CN101618053B - Preparation process of isatis root medical solution - Google Patents
Preparation process of isatis root medical solution Download PDFInfo
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- CN101618053B CN101618053B CN2009101648538A CN200910164853A CN101618053B CN 101618053 B CN101618053 B CN 101618053B CN 2009101648538 A CN2009101648538 A CN 2009101648538A CN 200910164853 A CN200910164853 A CN 200910164853A CN 101618053 B CN101618053 B CN 101618053B
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Abstract
The invention discloses a preparation process of isatis root medical solution, comprising the following steps: firstly, isatis root decoction tablets are processed by a water extraction method, and an isatis root water extract is obtained; secondly, the isatis root water extract passes through an inorganic ceramic membrane with the pore diameter of 100nm to 50nm under the pressure of 0.05 MPa to 0.1 MPa; and thirdly, the isatis root water extract then passes through an organic membrane with the intercepted molecular weight of 3000 to 1500 under the pressure of 0.05 MPa to 0.15 MPa to obtain the isatis root medical solution. The preparation process can run under low temperature, has short production period, little energy consumption, high separation efficiency and accuracy, little environmental pollution and up-and-up product quality. Through initial calculation, the invention can save about 3.42 tons of steam and 0.35 tons of alcohol by treating each ton of isatis root medicinal materials.
Description
Technical field
The present invention relates to a kind of preparation technology of Chinese patent medicine, particularly relate to a kind of preparation process of isatis root medical solution.
Background technology
Isatis root medical solution has heat-clearing and toxic substances removing, and the effect of removing heat from blood sore-throat relieving is one of the most frequently used anti-flu Chinese patent medicine, is the Chinese patent medicine preparation of being made by the single Radix Isatidis.In the preparation process of traditional isatis root medical solution, the extraction separation of Radix Isatidis is the process route of water extract-alcohol precipitation+evaporation and concentration with concentrated employing, and is specific as follows:
Isatis root extract → evaporation and concentration → precipitate with ethanol → recovery ethanol → evaporation and concentration → runny plaste.
Although this process route is the legal process route that many Chinese patent medicines are produced, and is legal and unreasonable.Problem mainly is, the used precipitate with ethanol separation and refining method specific aim of this technology is poor, and separation accuracy is not high, causes the loss of some effective ingredient in the Radix Isatidis easily.In addition, this technology exists also that processing step is many, the production cycle is long, and evaporation and concentration reclaims step such as ethanol also needs to consume shortcomings such as a large amount of ethanol and heat energy.
Summary of the invention
Be directed to this, the objective of the invention is to, a kind of preparation process of isatis root medical solution is provided, adopt membrane separation technique, reach Radix Isatidis separation accuracy height, effect with short production cycle.
For achieving the above object, technical scheme provided by the invention is: a kind of preparation process of isatis root medical solution may further comprise the steps:
(1) gets the Radix Isatidis decoction pieces and carry out the water extraction processing, obtain the Radix Isatidis water extract;
(2) the Radix Isatidis water extract is 0.05～0.1MPa at pressure, is the inorganic ceramic film of 100nm～50nm by the aperture;
(3) be under 0.05～0.15MPa at pressure again, the organic membrane by molecular cut off 3000～1500 obtains isatis root medical solution.
Further, the aperture of the inorganic ceramic film in the described step (2) is 50nm.
Further, the molecular cut off of the organic membrane in the described step (3) is 2000.
Further, the temperature in the described step (2) is 62 ℃～80 ℃.
Further, the temperature in the described step (3) is 40 ℃～45 ℃.
Further, this preparation technology also comprises concentration process, and described concentration process is: under 0.05～0.15MPa pressure, be 150～50 organic membrane by molecular cut off with isatis root medical solution.
Further, described organic membrane molecular cut off is 100.
Further, the temperature of described concentration process is 55 ℃～60 ℃.
Compared with prior art, the present invention has selected the film group technology of the organic membrane of the organic membrane of inorganic ceramic film, molecular cut off 2000 of 50nm and molecular cut off 100, carried out the separation of isatis root extract effectively and concentrated, pilot scale check operational effect is stable, and product quality meets the requirements and is better than traditional handicraft.
The advantage of this technology is: this preparation technology can be in cold operation, and with short production cycle, energy consumption is low, separation efficiency and precision height, and environmental pollution is little, and product quality turns for the better.Through initial estimate, handle Radix Isatidis medical material per ton and can save about 3.42 tons of steam, save 0.35 ton of ethanol.
