CN102319311B - Preparation method of tincture of oranges - Google Patents
Preparation method of tincture of oranges Download PDFInfo
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- CN102319311B CN102319311B CN 201110247791 CN201110247791A CN102319311B CN 102319311 B CN102319311 B CN 102319311B CN 201110247791 CN201110247791 CN 201110247791 CN 201110247791 A CN201110247791 A CN 201110247791A CN 102319311 B CN102319311 B CN 102319311B
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Abstract
The invention discloses a preparation method of tincture of oranges, which adopts diaphragm filter-pressing circulation extraction and separation integral technology to replace percolation method so as to extract active constituents of the tincture of the oranges, so that the production cycle can be greatly shortened, the environmental protection is facilitated, and waste residues are utilized, the usage quantity of solvent ethanol is reduced, and the recovery rate of the active constituents 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
The Sanitation Ministry medicine standard WS3-B-2265-96 record: Pericarpium Citri junoris tincture is the bitter stomachic of mending of armaticity.Its prescription is for Pericarpium Citri junoris 100g, and volume fraction is that 60% ethanol is an amount of.Its preparation method is that Pericarpium Citri junoris is ground into coarse powder, is that 60% ethanol is made solvent with volume fraction, flood after 24 hours, with the speed of per minute 3 ~ 5ml percolation slowly, to the full dose of percolate be 1000ml, namely.Adopt percolation to extract the effective ingredient of Pericarpium Citri junoris in the said method, exist in long, the percolation process of production cycle ethanol easily to wave problems such as the loss of loosing causes concentration to change, the effective ingredient response rate is low.
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 separation integrated technique to prepare Pericarpium Citri junoris tincture; not only can significantly shorten the production cycle, be beneficial to environmental conservation and waste residue utilization; and can reduce the consumption that extracts etoh solvent, and greatly improve the response rate of effective ingredient.
For achieving the above object, the invention provides following technical scheme:
A. Pericarpium Citri junoris is ground into coarse powder, standby;
B. in material-compound tank, add 50-60% ethanol; Three-way valve is switched to the material-compound tank position, 50-60% 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 a 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 50-60% 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, again three-way valve is switched to the material-compound tank position, in material-compound tank, add 50-60% ethanol, 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, as extracting solution;
C. the volume of measuring process b gained extracting solution and measure concentration of alcohol, (the drug standard regulation: concentration of alcohol should be 48-58% to ormal weight to adjust concentration of alcohol and cumulative volume, can add 95% ethanol as the case may be or water is regulated), mixing namely gets Pericarpium Citri junoris tincture.
Preferably, described step b adds earlier to be equivalent to Pericarpium Citri junoris weight 6-7 50-55% 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 Pericarpium Citri junoris weight 2.5-3.5 50-55% ethanol doubly, carry out the membrane filter pressing circulation second time and extract, extraction time is 15-25 minute; Add and be equivalent to Pericarpium Citri junoris weight 2-3 50-55% ethanol doubly, carry out membrane filter pressing circulation for the third time and extract, extraction time is 10-20 minute.
Preferred, described step b adds 55% ethanol that is equivalent to 6.5 times of Pericarpium Citri junoris weight earlier, carries out the membrane filter pressing circulation first time and extracts, and extraction time is 40 minutes; Add 55% ethanol that is equivalent to 3 times of Pericarpium Citri junoris weight again, carry out the membrane filter pressing circulation second time and extract, extraction time is 15 minutes; Add 55% ethanol that is equivalent to 2 times of Pericarpium Citri junoris weight again, carry out membrane filter pressing circulation for the third time and extract, extraction time is 10 minutes.
Preferably, also comprise step b ＇ between described step b and the step c: 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 Pericarpium Citri junoris.
Preferred, described step b ＇ adds to be equivalent to Pericarpium Citri junoris weight 2-4 water doubly, and the membrane filter pressing circulation was washed 3-7 minute thoroughly.
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 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 percolation and extracts the Pericarpium Citri junoris effective ingredient, 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 pressurization percolation, extraction efficiency significantly improves, and the index components Determination of Hesperidin Content can improve about 12%; 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 the clarity of gained extracting solution is good.(2) reduced the consumption that extracts etoh solvent: the inventive method can substitute the effective ingredient of 60% ethanol extraction Pericarpium Citri junoris of existing method with 50-55% ethanol, and the ethanol consumption reduces, but the response rate of index components increases on the contrary.(3) shortened the production cycle: extract the Pericarpium Citri junoris of same weight, adopt percolation to need 24 hours at least, and adopt the membrane filter pressing circulating extraction method to be no more than 1.5 hours, extraction time shortens more than 90%; And the inventive method can realize the integrated of extraction and solid-liquid separation that circulate equally, and because the filter cloth of diaphragm filter press is ultimate attainment close, the clarity of gained extracting solution is good.(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.
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, 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 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 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
A. Pericarpium Citri junoris 10kg is ground into coarse powder, standby;
B. in material-compound tank, add 55% ethanol that is equivalent to 6.5 times of Pericarpium Citri junoris 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, 55% 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 a 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 55% ethanol that is equivalent to 3 times of Pericarpium Citri junoris weight in material-compound tank, the membrane filter pressing circulation was extracted 15 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 55% ethanol that is equivalent to 2 times of Pericarpium Citri junoris weight in material-compound tank, the membrane filter pressing circulation was extracted 10 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, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge three pressing filtering liquids and pressed liquor, as extracting solution;
B ＇. 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 Pericarpium Citri junoris 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 Pericarpium Citri junoris;
C. the volume of measuring process b gained extracting solution and measure concentration of alcohol, regulating concentration of alcohol with 95% ethanol or water is 48-58%, and to make cumulative volume be 100L, mixing namely gets Pericarpium Citri junoris tincture.
