CN103641716A - Method for extracting refined chicoric acid - Google Patents
Method for extracting refined chicoric acid Download PDFInfo
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- CN103641716A CN103641716A CN201310654618.5A CN201310654618A CN103641716A CN 103641716 A CN103641716 A CN 103641716A CN 201310654618 A CN201310654618 A CN 201310654618A CN 103641716 A CN103641716 A CN 103641716A
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- chicoric acid
- extracting
- extraction
- refining
- elutriant
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention discloses a method for extracting refined chicoric acid. According to the method, echinacea raw materials are treated by steps of extracting by ultrasonic waves, decompressing and concentrating in vacuum, sampling macroporous resin, washing with de-ionized water, eluting, decompressing and concentrating in vacuum, spraying and drying, detecting, crushing, and packaging and storing. In the extraction process of the chicoric acid, ultrasonic wave assisting is utilized to improve the extraction rate of the chicoric acid; the problems that the extraction time in the extraction process is long and the extraction rate is low are effectively improved; a macroporous resin adsorption technology is used for removing impurities in an alcohol extracting solution and effective components are enriched; the problems that in the prior art, the impurity removing rate is low, the loss of effective components is great, the purity of later-period products is low and the like are solved.
Description
Technical field
The present invention relates to a kind of method of extracting refining chicoric acid, be specifically related to a kind of ultrasonic technology of using from the method for echinacea purpurea extraction and Macroporous Adsorption Resin chicoric acid.
Background technology
Chicoric acid (Chicoric acid) belongs to phenolic acids, and chemical name is (2R, 3R)-2, two [[(E)-3-(3, the 4-dihydroxy phenyl) third-2-alkene acyl] oxygen] succinic acid of 3-, molecular formula C
22h
18o
12, molecular weight is 474.37, its chemical structural formula is:
Chicoric acid is one of immune active ingredient very important in witloof and echinacea purpurea.Pharmacological research in recent years shows, chicoric acid has the immunologic function of enhancing and anti-inflammatory action, and can suppress Unidasa, and protection collagen protein avoids causing the impact of the free radical of degraded, also has the effect that suppresses HIV-1 and HIV-1 intergrase.
At present both at home and abroad about the Research Literature report of chicoric acid, being mainly limited to chicoric acid in the detection, echinacea purpurea of chicoric acid content in medicinal material and preparation just carries, utilizes preparative high pressure liquid chromatography to prepare the aspects such as witloof acidity scale product, prior art generally adopts the techniques such as alcohol extracting-water precipitating at chicoric acid aspect refining, remove the impurity such as resin in extracting solution, fat-soluble pigment, reach purifying, active constituent-enriched object.
In existing extraction echinacea purpurea, the equipment great majority of chicoric acid, for band stirs multi-function extractor, drop into raw material echinacea purpurea in extractor, add 60% ethanol as extracting solvent, under the condition of 70 ℃, stir and extract.The multi-function extractor that adopts band to stir extracts chicoric acid in echinacea purpurea, needs to extract 3 times, and first pass extraction time is 2 hours, and second time and the 3rd time is all 1.5 hours, and extraction time is long, makes the production cost increase of enterprise, and production efficiency is low; The extraction yield that extracts chicoric acid with the present invention is on average in 83.5% left and right, and extraction yield is lower, has caused the waste of natural resources of Chinese medicinal materials, does not meet the strategy of national sustainable development.