Description of drawings
Fig. 1 is G
2Membrane flux is schemed over time;
Fig. 2 is that the GM membrane flux is schemed over time;
Fig. 3 is RO
2Membrane flux is schemed over time.
The specific embodiment
Describe the present invention below in conjunction with accompanying drawing, the description of this part only is exemplary and explanatory, should any restriction not arranged to protection scope of the present invention.
The present invention uses the remove impurity of two-stage ultrafilter membrane to add the membrane separation process route of first-stage reverse osmosis membrance concentration according to the characteristics of chemical constituent in the Radix Isatidis aqueous extract:
Isatis root extract → one-level film remove impurity → secondary film remove impurity → membrance concentration → isatis root medical solution.Concrete preparation process is as described below:
A kind of preparation process of isatis root medical solution may further comprise the steps:
(1) gets the Radix Isatidis decoction pieces and carry out the water extraction processing, obtain the Radix Isatidis water extract;
(2) the Radix Isatidis water extract is 0.05～0.1MPa at pressure, is the inorganic ceramic film of 100nm～50nm by the aperture;
(3) be under 0.05～0.15MPa at pressure again, by the organic membrane of molecular cut off 3000～1500;
(4) under 0.05～0.15MPa pressure, be 150～50 organic membrane with isatis root medical solution by molecular cut off, obtain isatis root medical solution.
Test
1, materials and methods
1.1 reagent reagent
Adenosine (Chinese medicine bioassay institute is for assay usefulness, lot number 200201); Acetonitrile (chromatographically pure, Fisher company), methanol (analytical pure, Shanghai development chemical industry one factory), ethanol (analytical pure); Sodium hypochlorite, sodium hydroxide, sodium polyphosphate, dodecylbenzene sodium sulfonate etc. are chemical pure; Radix Isatidis water extract (from carrying, crossing 200 mesh sieves) by conventional method.
1.2 experimental facilities
1 of membrance separation Chinese style equipment, G
1Film (inorganic ceramic film of aperture 100nm), G
2Film (inorganic ceramic film of aperture 50nm), G
3Film (inorganic ceramic film of aperture 80nm);
GM film (organic membrane of molecular cut off 2000), GH film (organic membrane of molecular cut off 1500), GN film (organic membrane of molecular cut off 3000), GY film (organic membrane of molecular cut off 2500);
RO
1Film (organic membrane of molecular cut off 150), RO
2Film (organic membrane of molecular cut off 100), RO
3Film (organic membrane of molecular cut off 50).Provide by Wuhan Polytechnical Univ's membrane technology institute.
1.3 analytical method
1.3.1 the solid content dry weightless mensuration is seen Chinese Pharmacopoeia [S]. a .2005; Described in the appendix 47;
1.3.2 aminoacid inspection ninhydrin colorimetry;
1.3.3 the protein inspection is put in the 25ml test tube for examination isatis root medical solution 2ml, adds 60% ethanol 20ml, the amount of observing flocculent deposit after 30 minutes is left standstill in jolting 5 minutes;
1.3.4 adenosine is measured with high performance liquid chromatography and is adopted Agilent1100 high performance liquid chromatograph, chromatographic column: hypersil ODS (4.6mm * 250mm 5 μ m); Mobile phase: acetonitrile-water (6: 94); Detect wavelength: 260nm; Flow velocity: 1.0mm/min; Column temperature: 30 ℃; Sample size: 10 μ L.
2, result and discussion
2.1 process route is according to the characteristics of chemical constituent in the Radix Isatidis aqueous extract, and the situation of binding film remove impurity prerun, too fast for preventing The decline of membrane flux, we have designed the membrane separation process route with two-stage ultrafilter membrane remove impurity+first-stage reverse osmosis membrance concentration, and are specific as follows:
Isatis root extract → one-level film remove impurity → secondary film remove impurity → membrance concentration → isatis root medical solution
2.2 one-level remove impurity film preferably select Radix Isatidis film experiment on the extracting solution first for use, flux, the flux rate of decay, solid content clearance, the film of investigating the different size film clean complexity, result such as following table 1:
Table 1 one-level remove impurity film optimization experiment result
Annotate: membrane flux is between 0.1MPa pressure, temperature 62-80 ℃, and last film 1 hour is with interior institute measured value.
