylodis 6kg, Herba Asari 2kg, Rhizoma Chuanxiong 4kg, Radix Angelicae Dahuricae 4kg, Radix Scutellariae 4kg, Radix Glycyrrhizae 4kg, Radix Rehmanniae 4kg
Method for preparing may further comprise the steps:
A. the extraction of Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong
A1. the Rhizoma Et Radix Notopterygii of recipe quantity, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong are mixed, be ground into coarse powder, 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 distillation device is in addition collected, and is subsequent use;
A3. in the multi-function extractor that extracts medicinal residues behind the volatile oil is housed, add the water that is equivalent to 4 times of step a1 gained medicated powder weight, be heated with stirring to 80 ℃, 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 finishes, in multi-function extractor, add 80 ℃ the water of being preheated to be equivalent to 2 times of step a1 gained medicated powder weight again, 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;
A4. the medicinal residues oven dry after step a3 being handled mixes with the Radix Angelicae Dahuricae of recipe quantity, pulverizes, and sieves, and collects fine powder and remaining coarse powder respectively, and is subsequent use;
B. the extraction of Radix Scutellariae, Radix Glycyrrhizae and Radix Rehmanniae
B1. Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae with recipe quantity mixes, and is ground into coarse powder, and be subsequent use;
B2. the coarse powder with step a4 gained mixes with Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae coarse powder of step b1 gained, and is subsequent use;
B3. in material-compound tank, add the extracting solution A of step a3 gained and add the water ad pond om and be equivalent to 7.5 times of step b2 gained medicated powder weight, be heated to 65 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when pressing filtering liquid passes back into material-compound tank, in material-compound tank, at the uniform velocity add step b2 gained medicated powder; Finish; 65 ℃ of membrane filter pressing circulation extraction 35 minutes switch to the filtrate tank position with three-way valve afterwards 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 65 ℃ the water of being preheated to be equivalent to 3.5 times of step b2 gained medicated powder weight; Insulation membrane filter pressing circulation extraction 20 minutes switches to the filtrate tank position with three-way valve afterwards and carries out membrane filter pressing, collects 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 twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. preparation
C1. the extracting solution B concentrating under reduced pressure with step b3 gained becomes 70 ℃ of relative densities to be the clear paste of 1.03-1.05, and is subsequent use;
C2. with the clear paste of step c1 gained and the general ball of fine powder of step a4 gained, drying is put coldly, sprays into the volatile oil of step a2 gained, and mixing promptly gets Notopterygii Bolus of Nine Ingredients.
Embodiment 2
Prescription: Rhizoma Et Radix Notopterygii 6kg, windproof 6kg, Rhizoma Atractylodis 6kg, Herba Asari 2kg, Rhizoma Chuanxiong 4kg, Radix Angelicae Dahuricae 4kg, Radix Scutellariae 4kg, Radix Glycyrrhizae 4kg, Radix Rehmanniae 4kg
Method for preparing may further comprise the steps:
A. the extraction of Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong
A1. the Rhizoma Et Radix Notopterygii of recipe quantity, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong are mixed, be ground into coarse powder, 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 distillation device is in addition collected, and is subsequent use;
A3. in the multi-function extractor that extracts medicinal residues behind the volatile oil is housed, add the water that is equivalent to 2 times of step a1 gained medicated powder weight, 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 finishes, in multi-function extractor, add 75 ℃ the water of being preheated to be equivalent to 1 times of step a1 gained medicated powder weight again, 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;
A4. the medicinal residues oven dry after step a3 being handled mixes with the Radix Angelicae Dahuricae of recipe quantity, pulverizes, and sieves, and collects fine powder and remaining coarse powder respectively, and is subsequent use;
B. the extraction of Radix Scutellariae, Radix Glycyrrhizae and Radix Rehmanniae
B1. Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae with recipe quantity mixes, and is ground into coarse powder, and be subsequent use;
B2. the coarse powder with step a4 gained mixes with Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae coarse powder of step b1 gained, and is subsequent use;
B3. in material-compound tank, add the extracting solution A of step a3 gained and add the water ad pond om and be equivalent to 6 times of step b2 gained medicated powder weight, be heated to 60 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when pressing filtering liquid passes back into material-compound tank, in material-compound tank, at the uniform velocity add step b2 gained medicated powder; Finish; 60 ℃ of membrane filter pressing circulation extraction 40 minutes switch to the filtrate tank position with three-way valve afterwards 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 ℃ the water of being preheated to be equivalent to 3 times of step b2 gained medicated powder weight, insulation membrane filter pressing circulation extraction 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, 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 concentrating under reduced pressure with step b3 gained becomes 70 ℃ of relative densities to be the clear paste of 1.03-1.05, and is subsequent use;
C2. with the clear paste of step c1 gained and the general ball of fine powder of step a4 gained, drying is put coldly, sprays into the volatile oil of step a2 gained, and mixing promptly gets Notopterygii Bolus of Nine Ingredients.