Aspect chicoric acid refining, existing process using alcohol extracting-water precipitating is sent the impurity of removing in extracting solution.Adopting this method is first that solvent extracts with ethanol, can avoid the leaching of the compositions such as starch, protein and lymphatic temperament, after adding water treatment, can remove the impurity such as resin, fat-soluble pigment in alcohol extract, the method amount of water is difficult to control, chicoric acid in alcohol extract is water-soluble poor, easily by impurity, wrapped up and precipitatedly remove together, loss of effective components is larger; In addition, adopting said method, Impurity removal is not thorough, and later stage product purity is only 15% left and right, and purity is lower.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of method of extracting refining chicoric acid, in the leaching process of chicoric acid, utilize ultrasonic wave to assist, improve the extraction yield of chicoric acid; In solution leaching process, extraction time is grown and the low problem of extraction yield.Adopt macroporous adsorption resin technology to replace traditional alcohol extracting-water precipitating technology to remove the impurity in alcohol extract, active constituent-enriched; The problem such as solved that conventional art removal of impurity is low, loss of effective components is large and later stage product purity is low
A kind of method of extracting refining chicoric acid provided by the invention, comprises the steps:
1) dry echinacea purpurea is cut into the pipe nipple of length 2-3cm with medicine cutter, puts in the multi-function extractor with ultrasonic generator;
2) to the ethanol that adds 60% in the extractor having fed intake, extract, extract altogether twice, omnidistance stirring in leaching process, stirring velocity is 20 turn/min;
3) extracting solution, after Plate Filtration, concentrates with decompression concentrator, and to reclaim ethanol to concentrated solution be extracting liquid volume 1/10;
4) with macroporous resin, adsorb and wash-out;
5) collect elutriant, carry out vacuum concentration, when the proportion that is concentrated to concentrated solution is 1.2-1.25, with spray-drying tower, spray and be dried, obtain the chicoric acid that purity is the higher degree of 22% left and right.
Further, in described step 2, the material liquid volume of extracted twice is 1:8 than first pass, is for second time 1:7, and extraction time is 50min for the first time, is 30min for the second time.
Further, in described step 2, extracted twice temperature is 50 ℃, and the power of ultrasonic generator is 200W.
Further, the thickening temperature in described step 3 is 70 ℃, and the concentration of guaranteeing upper prop liquid is 3-4g/L.
Further, in described step 4, the AB-8 type macroporous adsorbent resin of handling well is utilized wet method dress post to insert in chromatography column, the upper prop concentration of chicoric acid extracting solution is 3-4g/L, the 2<PH<4 of upper prop liquid, loading speed is 1-1.5BV/h (BV is resin volume, and 1BV is a resin volume).
Further, after end of the sample, first use the washed with de-ionized water impurity of 2-3BV, then carry out wash-out with the elutriant of 5-6BV, the ethanolic soln that elutriant is 30%, elution speed is 1-1.5BV/h, the volume of elutriant is 5-6BV.
Beneficial effect of the present invention is:
1, overcome traditional extraction technology extraction yield low, the shortcoming that extraction time is long.Ultrasonic energy produces and transmits powerful energy, makes liquid be torn into a lot of little holes, produces cavitation effect.Hyperacoustic cavitation effect can produce great pressure and cause by the fragmentation of crushed material cell walls and whole organism; Meanwhile, the oscillating action that ultrasonic wave produces has been strengthened release, diffusion and the dissolving of intracellular organic matter, is conducive to the extraction of effective constituent in born of the same parents.In ultrasonic-assisted extraction echinacea purpurea, in the process of chicoric acid, ultrasonic wave, by cytoclasis, makes chicoric acid can enter fast and efficiently extraction solvent, thereby shortens extraction time, increases extraction efficiency.
Hyperacoustic optimum extraction temperature is at 40-60 ℃, and Heating temperature is low.The extraction temperature of conventional art is at 70 ℃, and the extraction temperature of this technique is 50 ℃, has reduced due to the high destruction to effective ingredient of temperature, has also reduced energy consumption simultaneously.Intensified by ultrasonic wave traditional Chinese medicine extraction can obtain optimum extraction rate at 24-40 minute conventionally, and extraction time shortens more than 2/3 greatly compared with traditional method, and medicinal material raw material disposal amount is large.The extraction yield of traditional extraction technology is 83.5% left and right, and after using this technology, extraction yield is by the checking of large-scale production, and average extraction yield is 94% left and right, and extraction yield has increased by 10.5%, has realized making full use of of natural resources of Chinese medicinal materials.
