CN102553294A - Method for forcedly extracting effective components of Chinese herbal medicine by using magnetic adsorbent under coordination of ultrasonic waves - Google Patents
Method for forcedly extracting effective components of Chinese herbal medicine by using magnetic adsorbent under coordination of ultrasonic waves Download PDFInfo
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Abstract
The invention relates to a method for forcedly extracting effective components of a Chinese herbal medicine by using a magnetic adsorbent under the coordination of ultrasonic waves. The method comprises the following steps of: firstly, mixing the Chinese herbal medicin, the magnetic adsorbent and an extraction solvent, and placing the mixture in an ultrasonic extractor at room temperature to carry out ultrasonic extraction; then, magnetically separating and recycling the magnetic adsorbent, filtering to obtain filtrate, desorbing the magnetic adsorbent to obtain desorption liquid, and merging the filtrate and the desorption liquid to obtain extraction solution, wherein when the magnetic adsorbent is enough, the filtrate can be ignored, and the desorption liquid is used as the extraction solution. The method has the advantages of simple process, high extraction speed, high extraction ratio, mild extraction condition (room temperature), high selectivity, recyclable solvent, high product extraction purity and the like and is very suitable for the rapid, high-selectivity and efficient extraction of heat sensitive components in a Chinese herbal medicine product.
Description
Technical field
The present invention relates to Chinese herbal medicine purification technique field, relate in particular to a kind of method of ultrasonic synergistic magnetic adsorbent strengthening extraction Chinese herbal medicine effective ingredients.
Background technology
Chinese herbal medicine contains many effective components as a kind of pure natural plant medicine, can treat many kinds of diseases; For realize that effective utilization of Chinese herbal medicine is needed these effective components are extracted from plant tissue; Through further separation and purification, process Chinese patent drug and various preparation again, these Chinese herbal and crude drugs preparationses are because of pure natural; Toxic and side effect is few, and extremely people's likes.
Utilize in the process at Chinese herbal medicine effective ingredients, extractive technique is crucial.Conventional method of extraction is to adopt organic solvent extraction, as: heat reflow method and soxhlet extraction, it is big that these methods exist the organic solvent consumption, consuming time longer, and high temperature causes the thermal sensitivity composition because of defectives such as degraded losses.For addressing these problems; People have developed some new extracting process like supercritical fluid extraction, microwave auxiliary extraction method and ultrasonic wave auxiliary extraction method in recent years, these new abstraction techniques overcome conventional art defective aspect all obtained good effect.
CN 102283888A discloses the method for general flavone in a kind of ultrasonic wave auxiliary extraction cassia seed; Be that petroleum ether degreasing is used in cassia seed raw material drying, pulverizing back; Then through the auxiliary ethanol lixiviate of ultrasonic wave; Leave and take supernatant after leaching liquor is centrifugal, promptly get the cassia seed extractive of general flavone after supernatant is evaporated to pulpous state and drying and crushing.
CN 1256142A relates to active component supercritical CO 2 extraction technology method in the salviamiltiorrhizabung; With carrying out supercritical carbon dioxide cyclic countercurrent extraction and separate after the pelletizing of red sage root rhizome; With obtain have medical curative effect active material in extraction process; Extract with first entrainer earlier; To obtain with the tanshinone is master's active material, treat that the tanshinone material comes together basically to use second entrainer instead after finishing and continue extraction and lock out operation, and be master's active material to obtain with danshensu and protocatechualdehyde.
The action principle of ultrasonic wave auxiliary extraction method is: utilize ultrasonic wave to increase molecular motion of material frequency and speed; Strengthen the solvent penetration power, improve medicine dissolution rate and stripping number of times, thereby accelerate extraction rate; Just so-called cavitation effect, the also subsidiary simultaneously perturbation action that machinery is arranged.According to this principle, total mass transfer rate equation N from the phase border
A=K
CΔ C can release, and the essence of ultrasonic wave effect is to have improved the overall mass transfer coefficient K of Chinese herbal medicine effective ingredients
CAnd according to this mass transfer rate equation, the applicant has successfully developed the suction-operated that utilizes magnetic adsorbent and has caused between extract and matrix one big concentration difference, thereby the magnetic adsorbent auxiliary extraction of strengthening extraction rate and extraction rate is technological greatly.