Embodiment 2
A. Pericarpium Citri junoris 10kg is ground into coarse powder, standby;
B. in material-compound tank, add 50% ethanol that is equivalent to 7 times of Pericarpium Citri junoris 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, 50% 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 a 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 50% ethanol that is equivalent to 2.5 times of Pericarpium Citri junoris weight in material-compound tank, the membrane filter pressing circulation was extracted 20 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 50% ethanol that is equivalent to 2.5 times of Pericarpium Citri junoris weight in material-compound tank, the membrane filter pressing circulation was extracted 15 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, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge three pressing filtering liquids and pressed liquor, as extracting solution;
B ＇. three-way valve is switched to the material-compound tank position, in material-compound tank, add the water that is equivalent to 4 times of Pericarpium Citri junoris 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 Pericarpium Citri junoris;
C. the volume of measuring process b gained extracting solution and measure concentration of alcohol, regulating concentration of alcohol with 95% ethanol or water is 48-58%, and to make cumulative volume be 100L, mixing namely gets Pericarpium Citri junoris tincture.
Embodiment 3
A. Pericarpium Citri junoris 10kg is ground into coarse powder, standby;
B. in material-compound tank, add 55% ethanol that is equivalent to 6 times of Pericarpium Citri junoris 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, 55% 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 a 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 55% ethanol that is equivalent to 3.5 times of Pericarpium Citri junoris weight in material-compound tank, the membrane filter pressing circulation was extracted 25 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 55% ethanol that is equivalent to 3 times of Pericarpium Citri junoris weight in material-compound tank, the membrane filter pressing circulation was extracted 20 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, start the squeezing program of diaphragm filter press, collect pressed liquor; Merge three pressing filtering liquids and pressed liquor, as extracting solution;
B ＇. 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 Pericarpium Citri junoris 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 Pericarpium Citri junoris;
C. the volume of measuring process b gained extracting solution and measure concentration of alcohol, regulating concentration of alcohol with 95% ethanol or water is 48-58%, and to make cumulative volume be 100L, mixing namely gets Pericarpium Citri junoris tincture.
Employing is with a collection of medicinal raw material, adopt the described method of embodiment 1-3 and existing method (the Sanitation Ministry medicine standard WS3-B-2265-96 records 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 Determination of Hesperidin Content improves about 12% in the products obtained therefrom.
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 Pericarpium Citri junoris tincture is characterized in that, may further comprise the steps:
A. Pericarpium Citri junoris is ground into coarse powder, standby;
B. adding concentration of volume percent in the material-compound tank is the ethanol of 50-60%; Three-way valve is switched to the material-compound tank position, be that the ethanol of 50-60% 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 a 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 50-60% 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, 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 50-60% again, carries out membrane filter pressing circulation for the third time and extracts, 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, as extracting solution;
C. the volume of measuring process b gained extracting solution and measure concentration of alcohol is adjusted concentration of alcohol and cumulative volume to ormal weight, and mixing namely gets Pericarpium Citri junoris tincture.
2. the preparation method of Pericarpium Citri junoris tincture according to claim 1, it is characterized in that, described step b adds earlier that to be equivalent to Pericarpium Citri junoris weight 6-7 concentration of volume percent doubly be the ethanol of 50-55%, carries out membrane filter pressing circulation extraction first time, and extraction time is 30-40 minute; Adding and being equivalent to Pericarpium Citri junoris weight 2.5-3.5 concentration of volume percent doubly is the ethanol of 50-55%, carries out the membrane filter pressing circulation second time and extracts, and extraction time is 15-25 minute; Adding and being equivalent to Pericarpium Citri junoris weight 2-3 concentration of volume percent doubly is the ethanol of 50-55%, carries out membrane filter pressing circulation for the third time and extracts, and extraction time is 10-20 minute.
3. the preparation method of Pericarpium Citri junoris tincture according to claim 2 is characterized in that, described step b is that to add earlier the concentration of volume percent that is equivalent to 6.5 times of Pericarpium Citri junoris weight be 55% ethanol, carries out membrane filter pressing circulation extraction first time, and extraction time is 40 minutes; Add the concentration of volume percent be equivalent to 3 times of Pericarpium Citri junoris weight again and be 55% ethanol, carry out membrane filter pressing circulation extraction second time, extraction time is 15 minutes; Add the concentration of volume percent be equivalent to 2 times of Pericarpium Citri junoris weight again and be 55% ethanol, carry out membrane filter pressing circulation for the third time and extract, extraction time is 10 minutes.
4. according to the preparation method of the described Pericarpium Citri junoris tincture of the arbitrary claim of claim 1 to 3, it is characterized in that, also comprise step b ＇ between described step b and the step c: 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 Pericarpium Citri junoris.
5. the preparation method of Pericarpium Citri junoris tincture according to claim 4 is characterized in that, described step b ＇ adds to be equivalent to Pericarpium Citri junoris weight 2-4 water doubly, and the membrane filter pressing circulation was washed 3-7 minute thoroughly.
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| CN 201110247791 CN102319311B (en) | 2011-08-26 | 2011-08-26 | Preparation method of tincture of oranges |
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| CN 201110247791 CN102319311B (en) | 2011-08-26 | 2011-08-26 | Preparation method of tincture of oranges |
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