2, absorption with macroporous adsorbent resin isolation technique is to adopt macroporous resin from Chinese medicine and Chinese medicine compound prescription, selectively to adsorb effective constituent wherein, that removes invalid components a kind ofly extracts refining novel process, and it has, and selectivity is good, adsorptive capacity is large, manipulation of regeneration is convenient, absorption is rapid, desorb is easy and simple operation and other advantages.Adopt conventional art refine chicoric acid, have that removal of impurity is low, loss of effective components greatly and the problem such as later stage product purity is low.
The AB-8 resin of institute of the present invention Select to use, it is when absorption chicoric acid extracting solution, selectivity to chicoric acid is high, can optionally adsorb chicoric acid, few especially to other invalid components absorption, during wash-out, 30% ethanol elutes chicoric acid, and most impurity can not be eluted, the removing method of impurity is different, makes loss the present invention of effective constituent than conventional art much less.Removal of impurity of the present invention is high more a lot of than routine techniques; Because removal of impurity is high, the purity of later stage product improves a lot, and the chicoric acid average purity of conventional art gained is 15% left and right, and uses the chicoric acid average purity of gained of the present invention up to 22% left and right, and purity exceeds 7% than conventional art.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention
Embodiment
As shown in Figure 1, a kind of method of extracting refining chicoric acid, comprises the steps:
1) dry echinacea purpurea is cut into the pipe nipple of length 2-3cm with medicine cutter, puts in the multi-function extractor with ultrasonic generator;
2) to the ethanol that adds 60% in the extractor having fed intake, extract, extract altogether twice, omnidistance stirring in leaching process, stirring velocity is 20 turn/min; The material liquid volume of extracted twice is 1:8 than first pass, is for second time 1:7, and extraction time is 50min for the first time, is 30min for the second time; Extract temperature and be 50 ℃, the power of ultrasonic generator is 200W.
3) extracting solution, after Plate Filtration, concentrates with decompression concentrator, and thickening temperature is 70 ℃, and to reclaim ethanol to concentrated solution be extracting liquid volume 1/10, and the concentration of guaranteeing upper prop liquid is 3-4g/L.
4) with macroporous resin, adsorb and wash-out; Utilize wet method dress post to insert in chromatography column the AB-8 type macroporous adsorbent resin of handling well, the upper prop concentration of chicoric acid extracting solution is 3-4g/L, the 2<PH<4 of upper prop liquid, and loading speed is 1-1.5BV/h.Described BV is resin volume, and 1BV is a resin volume.After end of the sample, first use the washed with de-ionized water impurity of 2-3BV, then carry out wash-out with the elutriant of 5-6BV, the ethanolic soln that elutriant is 30%, elution speed is 1-1.5BV/h, the volume of elutriant is 5-6BV.
5) collect elutriant, carry out vacuum concentration, when the proportion that is concentrated to concentrated solution is 1.2-1.25, with spray-drying tower, spray and be dried, obtain the chicoric acid that purity is the higher degree of 22% left and right.
The above,, only to the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various modifications and variations.Every in claim limited range of the present invention, any modification of making, be equal to replacement, improvement etc., all should be within protection scope of the present invention.
Claims (6)
1. extract a method for refining chicoric acid, it is characterized in that comprising the steps:
1) dry echinacea purpurea is cut into the pipe nipple of length 2-3cm with medicine cutter, puts in the multi-function extractor with ultrasonic generator;
2) to the ethanol that adds 60% in the extractor having fed intake, extract, extract altogether twice, omnidistance stirring in leaching process, stirring velocity is 20 turn/min;
3) extracting solution, after Plate Filtration, concentrates with decompression concentrator, and to reclaim ethanol to concentrated solution be extracting liquid volume 1/10;
4) with macroporous resin, adsorb and wash-out;
5) collect elutriant, carry out vacuum concentration, when the proportion that is concentrated to concentrated solution is 1.2-1.25, with spray-drying tower, spray and be dried, obtain the chicoric acid that purity is the higher degree of 22% left and right.