Embodiment 3
Prescription: Rhizoma Et Radix Notopterygii 6kg, windproof 6kg, Rhizoma Atractylodis 6kg, Herba Asari 2kg, Rhizoma Chuanxiong 4kg, Radix Angelicae Dahuricae 4kg, Radix Scutellariae 4kg, Radix Glycyrrhizae 4kg, Radix Rehmanniae 4kg
Method for preparing may further comprise the steps:
A. the extraction of Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong
A1. the Rhizoma Et Radix Notopterygii of recipe quantity, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong are mixed, be ground into coarse powder, 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 distillation device is in addition collected, and is subsequent use;
A3. in the multi-function extractor that extracts medicinal residues behind the volatile oil is housed, add the water that is equivalent to 3 times of step a1 gained medicated powder weight, be heated with stirring to 85 ℃, 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 finishes, in multi-function extractor, add 85 ℃ the water of being preheated to be equivalent to 3 times of step a1 gained medicated powder weight again, 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;
A4. the medicinal residues oven dry after step a3 being handled mixes with the Radix Angelicae Dahuricae of recipe quantity, pulverizes, and sieves, and collects fine powder and remaining coarse powder respectively, and is subsequent use;
B. the extraction of Radix Scutellariae, Radix Glycyrrhizae and Radix Rehmanniae
B1. Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae with recipe quantity mixes, and is ground into coarse powder, and be subsequent use;
B2. the coarse powder with step a4 gained mixes with Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae coarse powder of step b1 gained, and is subsequent use;
B3. in material-compound tank, add the extracting solution A of step a3 gained and add the water ad pond om and be equivalent to 9 times of step b2 gained medicated powder weight, be heated to 55 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when pressing filtering liquid passes back into material-compound tank, in material-compound tank, at the uniform velocity add step b2 gained medicated powder; Finish; 55 ℃ of membrane filter pressing circulation extraction 30 minutes switch to the filtrate tank position with three-way valve afterwards 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 55 ℃ the water of being preheated to be equivalent to 5 times of step b2 gained medicated powder weight, insulation membrane filter pressing circulation extraction 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 twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. preparation
C1. the extracting solution B concentrating under reduced pressure with step b3 gained becomes 70 ℃ of relative densities to be the clear paste of 1.03-1.05, and is subsequent use;
C2. with the clear paste of step c1 gained and the general ball of fine powder of step a4 gained, drying is put coldly, sprays into the volatile oil of step a2 gained, and mixing promptly gets Notopterygii Bolus of Nine Ingredients.
Employing is with a collection of medicinal raw material; Adopt said method of embodiment 1-3 and existing method (WS-11376 (ZD-1376)-2002 records method) to compare experiment respectively; And products obtained therefrom carried out quality inspection; The result shows: the product that adopts the said 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 said method is than best, and the index components content of baicalin reaches 9.14mg/g in the products obtained therefrom, is higher than existing method products obtained therefrom (7.05mg/g) far away.