Based on this; If ultrasonic technology and magnetic adsorbent auxiliary extraction technology are combined, according to total mass transfer rate equation, this technology will be strengthened the extraction mass transport process from mass tranfer coefficient and concentration difference two aspects; Utilize its synergy, be expected to provide a kind of brand-new efficient abstraction technique.Therefore ultrasonic synergistic magnetic adsorbent strengthening extraction technology combines the advantage of two kinds of technology; Have that technology is simple, extraction rate is fast, recovery rate is high, extract temperature low (room temperature), selectivity height, solvent reusable edible, extract the product purity advantages of higher, be very suitable for quick, high selectivity, the high efficiency extraction of thermal sensitivity composition in the tcm product.
Summary of the invention
The object of the present invention is to provide a kind of ultrasonic synergistic magnetic adsorbent strengthening extraction method of new and effective Chinese herbal medicine effective ingredients, overcome the defective of existing extracting process.Advantages such as that this method has is simple to operate, rate of extraction is fast, extraction yield is high, carry out under the room temperature, solvent reusable edible are very suitable for the extraction of active ingredient in the Chinese herbal medicine.
For reaching this purpose, the present invention adopts following technical scheme:
A kind of method of ultrasonic synergistic magnetic adsorbent strengthening extraction Chinese herbal medicine effective ingredients at first with Chinese herbal medicine, magnetic adsorbent and extraction solvent, places the Extraction by Ultrasound device to carry out ultrasonic Extraction; Magnetic Separation and Recovery magnetic adsorbent, and desorb then gets stripping liquid and is extract.
Preferably, in the ultrasonic Extraction process, use recirculated cooling water to keep the extraction temperature and be room temperature, cause thermal sensitivity composition degraded loss, make this method more be applicable to the extraction of the high selectivity of the active ingredient of thermal sensitivity in the Chinese herbal medicine to avoid Yin Gaowen.Filtrating that filtration extraction mixed liquor produces after can magnetic being separated in addition and stripping liquid are together as extract.When magnetic adsorbent is enough, can ignore amount of filtrate, stripping liquid is extract.
Chinese herbal medicine according to the invention is simple or multi-flavor medicine, is preferably the mixture of the red sage root, the banksia rose, rhizoma zingiberis, dried orange peel, rhizoma atractylodis macrocephalae or at least two kinds.Form is preferably Powdered or graininess, can increase the specific area of Chinese herbal medicine, increases and the contact area of extracting solvent, thereby helps improving recovery rate.
Magnetic adsorbent of the present invention is the microballoon with superparamagnetism, the aglucon of the affine absorption effective component of surface-functionalized modification ability; Its average grain diameter is 10nm～500 μ m, for example can select 12nm, 50nm, and 100nm, 900nm, 2 μ m, 80 μ m, 220 μ m, 300 μ m, 450 μ m, 490 μ m etc. are used for the present invention, preferred 30nm～2 μ m, further preferred 1 μ m; Add 5～1000mg magnetic adsorbent in every gram Chinese herbal medicine, add magnetic adsorbent 20mg, 100mg, 250mg, 380mg, 500mg, 760mg, 880mg, 980mg etc. in for example every gram Chinese herbal medicine.
Aglucon of the present invention comprises that molecularly imprinted polymer aglucon, hydrogen bond type aglucon, solvay-type aglucon, electrostatic aglucon, mixed type aglucon all can be used for embodiment of the present invention, and those skilled in the art can carry out choose reasonable according to industry experience and actual conditions.
Described molecularly imprinted polymer aglucon is to be that template and suitable monomers prepare with the active component of Chinese herbal medicine or its analog; The preferred flavones of described template, polyphenol, steroidal, alkaloid.The preparation of molecularly imprinted polymer aglucon and the selection of proper monomer can be carried out according to technical staff's domain knowledge.Described template is active component or its analog in the Chinese herbal medicine that will extract, and the technical staff can select flexibly.