2. a kind of method of extracting refining chicoric acid according to claim 1, is characterized in that: in described step 2, the material liquid volume of extracted twice is 1:8 than first pass, is for second time 1:7, and extraction time is 50min for the first time, is 30min for the second time.
3. a kind of method of extracting refining chicoric acid according to claim 1, is characterized in that: in described step 2, extracted twice temperature is 50 ℃, and the power of ultrasonic generator is 200W.
4. a kind of method of extracting refining chicoric acid according to claim 1, is characterized in that: the thickening temperature in described step 3 is 70 ℃, and the concentration of guaranteeing upper prop liquid is 3-4g/L.
5. a kind of method of extracting refining chicoric acid according to claim 1, it is characterized in that: in described step 4, the AB-8 type macroporous adsorbent resin of handling well is utilized wet method dress post to insert in chromatography column, the upper prop concentration of chicoric acid extracting solution is 3-4g/L, the 2<PH<4 of upper prop liquid, loading speed is 1-1.5BV/h.
6. a kind of method of extracting refining chicoric acid according to claim 5, it is characterized in that: the washed with de-ionized water impurity of first using 2-3BV after end of the sample, with the elutriant of 5-6BV, carry out wash-out again, elutriant is 30% ethanolic soln, elution speed is 1-1.5BV/h, and the volume of elutriant is 5-6BV.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104257713A (en) * | 2014-09-11 | 2015-01-07 | 华南农业大学 | Echinacea purpurea (L.) Moench root oral liquid as well as preparation method and application thereof to preparation of swine and chicken vaccine immunopotentiators |
| CN104257714A (en) * | 2014-09-11 | 2015-01-07 | 华南农业大学 | Echinacea purpurea (L.) Moench root granules as well as preparation method and application thereof to preparation of swine and chicken vaccine immunopotentiators |
| CN109867603A (en) * | 2019-04-27 | 2019-06-11 | 蚌埠学院 | A kind of purification process of Cichoric acid |
| CN111714532A (en) * | 2020-07-20 | 2020-09-29 | 吉林省宏久生物科技股份有限公司 | Echinacea purpurea extract and preparation method thereof |
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| CN101148410A (en) * | 2007-10-30 | 2008-03-26 | 聊城大学 | Method for extracting high pure chicoric acid from Coneflower |
| CN102161620A (en) * | 2011-03-10 | 2011-08-24 | 湖南师范大学 | Method for non column chromatography separation and purification of witloof acid from Echinacea purpurea extractive |
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| CN101032541A (en) * | 2006-07-28 | 2007-09-12 | 成都地奥九泓制药厂 | Echinacea purpurea extractive and the preparing method and the content measuring method |
| CN101148410A (en) * | 2007-10-30 | 2008-03-26 | 聊城大学 | Method for extracting high pure chicoric acid from Coneflower |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104257713A (en) * | 2014-09-11 | 2015-01-07 | 华南农业大学 | Echinacea purpurea (L.) Moench root oral liquid as well as preparation method and application thereof to preparation of swine and chicken vaccine immunopotentiators |
| CN104257714A (en) * | 2014-09-11 | 2015-01-07 | 华南农业大学 | Echinacea purpurea (L.) Moench root granules as well as preparation method and application thereof to preparation of swine and chicken vaccine immunopotentiators |
| CN109867603A (en) * | 2019-04-27 | 2019-06-11 | 蚌埠学院 | A kind of purification process of Cichoric acid |
| CN109867603B (en) * | 2019-04-27 | 2022-02-22 | 蚌埠学院 | Method for purifying chicoric acid |
| CN111714532A (en) * | 2020-07-20 | 2020-09-29 | 吉林省宏久生物科技股份有限公司 | Echinacea purpurea extract and preparation method thereof |
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Application publication date: 20140319 |