CN102247469A - Preparation method for Jizhi syrup - Google Patents
Preparation method for Jizhi syrup Download PDFInfo
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- CN102247469A CN102247469A CN2011102477469A CN201110247746A CN102247469A CN 102247469 A CN102247469 A CN 102247469A CN 2011102477469 A CN2011102477469 A CN 2011102477469A CN 201110247746 A CN201110247746 A CN 201110247746A CN 102247469 A CN102247469 A CN 102247469A
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Abstract
The invention discloses a preparation method for Jizhi syrup. According to the invention, active ingredients of prescribed medicinal materials are extracted by the integrated technology of diaphragm press filtration and cyclic extraction and separation instead of by the method of decoction; therefore, the flow of the preparation is simplified, production period is greatly shortened, energy consumption is reduced, benefits to environmental protection and utilization of waste residues are obtained, and the recovery rate of the active ingredients is substantially improved.
Description
Technical field
The invention belongs to pharmaceutical field, relate to a kind of preparation method of Chinese medicine preparation.
Background technology
Chinese patent ZL91107258.6 discloses a kind of cough-relieving Chinese patent medicine---JIZHI TANGJIANG, and its prescription is: Rhizoma Fagopyri Dibotryis 10-250g, Herba Houttuyniae 10-250g, Ilex purpurea Hassk.[I.chinensis Sims 10-250g, Radix Asteris 5-150g, Radix Peucedani 5-100g, Fructus Aurantii 5-100g, Herba Ephedrae 5-60g, Radix Glycyrrhizae 5-50g, sweeting agent 400-900g, benzoic acid 0.1-3g, ethyl hydroxybenzoate 0.05-0.5g, add water to 1000ml; Its preparation method is: press formula ratio, with Herba Houttuyniae, Fructus Aurantii boiling reflux 0.5-1 hour, begin distillation, collect Aromatic water, concentrate Herba Houttuyniae, mother liquid of bitter orange, wait to prepare burden; Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae, the Radix Glycyrrhizae of Herba Houttuyniae and Fructus Aurantii medicinal residues adding formula ratio are decocted with water secondary, hold at every turn and boil 2-4 hour, decoction liquor gradation filtering and concentrating; Concentrated solution and Herba Houttuyniae, mother liquid of bitter orange be heated to boil, respectively add half amount sucrose dissolved respectively after, combine, add preservative benzoic acid and ethyl hydroxybenzoate and Aromatic water, stir evenly, filter, add water to 1000ml, fill, sterilization, promptly.Adopt decocting method to extract the effective ingredient of prescription medical material in the said method, exist extraction time long, extract that 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 warm macerating extraction separation integrated technique to prepare above-mentioned JIZHI TANGJIANG; 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 JIZHI TANGJIANG, made by following raw materials by weight proportions: Rhizoma Fagopyri Dibotryis 10-250 part, Herba Houttuyniae 10-250 part, Ilex purpurea Hassk.[I.chinensis Sims 10-250 part, Radix Asteris 5-150 part, Radix Peucedani 5-100 part, Fructus Aurantii 5-100 part, Herba Ephedrae 5-60 part and Radix Glycyrrhizae 5-50 part may further comprise the steps:
A. the extraction of Herba Houttuyniae and Fructus Aurantii
A1. Herba Houttuyniae and Fructus Aurantii are mixed, be ground into coarse powder, standby;
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 standby;
A3. in the medicinal residues of step a2 gained, add water, be heated with stirring to 60-95 ℃, slip is pumped into diaphragm filter press carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, will be preheated to 60-95 ℃ 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;
B. the extraction of Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae
B1. Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae are mixed, be ground into coarse powder, standby;
B2. the extracting solution A and the water that add step a3 gained in material-compound tank are heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, water in the material-compound tank is pumped into diaphragm filter press, when pressing filtering liquid passes back into material-compound tank, under stirring condition, in material-compound tank, add step b1 gained medicated powder, finish, under 50-90 ℃ condition, carry out the membrane filter pressing circulation first time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing 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 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 B;
C. preparation
The extracting solution B of step b2 gained is concentrated, add the volatile oil of acceptable accessories and step a2 gained, adopt practice of pharmacy to make syrup, promptly get JIZHI TANGJIANG.
Preferably, described 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 75-95 ℃, insulated and stirred 5-15 minute, with slip pump into diaphragm filter press carry out the membrane filter pressing To be equivalent to again step a1 gained medicated powder weight 1-3 doubly be preheated to 75-95 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds earlier the described extracting solution A of step a3, and adds 6-8 that the water ad pond om is equivalent to step b1 gained medicated powder weight doubly, carries out membrane filter pressing circulation extraction first time under 55-65 ℃ condition, and extraction time is 30-40 minute; Add and be equivalent to step b1 gained medicated powder weight 3-5 water doubly, carry out the membrane filter pressing circulation second time and extract under 55-65 ℃ condition, extraction time is 10-20 minute.