Explanation is at last; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although through invention has been described with reference to the preferred embodiments of the present invention; But those of ordinary skill in the art should be appreciated that and can make various changes to it in form with on the details, and the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (3)
1. the method for preparing of Notopterygii Bolus of Nine Ingredients; Process by following raw materials by weight proportions: 200 parts of 300 parts of Rhizoma Et Radix Notopterygiis, windproof 300 parts, 300 parts of Rhizoma Atractylodis, 100 parts of Herba Asaris, 200 parts of Rhizoma Chuanxiongs, 200 parts of the Radixs Angelicae Dahuricae, 200 parts of Radix Scutellariaes, 200 parts in Radix Glycyrrhizae and Radix Rehmanniae; It is characterized in that method for preparing may further comprise the steps:
A. the extraction of Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong
A1. Rhizoma Et Radix Notopterygii, windproof, Rhizoma Atractylodis, Herba Asari and Rhizoma Chuanxiong are mixed, be ground into coarse powder, subsequent use;
A2. the medicated powder with step a1 gained extracts volatile oil with steam distillation, and the aqueous solution after medicinal residues and the distillation is 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 finishes, will be preheated to 60-90 ℃ water again and pump into diaphragm filter press 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; Aqueous solution after the distillation of twice pressing filtering liquid, pressed liquor and step a2 gained is merged, be designated as extracting solution A;
A4. the medicinal residues after step a3 being handled are dry, mix with the Radix Angelicae Dahuricae, pulverize, and sieve, and collect fine powder and remaining coarse powder respectively, and are subsequent use;
B. the extraction of Radix Scutellariae, Radix Glycyrrhizae and Radix Rehmanniae
B1. Radix Scutellariae, Radix Glycyrrhizae and Radix Rehmanniae are mixed, be ground into coarse powder, subsequent use;
B2. the coarse powder with step a4 gained mixes with Radix Scutellariae, Radix Glycyrrhizae and the Radix Rehmanniae coarse powder of step b1 gained, and is subsequent use;
B3. in material-compound tank, add the extracting solution A and the water of step a3 gained, 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 pressing filtering liquid passes back into material-compound tank, under stirring condition, in material-compound tank, add the medicated powder of step b2 gained; Finish; Under 50-90 ℃ condition, carry out the membrane filter pressing circulation extraction first 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, 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 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 B;
C. preparation
C1. the extracting solution B concentrating under reduced pressure with step b3 gained becomes 70 ℃ of relative densities to be the clear paste of 1.03-1.05, and is subsequent use;
C2. with the clear paste of step c1 gained and the general ball of fine powder of step a4 gained, drying is put coldly, sprays into the volatile oil of step a2 gained, and mixing promptly gets Notopterygii Bolus of Nine Ingredients.
2. the method for preparing of Notopterygii Bolus of Nine Ingredients according to claim 1; It is characterized in that; Said step a3 adds earlier to be equivalent to step a1 gained medicated powder weight 2-4 water doubly in medicinal residues; Be heated with stirring to 75-85 ℃, insulated and stirred 5-15 minute, slip pumped into diaphragm filter press carry out membrane filter pressing To be equivalent to again step a1 gained medicated powder weight 1-3 doubly be preheated to 75-85 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Said step b3 is the extracting solution A that adds earlier step a3 gained, adds 6-9 that the water ad pond om is equivalent to step b2 gained medicated powder weight more doubly, under 55-65 ℃ condition, carries out the membrane filter pressing circulation extraction first time, and extraction time is 30-40 minute; Add and be equivalent to step b2 gained medicated powder weight 3-5 water doubly, under 55-65 ℃ condition, carry out the membrane filter pressing circulation extraction second time, extraction time is 10-20 minute.
3. the method for preparing of Notopterygii Bolus of Nine Ingredients according to claim 2; It is characterized in that said step a3 adds the water that is equivalent to 4 times of step a1 gained medicated powder weight earlier 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 step a1 gained medicated powder weight be preheated to 80 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Said step b3 is the extracting solution A that adds earlier step a3 gained, adds the water ad pond om again and is equivalent to 7.5 times of step b2 gained medicated powder weight, under 65 ℃ condition, carries out the membrane filter pressing circulation extraction first time, and extraction time is 35 minutes; Add the water that is equivalent to 3.5 times of step b2 gained medicated powder weight again, under 65 ℃ condition, carry out the membrane filter pressing circulation extraction second time, extraction time is 20 minutes.
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