As shown in Table 1, G
1The flux of film is less than normal, and the flux decay is fast, and remove impurity aluminum is less, is not suitable for using.G
2And G
3Membrane flux is big, and is stable, and G
2The flux decay of film is slow, and cleaning performance is good, and therefore, one-level remove impurity film is preferably used G
2Film.
2.3 secondary remove impurity film preferably with Radix Isatidis first extracting solution cross G
2Film experiment on the medicinal liquid behind the film of film, identification, the adenosine content of medicinal liquid behind the flux of investigation different size film, the flux rate of decay, solid content clearance, film cleaning complexity, the film, result such as following table 2:
Table 2 secondary remove impurity film preferred result
Annotate: membrane flux is between 0.15MPa pressure, temperature 40-45 ℃, and last film 1.5 hours is with interior institute measured value.
As shown in Table 2, the solid content clearance of GH film is very high, reaches 77.1%, but the adenosine loss is also more; The impurities removing efficiency of GN film and GY film is not high, and the remove impurity ability of GM film is moderate, and the adenosine loss rate is less, and product quality still at tolerance interval, therefore, still selects GM membrane filtration liquid as secondary remove impurity film according to the assessment of Radix Isatidis granule quality standard.
2.4 concentrate film preferred with the RO film to through G
1And the isatis root medical solution handled of GM film concentrates, color, abnormal smells from the patient, identification, the adenosine loss rate of water liquid behind the flux of investigation different size film, the flux rate of decay, solid content rejection, film cleaning complexity, the film, and result such as following table 3:
Table 3 concentrates the film preferred result
Annotate: membrane flux is between 0.1MPa pressure, temperature 40-56 ℃, and last film 1.5 hours is with interior institute measured value.
As shown in Table 3, RO
1Film is used for the concentrating of isatis root medical solution after the film remove impurity, water liquid color slightly behind its film, and certain aminoacid and adenosine loss, RO are arranged
3The adenosine loss of film is comparatively serious; And RO
2Water removal effect is good, and the eccrine gland glycosides content behind the film is extremely low, does not contain aminoacid simultaneously, therefore is elected to be to concentrate to use film.
2.5 new old technology contrast
Traditional process route is: isatis root extract → evaporation and concentration → precipitate with ethanol → recovery ethanol → evaporation and concentration → isatis root medical solution.
Get the clean medical material of 49KG Radix Isatidis, press the Radix Isatidis granule traditional handicraft and extract, extracting solution is divided into two parts according to 2: 8 ratio, measures few portion for making runny plaste by traditional handicraft, and amount portion how is then according to G
2-GM-RO
2Runny plaste is handled and made to film on the route, observes Radix Isatidis membrane separation process for extracting solution ruuning situation, and compare two kinds of handicraft product yields and quality.Result such as table 4,
Fig. 1-3, table 5:
Table 4 isatis root extract membrane separation process pilot scale service condition and result
Table 5 isatis root extract membrane separation process and traditional handicraft pilot product quality situation
From table 4 and Fig. 1, Fig. 2, Fig. 3 as can be seen, G
2+ GM combined films technology can effectively be removed the microgranule and the soluble large molecule impurity of Radix Isatidis aqueous extract, and membrane flux to change plateau all longer, from flux trend over time, G
2All can move continuously more than 6 hours with the GM film.Select RO for use
2Film can be to through G
2The isatis root extract that+GM combined films was handled carries out concentrating effectively, and the rate that dewaters is up to 76.5%, and The decline of membrane flux is very fast, but also can keep operation continuously more than 6 hours.The mixed liquor of selecting sodium hypochlorite and sodium hydroxide for use is to cleaning G
2Film selects for use the complex cleaning and washing agent of sodium polyphosphate, dodecylbenzene sodium sulfonate and EDTA sodium salt to clean GM and RO
2Film all can be received excellent cleaning effect, and the flux of film is effectively restored.
As can be known from the results of Table 5, compare with traditional precipitate with ethanol+evaporation technology, selected membrane separation process solid content clearance is low by 24%, and the runny plaste yield is high by 27.1%, and adenosine content is high by 2.3%.May to be some molecular weight be removed in the precipitate with ethanol process at 100 to 2000 low molecular weight compositions for this, and the result who in the membrance separation process, is kept.Studies show that the pharmaceutically active ingredient molecular weight is below 2000 among the overwhelming majority, and invalid components such as starch, protein, cellulose equimolecular quantity are more than 50,000.Therefore, the composition of complete reservation molecular weight below 2000, the drug effect that helps Radix Isatidis improves.
