CN101780114A - Extraction and separation method of effective constituents of traditional Chinese medicine - Google Patents
Extraction and separation method of effective constituents of traditional Chinese medicine Download PDFInfo
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- CN101780114A CN101780114A CN 201010126488 CN201010126488A CN101780114A CN 101780114 A CN101780114 A CN 101780114A CN 201010126488 CN201010126488 CN 201010126488 CN 201010126488 A CN201010126488 A CN 201010126488A CN 101780114 A CN101780114 A CN 101780114A
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Abstract
The invention relates to an extraction and separation method of effective constituents of a traditional Chinese medicine, which comprises the following steps that: (1) the traditional Chinese medicine is put an extraction device, and an extraction solvent is added to extract; (2) when extracting, an extract containing the effective constituents of the traditional Chinese medicine is conveyed to a separation device to be separated, and the separated remaining liquid is conveyed back to the extraction device to continue to be extracted; and (3) the extraction is stopped until the concentration of the target constituents of the extract is lower than a set value. The invention solves the problems that the existing traditional Chinese medicine has multiple extraction and separation steps, long consuming time, low yield of products and the like, the combination of extraction and separation devices with efficiency purification effect is screened out of various extraction and separation devices, accordingly, the target constituents with high purity and high yield can be directly obtained from the traditional Chinese medicine, thereby greatly shortening time and energy consumption, significantly reducing the use amount of the organic solvent, and protecting environment.
Description
Technical field
The present invention relates to a kind of extraction separation method of middle pharmaceutically active ingredient.
Background technology
The chemical constituent of Chinese medicine is very complicated, and what wherein play drug action is the close chemical constituents of one or more structures, and these chemical constituents are extracted and separated by effective means, can be used for the subsequent development and the production of tcm product.In tcm manufacturing process, the expense of separation and purification often accounts for bigger proportion, and the equipment that needs is many, and technical process is long.Usually the extraction and the separation process of Chinese medicine ingredients are made up of a series of unit operations, at first select for use suitable method that the target component in the Chinese crude drug is extracted in the solution, adopt suitable separation means such as centrifugal, filtration, extraction, chromatography, membrance separation etc. to obtain corresponding target product then.There are problems such as leaching process complexity, length consuming time, product yield be low in traditional Chinese medicine extraction separation method.Along with the continuous development of science and technology, people are exploring extraction separation method more efficiently always, to reach the purpose of High-efficient Production, reduce production costs simultaneously, make Chinese medicine possess more high-quality and more low-cost.Some modern high-new engineerings are constantly being used for reference Chinese medicine production, have developed multiple method for extraction and purification on traditional separation means basis.Therefore, the research of the high efficiency extraction of effective ingredient and separation method is the important component part of modernization of cmm in the Chinese medicine.
21 century, industrial technology has obtained great advance and development in the whole world, and monotechnics has reached very high level, and the production scale of industry and efficient are improved constantly.But development is still problem demanding prompt solution with the contradiction of contradiction, high investment and the low output polluted.Process integration is as a frontier of process engineering research, is that some new techniques, new technological process are integrated from angle more widely, just might solve the problems such as high-quality, energy-saving and environmental protection and sustainable development of process industrial from the source.
In recent years, the application of process integration was progressively expanded to aspects such as improving raw material availability, reduction pollutant emission and process operation.The yardstick of process integration at present is mainly in macro-scope, and its level of simplifying most is integrated in the single production process; Secondly, be energy between the different process process and the integrated consideration of uniting of material, constitute the process integration of enterprise-level; Highest level is to consider industry and coordinated development social, environment, forms Ecological Industrial.
Summary of the invention
Technical problem to be solved by this invention has been to overcome the extraction and many, the consuming time length of separation method step of existing Chinese medicine effective ingredient, problem such as consumption of organic solvent is big, productive rate is low, to extract with disjoint set and be formed in the operating unit, and from numerous extractions and segregation apparatus, filter out the extraction with efficient refining effect and the combination of segregation apparatus, thereby can directly from Chinese crude drug, obtain the target component of high-purity high yield, and significantly reduce the use amount of organic solvent, environmental protection.
The present invention solves the problems of the technologies described above by following technical proposals.
The invention provides a kind of extraction separation method of middle pharmaceutically active ingredient, it comprises the steps:
(1) Chinese medicine is placed extraction element, extract by extractant; Wherein said extraction element is one or more in decocting for Chinese herbal medicine extraction pot, dynamic circulation extraction element, jar group countercurrent extraction device, ultrasonic extraction device, microwave extraction device and the percolating extractor;
(2) in extraction, the extracting solution that will contain middle pharmaceutically active ingredient is delivered in the segregation apparatus and separates, and separates surplus liquid stream and is back to continuation participation extraction in the extraction element; Described segregation apparatus is fixed bed chromatographic separation device and/or expansion bed chromatographic separation device; Wherein, when extraction element was the decocting for Chinese herbal medicine extraction pot, segregation apparatus was not the fixed bed chromatographic separation device; When extraction element was ultrasonic extraction device, microwave extraction device or percolating extractor, segregation apparatus was not the expansion bed chromatographic separation device;
(3) the target component concentration of extracting solution stops to extract after being lower than setting value in the device to be extracted, collects target component.