Preferred, described step a3 adds earlier the water that is equivalent to 2 times of step a1 gained medicated powder weight in medicinal residues, be heated with stirring to 85 ℃, 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 85 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds earlier the described extracting solution A of step a3, and adds the water ad pond om and be equivalent to 8 times of step b1 gained medicated powder weight, carries out membrane filter pressing circulation extraction first time under 65 ℃ condition, and extraction time is 30 minutes; Add the water that is equivalent to 3 times of step b1 gained medicated powder weight again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 10 minutes.
Membrane filter pressing circulation extraction separation integrated technique 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 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 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) when passing back into material-compound tank when observing pressing filtering liquid (this moment is actual to be solvent) from the manhole of material-compound tank, 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, extract temperature and can be controlled at 50-90 ℃, according to polarized light microscopy method measurement result and in conjunction with bibliographical information, starch gelatinization temperature in the plant tissue mostly is 70-71 ℃, for fear of occurring because of 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 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 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 with medicinal residues and other medical material merging carrying 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 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.
Beneficial effect of the present invention is: (1) has improved the response rate of effective ingredient: the present invention adopts the membrane filter pressing circulating extraction method to substitute the effective ingredient that decocting method extracts the prescription medical material, 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, and can be increased to 1.12mg/ml by the 0.87mg/ml of existing method as the content of naringin; And the filter cloth aperture of adopting because of diaphragm filter press is far below being 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 enter in the finished product, has also correspondingly improved the content of active ingredient in the finished product.(2) simplified technological process, shortened the production cycle: Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and the Radix Glycyrrhizae of extracting same weight, adopt decocting method to need 4-8 hour, and adopt the membrane filter pressing circulating extraction method to be no more than 1 hour, extraction time shortens more than 75%; And the inventive method can realize the integrated of extraction and solid-liquid separation that circulate, and does not have the worry of the existing follow-up solid-liquid separation of decocting method.(3) energy savings: with 1m
3Water is heated to 55-65 ℃ from 20 ℃ and needs raw coal 18.4-21.7kg, needs raw coal 37.6kg and be heated to 98 ℃, and 42-51% on year-on-year basis lowers consumption; The extraction time of prescription medical material foreshortened to 1 hour by 2 hours, and the extraction energy consumption is reduced greatly.(4) be beneficial to environmental conservation and waste residue utilization: the medicinal residues after membrane filter pressing circulation extraction separation integrated technique is handled 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.(5) require in the existing method medicinal residues and Rhizoma Fagopyri Dibotryis behind Herba Houttuyniae and the Fructus Aurantii extraction volatile oil, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae add water and fry in shallow oil altogether, reach a few hours owing to extract the process of volatile oil with the water azeotropic, during the water soluble ingredient of Herba Houttuyniae and Fructus Aurantii fully is soluble in the aqueous phase in the process of extracting volatile oil, so the medicinal residues that the inventive method no longer will be extracted behind the volatile oil decoct with water, and only with hot water medicinal residues are washed thoroughly, aqueous solution after saturating washing liquid and the distillation merges, as Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, the solvent of extraction first of Herba Ephedrae and Radix Glycyrrhizae is applied mechanically, when guaranteeing the effective ingredient response rate, reduce and extract solvent load, reduce follow-up concentrated energy consumption.
Description of drawings
Fig. 1 is the preferred corollary apparatus figure of membrane filter pressing circulation extraction separation integrated technique.
The specific embodiment
In order to make the purpose, technical solutions and advantages of the present invention clearer, the preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing.
The preferred corollary apparatus figure of membrane filter pressing circulation extraction separation integrated technique 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 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, 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 Fagopyri Dibotryis 5kg, Herba Houttuyniae 5kg, Ilex purpurea Hassk.[I.chinensis Sims 5kg, Radix Asteris 2.5kg, Radix Peucedani 2.5kg, Fructus Aurantii 2.5kg, Herba Ephedrae 2.5kg, Radix Glycyrrhizae 2.5kg
Preparation method may further comprise the steps:
A. the extraction of Herba Houttuyniae and Fructus Aurantii
A1. Herba Houttuyniae and Fructus Aurantii are mixed, be ground into coarse powder, standby;
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 standby;
A3. add the water that is equivalent to 3 times of step a1 gained medicated powder weight in the multi-function extractor that extracts medicinal residues behind the volatile oil is housed, is heated with stirring to 95 ℃, 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 95 ℃ 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;
B. the extraction of Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae
B1. Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae are mixed, be ground into coarse powder, standby;
B2. 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 b1 gained medicated powder weight, be heated to 60 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when pressing filtering liquid passes back into material-compound tank, in material-compound tank, at the uniform velocity add step b1 gained medicated powder, 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 be equivalent to 5 times of step b1 gained medicated powder weight in 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, 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
The extracting solution B of step b2 gained is concentrated, add the volatile oil of sucrose 200kg, benzoic acid 5g, ethyl hydroxybenzoate 25g and step a2 gained, add water to 500L, mixing promptly gets JIZHI TANGJIANG.