In addition, can find out also from table 5 that the prepared runny plaste amount of membrance concentration is bigger, it is more to contain moisture, if adopt wet granulation, still needs further to concentrate.As for the visible slight proteins react of membrane separation process gained runny plaste inspection, then with in the membrance separation process have a small amount of low molecular protein or polypeptide by relevant, " the Chinese pharmacopoeia standard determination then can be ignored according to 2005 editions for the influence of Radix Isatidis granule quality for it.
3, conclusion
3.1 preferred G
2+ GM+RO
2Membrane separation process can effectively separate and concentrates isatis root extract, and the Radix Isatidis runny plaste inherent quality of this prepared meets the requirements substantially, and is better than precipitate with ethanol+evaporation technology gained runny plaste in a sense.
3.2 isatis root medical solution is being carried out in the pilot scale processing procedure G
2, GM and RO
2Film spare all can be realized many hours operation continuously, and selects for use suitable abluent that its flux is effectively restored, and shows G
2+ GM+RO
2Membrane separation process has possessed the condition that is used for the Radix Isatidis granule suitability for industrialized production technically.
It below only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. preparation process of isatis root medical solution may further comprise the steps:
(1) gets the Radix Isatidis decoction pieces and carry out the water extraction processing, obtain the Radix Isatidis water extract;
(2) the Radix Isatidis water extract is 0.05～0.1MPa at pressure, is the inorganic ceramic film of 100nm～50nm by the aperture;
(3) be under 0.05～0.15MPa at pressure again, by the organic membrane of molecular cut off 3000～1500;
(4) under 0.05～0.15MPa pressure, be 150～50 organic membrane by molecular cut off, obtain isatis root medical solution.
2. preparation process of isatis root medical solution according to claim 1 is characterized in that: the aperture of the inorganic ceramic film in the described step (2) is 50nm.
3. preparation process of isatis root medical solution according to claim 1 is characterized in that: the molecular cut off of the organic membrane in the described step (3) is 2000.
4. preparation process of isatis root medical solution according to claim 1 and 2 is characterized in that: the temperature in the described step (2) is 62 ℃～80 ℃.
5. preparation process of isatis root medical solution according to claim 1 and 2 is characterized in that: the temperature in the described step (3) is 40 ℃～45 ℃.
6. preparation process of isatis root medical solution according to claim 1 is characterized in that: described step (4) organic membrane molecular cut off is 100.
7. according to claim 6 or 1 described preparation process of isatis root medical solution, it is characterized in that: the temperature of described step (4) is 55 ℃～60 ℃.
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| CN103143257B (en) * | 2012-12-31 | 2016-06-29 | 三达膜科技（厦门）有限公司 | A kind of impurity-removing method of puerarin saccharification liquid |
| CN111617117A (en) * | 2019-12-31 | 2020-09-04 | 江苏久吾高科技股份有限公司 | Method and device for extracting effective components of radix isatidis |
| CN112675706A (en) * | 2020-12-30 | 2021-04-20 | 荣昌制药(淄博)有限公司 | Method for treating traditional Chinese medicine oral liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1943605A (en) * | 2006-10-20 | 2007-04-11 | 中山大学 | Process for preparing hypericum japonicum extract |
| CN1943735A (en) * | 2006-10-20 | 2007-04-11 | 中山大学 | The preparation method of a kind of radix ophiopogonis extract and its use |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1943605A (en) * | 2006-10-20 | 2007-04-11 | 中山大学 | Process for preparing hypericum japonicum extract |
| CN1943735A (en) * | 2006-10-20 | 2007-04-11 | 中山大学 | The preparation method of a kind of radix ophiopogonis extract and its use |
Non-Patent Citations (3)
| Title |
|---|
| 任建新.膜分离技术及其应用.《膜分离技术及其应用》.化学工业出版社,2003,(第1版),195-199. * |
| 戴光强 等.医院药学 医院中药学分册 进展篇.《医院药学 医院中药学分册 进展篇》.安徽科学技术出版社,2001,(第1版),89. |
| 戴光强等.医院药学 医院中药学分册 进展篇.《医院药学 医院中药学分册 进展篇》.安徽科学技术出版社,2001,(第1版),89. * |
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