Wherein, preferably, when described extraction element was the dynamic circulation extraction element, described segregation apparatus was fixed bed chromatographic separation device or expansion bed chromatographic separation device; When described extraction element was ultrasonic extraction device, described segregation apparatus was the fixed bed chromatographic separation device; When described extraction element was the combination of dynamic circulation extraction element and ultrasonic extraction device, described segregation apparatus was fixed bed chromatographic separation device or expansion bed chromatographic separation device.
Wherein, all kinds of extractants that the extractant that uses in the step (1) is used always when being used to extract Chinese medicine in this area can be selected according to a conventional method according to Chinese medicine among the present invention.
Wherein, the method of the collection target component described in the step (3) can adopt the method for this area routine to carry out, be preferably among the present invention: with the debris in washed with de-ionized water fixed bed chromatographic separation device or the expansion bed chromatographic separation device, with eluant eluting target component, collection contains the eluent of target component, gets final product.
What wherein, described Chinese medicine was preferable is the prepared slices of Chinese crude drugs or Chinese medicinal powder.Described Chinese medicine can be the various Chinese medicines that can extract with extractant, as Radix Salviae Miltiorrhizae or Fructus Gardeniae.
Preferably, if need more highly purified effective ingredient, can adopt normally used other methods of purification in this area that the target component that obtains through extraction separation method of the present invention is further purified.
Among the present invention, but above-mentioned optimum condition combination in any on the basis that meets this area general knowledge promptly gets the preferred embodiments of the invention.
All commercially available the getting of raw material, reagent that the present invention is used.
Positive progressive effect of the present invention is:
(1) especially the combination of specific extraction element and segregation apparatus has been carried out preferably among the present invention, in carrying out the process of extraction separation, the centering pharmaceutically active ingredient greatly reduces the consumption of organic solvent, make that the purification expense and the cost of investment of this extraction separation method are lower, environmental protection more.
(2) extraction separation method of the present invention save centrifugal in traditional extraction and the separation process, step such as filter, concentrate, the extraction of middle pharmaceutically active ingredient and separation function be integrated in the operating unit carry out, can directly from Chinese crude drug, obtain effective ingredient, have the characteristics of efficient height, step simplification;
(3) extraction separation method of the present invention adopts dynamic extraction to strengthen mass transport process, and therefore under the prerequisite that guarantees extraction efficiency and effective component yield, the operation cycle significantly shortens than traditional approach;
(4) the inventive method and device adopt channelization, totally-enclosed production process, have reduced the time of contact with air, can avoid the pollution of material;
(5) because the integrated extraction separation of the inventive method weak point consuming time can reduce some to thermally sensitive composition and hot time of contact, can prevent the problem of the yield reduction that its degraded brings, and reduce energy resource consumption.
Description of drawings
Fig. 1 is the schematic flow sheet of extraction separation method of the present invention, wherein F
EBe extracting solution stream, C
EBe extract concentration, the flow direction of footmark 1,2 expression stream; F
SBe separating medium stream, C
SBe separating medium concentration, the flow direction of footmark 1,2 expression stream.
The specific embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further, but the present invention is not limited.
Embodiment 1
(1) with technology purification Radix Salviae Miltiorrhizae of the present invention: add red rooted salvia 25 grams in the dynamic circulation extraction element of electrical heating chuck is housed, adds 500ml water again as extracting solvent, heating 15min makes the extraction solvent reach 100 ℃.Open infusion pump, cooled extracting solution is delivered in the expansion bed chromatographic separation device, and keeps this flow velocity to make the expansion bed bed maintain the height of 40cm.After extracting end, 1BV (137.5ml) deionized water is sent in the resin column of expansion bed from top to down, and the debris of absorption not in the flush away resin is imported the alcoholic solution of 5BV (687.5ml) 50% then from top to bottom, elution speed 2.4BV/h collects the salvianolic acid eluent.
(2) with traditional batch technology purification Radix Salviae Miltiorrhizae:, add 250ml water and extract each 1 hour three times as extracting solvent, decocting with red rooted salvia 25 grams.Merge extractive liquid,, through centrifugal, filtration, the concentrated concentrated solution that obtains, adding ethanol to concentration of alcohol is 75%, leaves standstill 12 hours.Filter back volatilization ethanol and upper prop and separate, with 1BV (137.5ml) deionized water eluting impurity component, use the alcoholic solution of 5BV (687.5ml) 50% then, elution speed 2.4BV/h collects eluent, obtains the salvianolic acid B product after the drying.
The present invention compares with traditional batch (-type) extraction process condition, and the every index comparing result of leaching process is as shown in table 1:
Table 1
By table 1 as can be seen, the technology of extraction separation Radix Salviae Miltiorrhizae of the present invention is simple, and consumption of organic solvent, energy consumption and operating time significantly reduce, and the extraction ratio of target product, yield and purity all are improved, and has production application and is worth.