Embodiment 2
Prescription: Rhizoma Fagopyri Dibotryis 5kg, Herba Houttuyniae 5kg, Ilex purpurea Hassk.[I.chinensis Sims 5kg, Radix Asteris 3kg, Radix Peucedani 2kg, Fructus Aurantii 2kg, Herba Ephedrae 1.2kg, Radix Glycyrrhizae 1kg
Preparation method may further comprise the steps:
A. the extraction of Herba Houttuyniae and Fructus Aurantii
A1. Herba Houttuyniae and Fructus Aurantii are mixed, be ground into coarse powder, standby;
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 standby;
A3. add the water that is equivalent to 4 times of step a1 gained medicated powder weight in the multi-function extractor that extracts medicinal residues behind the volatile oil is housed, is 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;
B. the extraction of Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae
B1. Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae are mixed, be ground into coarse powder, standby;
B2. 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 times of step b1 gained medicated powder weight, be heated to 55 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when pressing filtering liquid passes back into material-compound tank, in material-compound tank, at the uniform velocity add step b1 gained medicated powder, finish, 55 ℃ of membrane filter pressing circulations were extracted 40 minutes, afterwards three-way valve were switched to the filtrate tank position and carried out membrane filter pressing, collected pressing filtering liquid; After filter pressing finishes, three-way valve is switched to the material-compound tank position again, add 55 ℃ the water of being preheated to be equivalent to 4 times of step b1 gained medicated powder weight in 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 twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. preparation
The extracting solution B of step b2 gained is concentrated, add the volatile oil of sucrose 19kg, benzoic acid 60g, ethyl hydroxybenzoate 10g and step a2 gained, add water to 20L, mixing promptly gets JIZHI TANGJIANG.
Embodiment 3
Prescription: Rhizoma Fagopyri Dibotryis 4.8kg, Herba Houttuyniae 4.8kg, Ilex purpurea Hassk.[I.chinensis Sims 4.2kg, Radix Asteris 1.35kg, Radix Peucedani 1.65kg, Fructus Aurantii 2.25kg, Herba Ephedrae 1.35kg, Radix Glycyrrhizae 0.45kg
Preparation method may further comprise the steps:
A. the extraction of Herba Houttuyniae and Fructus Aurantii
A1. Herba Houttuyniae and Fructus Aurantii are mixed, be ground into coarse powder, standby;
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 standby;
A3. add the water that is equivalent to 2 times of step a1 gained medicated powder weight in the multi-function extractor that extracts medicinal residues behind the volatile oil is housed, is heated with stirring to 85 ℃, insulated and stirred 10 minutes pumps into diaphragm filter press with slip and (adopts 80 ± 10 L/m
2.s polypropylene multifilament filter cloth) carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, in multi-function extractor, add 85 ℃ 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;
B. the extraction of Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae
B1. Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae are mixed, be ground into coarse powder, standby;
B2. in material-compound tank, add the extracting solution A of step a3 gained and add the water ad pond om and be equivalent to 8 times of step b1 gained medicated powder weight, be heated to 65 ℃ and insulation; Three-way valve is switched to the material-compound tank position, open agitator, membrane pump and the diaphragm filter press of material-compound tank, the water in the material-compound tank is pumped into diaphragm filter press (adopt 80 ± 10 L/m
2.s polypropylene multifilament filter cloth), when pressing filtering liquid passes back into material-compound tank, in material-compound tank, at the uniform velocity add step b1 gained medicated powder, 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 be equivalent to 3 times of step b1 gained medicated powder weight in 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 twice pressing filtering liquid and pressed liquor, be designated as extracting solution B;
C. preparation
The extracting solution B of step b2 gained is concentrated, add the volatile oil of sucrose 25.5kg, benzoic acid 60g, ethyl hydroxybenzoate 12.9g and step a2 gained, add water to 30L, mixing promptly gets JIZHI TANGJIANG.
Employing is with a collection of raw material, adopt described method of embodiment 1-3 and existing method (Chinese patent ZL 91107258.6 open methods) to compare experiment respectively, and the concentrated thick paste of extracting solution carried out quality inspection, the result shows: do not have in the relative density of thick paste under the situation of significant difference, the content of index components naringin is significantly higher than the thick paste that existing method makes in the thick paste that the described method of employing embodiment 1-3 makes.Wherein, the cost-effectiveness of embodiment 3 described methods is than best, and the content of index components naringin is increased to 1.12mg/ml by the 0.87mg/ml of existing method.
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 the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (3)
1. the preparation method of JIZHI TANGJIANG, make by following raw materials by weight proportions: Rhizoma Fagopyri Dibotryis 10-250 part, Herba Houttuyniae 10-250 part, Ilex purpurea Hassk.[I.chinensis Sims 10-250 part, Radix Asteris 5-150 part, Radix Peucedani 5-100 part, Fructus Aurantii 5-100 part, Herba Ephedrae 5-60 part and Radix Glycyrrhizae 5-50 part, it is characterized in that, may further comprise the steps:
A. the extraction of Herba Houttuyniae and Fructus Aurantii
A1. Herba Houttuyniae and Fructus Aurantii are mixed, be ground into coarse powder, standby;
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 standby;
A3. in the medicinal residues of step a2 gained, add water, be heated with stirring to 60-95 ℃, slip is pumped into diaphragm filter press carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing finishes, will be preheated to 60-95 ℃ 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;
B. the extraction of Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae
B1. Rhizoma Fagopyri Dibotryis, Ilex purpurea Hassk.[I.chinensis Sims, Radix Asteris, Radix Peucedani, Herba Ephedrae and Radix Glycyrrhizae are mixed, be ground into coarse powder, standby;
B2. the extracting solution A and the water that add step a3 gained in material-compound tank are heated to 50-90 ℃ and insulation; Three-way valve is switched to the material-compound tank position, water in the material-compound tank is pumped into diaphragm filter press, when pressing filtering liquid passes back into material-compound tank, under stirring condition, in material-compound tank, add step b1 gained medicated powder, finish, under 50-90 ℃ condition, carry out the membrane filter pressing circulation first time and extract, afterwards three-way valve is switched to the filtrate tank position and carry out membrane filter pressing, collect pressing filtering liquid; After filter pressing 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 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 B;
C. preparation
The extracting solution B of step b2 gained is concentrated, add the volatile oil of acceptable accessories and step a2 gained, adopt practice of pharmacy to make syrup, promptly get JIZHI TANGJIANG.
2. the preparation method of JIZHI TANGJIANG according to claim 1, it is characterized in that, described 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 75-95 ℃, insulated and stirred 5-15 minute, slip is pumped into diaphragm filter press carry out membrane filter pressing To be equivalent to again step a1 gained medicated powder weight 1-3 doubly be preheated to 75-95 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds earlier the described extracting solution A of step a3, and adds 6-8 that the water ad pond om is equivalent to step b1 gained medicated powder weight doubly, carries out membrane filter pressing circulation extraction first time under 55-65 ℃ condition, and extraction time is 30-40 minute; Add and be equivalent to step b1 gained medicated powder weight 3-5 water doubly, carry out the membrane filter pressing circulation second time and extract under 55-65 ℃ condition, extraction time is 10-20 minute.
3. the preparation method of JIZHI TANGJIANG according to claim 2, it is characterized in that described step a3 adds the water that is equivalent to 2 times of step a1 gained medicated powder weight earlier in medicinal residues, be heated with stirring to 85 ℃, 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 85 ℃ water pump into diaphragm filter press carry out the membrane filter pressing
Described step b2 adds earlier the described extracting solution A of step a3, and adds the water ad pond om and be equivalent to 8 times of step b1 gained medicated powder weight, carries out membrane filter pressing circulation extraction first time under 65 ℃ condition, and extraction time is 30 minutes; Add the water that is equivalent to 3 times of step b1 gained medicated powder weight again, carry out the membrane filter pressing circulation second time and extract under 65 ℃ condition, extraction time is 10 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108835354A (en) * | 2018-07-10 | 2018-11-20 | 湖南华夏湘众药业饮片有限公司 | A kind of Fructus Aurantii sugar formula manufacture craft |
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| CN1060213A (en) * | 1991-07-27 | 1992-04-15 | 四川涪陵制药厂 | The preparation method that contains the antitussive of Rhizoma Fagopyri Dibotryis |
| CN1366898A (en) * | 2001-01-22 | 2002-09-04 | 杨孟君 | Nano jizhi preparation medicine and preparation method thereof |
| CN1745785A (en) * | 2005-09-16 | 2006-03-15 | 江西本草天工科技有限责任公司 | Jizhi solid preparation |
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| CN1060213A (en) * | 1991-07-27 | 1992-04-15 | 四川涪陵制药厂 | The preparation method that contains the antitussive of Rhizoma Fagopyri Dibotryis |
| CN1366898A (en) * | 2001-01-22 | 2002-09-04 | 杨孟君 | Nano jizhi preparation medicine and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108835354A (en) * | 2018-07-10 | 2018-11-20 | 湖南华夏湘众药业饮片有限公司 | A kind of Fructus Aurantii sugar formula manufacture craft |
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