Embodiment 2
(1) with technology purification Fructus Gardeniae of the present invention: in the decocting for Chinese herbal medicine jar, add Fructus Gardeniae medical material 25 grams, add 250ml water again as extracting solvent, be heated to the interior temperature of extraction pot and reach 100 ℃, cooled extracting solution is delivered in the expansion bed chromatographic separation device, and keeps this flow velocity to make the expansion bed bed maintain the height of 40cm.After extracting end, send into 1BV (137.5ml) deionized water in the resin column from top to down, be the debris of absorption in the flush away resin, use the alcoholic solution eluting cylinder of 5BV 30%, 60% then respectively, substep is collected and is obtained iridoid glycoside constituents and crocin constituents.
(2) with traditional batch technology purification Fructus Gardeniae:, add 250ml water and extract each 1 hour three times as extracting solvent, decocting with Fructus Gardeniae medical material 25 grams.Merge extractive liquid,, through centrifugal, filtration, the concentrated concentrated solution that obtains, adding ethanol to concentration is 75%, leaves standstill 12 hours.Filter back volatilization ethanol and upper prop and separate, with 1BV (137.5ml) deionized water eluting impurity component, use the alcoholic solution eluting cylinder of 5BV 30%, 60% then respectively, substep is collected and is obtained iridoid glycoside constituents and crocin constituents.
The present invention compares with traditional batch (-type) extraction process condition, and the every index comparing result of leaching process is as shown in table 2:
Table 2
By contrast as can be seen, the technology of extraction separation Fructus Gardeniae of the present invention is simple, and consumption of organic solvent, energy consumption and operating time significantly reduce, and the yield of target product crocin-I is largely increased, and has production application and is worth.
Claims (5)
1. the extraction separation method of pharmaceutically active ingredient in a kind is characterized in that it comprises the steps:
(1) Chinese medicine is placed extraction element, extract by extractant; Wherein, described extraction element is one or more in decocting for Chinese herbal medicine extraction pot, dynamic circulation extraction element, jar group countercurrent extraction device, ultrasonic extraction device, microwave extraction device and the percolating extractor;
(2) when extracting, the extracting solution of pharmaceutically active ingredient is delivered in the segregation apparatus and separates in will containing, and will separate surplus liquid and carry back and proceed extraction in the extraction element; Described segregation apparatus is fixed bed chromatographic separation device and/or expansion bed chromatographic separation device; Wherein, when extraction element was the decocting for Chinese herbal medicine extraction pot, segregation apparatus was not the fixed bed chromatographic separation device; When extraction element was ultrasonic extraction device, microwave extraction device or percolating extractor, segregation apparatus was not the expansion bed chromatographic separation device;
(3) after the target component concentration of extracting solution is lower than setting value in the device to be extracted, stop to extract, collect target component.
2. the extraction separation method of pharmaceutically active ingredient in as claimed in claim 1, it is characterized in that: when described extraction element was the dynamic circulation extraction element, described segregation apparatus was fixed bed chromatographic separation device or expansion bed chromatographic separation device; When described extraction element was ultrasonic extraction device, described segregation apparatus was the fixed bed chromatographic separation device; When described extraction element was the combination of dynamic circulation extraction element and ultrasonic extraction device, described segregation apparatus was fixed bed chromatographic separation device or expansion bed chromatographic separation device.
3. the extraction separation method of pharmaceutically active ingredient in as claimed in claim 1, it is characterized in that: the method for the collection target component described in the step (3) is: with the debris in washed with de-ionized water fixed bed chromatographic separation device or the expansion bed chromatographic separation device, with eluant eluting target component, collection contains the eluent of target component, gets final product.
4. as the extraction separation method of each described middle pharmaceutically active ingredient in the claim 1～3, it is characterized in that described Chinese medicine is the prepared slices of Chinese crude drugs or Chinese medicinal powder.
5. as the extraction separation method of each described middle pharmaceutically active ingredient in the claim 1～4, it is characterized in that described Chinese medicine is Radix Salviae Miltiorrhizae or Fructus Gardeniae.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105287280A (en) * | 2015-10-20 | 2016-02-03 | 上海承曜生物科技有限公司 | Plant allergy-relieving agent and preparation method thereof |
| CN113402635A (en) * | 2021-06-18 | 2021-09-17 | 汕头大学 | Method for separating and purifying heparin by expanded bed countercurrent chromatography |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1973941A (en) * | 2006-11-10 | 2007-06-06 | 清华大学 | Integrated process and apparatus for extracting and separating effective Chinese medicine components |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1973941A (en) * | 2006-11-10 | 2007-06-06 | 清华大学 | Integrated process and apparatus for extracting and separating effective Chinese medicine components |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105287280A (en) * | 2015-10-20 | 2016-02-03 | 上海承曜生物科技有限公司 | Plant allergy-relieving agent and preparation method thereof |
| CN105287280B (en) * | 2015-10-20 | 2018-06-22 | 上海承曜生物科技有限公司 | A kind of plant Shu Min agent and preparation method thereof |
| CN113402635A (en) * | 2021-06-18 | 2021-09-17 | 汕头大学 | Method for separating and purifying heparin by expanded bed countercurrent chromatography |
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Application publication date: 20100721 |