Extraction solvent according to the invention is mixture, preferred water and/or the ethanol of water, methyl alcohol, ethanol, n-hexane, acetone, chloroform or at least two kinds.Traditional Chinese medicine extraction solvent commonly used has: water, hydrophilic organic solvent, lipophilic organic solvent.Water is a kind of strong polar solvent, and hydrophilic composition in the Chinese herbal medicine can both be gone out by water-soluble like the not too big polysaccharide of inorganic salts, carbohydrate, molecule, tannin, amino acid, protein, acylate, alkaloid salt and glucoside etc.The just general said and miscible organic solvent of water of hydrophilic organic solvent, like ethanol, methyl alcohol, acetone etc., the most frequently used with ethanol.The solubility property of ethanol is relatively good, and is stronger to the penetration capacity of Chinese herbal medicine cell.The character of methyl alcohol is similar with ethanol, boiling point lower (64 ℃), but toxic, should note during use.Lipophilic organic solvent is exactly the organic solvent that generally said and water can not be miscible, like benzinum, benzene, chloroform, ether, ethyl acetate, dichloroethanes etc.
The consumption that extracts solvent is 5～30 times of medium-height grass dose, and for example every g Chinese herbal medicine uses and extracts solvent 5.5g, 7g, 10g, 11g, 13.8g, 20g, 24.2g, 28g etc., preferred 5～15 times, further preferred 10 times.
The said ultrasonic Extraction time is 1～180min, and for example the technical staff can select 1.2min, 3min, and 8min, 20min, 85min, 100min, 135min, 160min, the 178min equal time is used for the present invention, preferred 1～40min, further preferred 20min.Ultrasonic power is 50～500W, 52W for example, 85W, 135W, 180W, 220W, 300W, 400W, 490W etc., preferred 100～300W, further preferred 200W.
In the ultrasonic Extraction process, can stir simultaneously, be beneficial to efficiently carrying out of leaching process.Said alr mode can be the paddle stirring or integral body places shaking table to vibrate.Other stirring or modes of oscillation that adsorbing and extracting process is more thoroughly carried out all can be selected according to actual conditions by those skilled in the art, and speed is 50～2000rpm, 60rpm for example, 120rpm; 187rpm, 280rpm, 450rpm; 800rpm, 1250rpm, 1600rpm; 1980rpm etc. are preferably 50～600rpm, further preferred 200rpm.
The used magnet of magnetic separation process according to the invention is for having ferromagnetic electromagnet or permanent magnet.
Said separating smokes absorbent for formulated with methyl alcohol or ethanol and acetic acid; Its volume ratio is 3: 1～12: 1, for example 3.5: 1, and 5: 1,6.8: 1,8: 1,10.4: 1,11: 1,11.8: 1 etc., preferred 6: 1～10: 1, further preferred 9: 1.
Magnetic separation process of the present invention is for the mixed liquor of magnetic adsorbent with Chinese herbal medicine matrix and extract separated; Concrete operations are: magnet is put into a teat glass; With moving back and forth fully to catch magnetic adsorbent in the mixed liquor of this teat glass after extraction, remove magnet then, with a small amount of absorbent drip washing test tube outer surface; Magnetic adsorbent is split away off, carry out next step desorb.
The invention provides a kind of method of ultrasonic synergistic magnetic adsorbent strengthening extraction Chinese herbal medicine effective ingredients; Concrete operations are following: at first with Chinese medicine, magnetic adsorbent and extraction solvent; Place the Extraction by Ultrasound device to carry out ultrasonic Extraction; Use recirculated cooling water to keep the extraction temperature and be room temperature, simultaneously it is constantly stirred or puts into constant temperature oscillator and vibrate; Magnetic Separation and Recovery magnetic adsorbent then, concrete operations as stated.Filtering out Chinese herbal medicine matrix must filtrate, and magnetic adsorbent desorb in the mixed liquor of methyl alcohol or ethanol and acetic acid is got stripping liquid, and merging filtrate and stripping liquid get extract, detect with liquid chromatogram.
In the desorption process of the present invention how many direct relations of desorption efficiency the size of extraction yield, therefore need that separating of being adopted smoked absorbent and be optimized, desorb is complete as far as possible.
Can provide bigger concentration difference and ultrasonic wave energy that big mass tranfer coefficient is provided based on magnetic adsorbent, according to total mass transfer rate equation N
A=K
CΔ C the present invention proposes the new abstraction technique of ultrasonic synergistic magnetic adsorbent strengthening extraction Chinese herbal medicine effective ingredients.Thereby hyperacoustic cavitation effect and mechanical disturbance interaction energy improve mass tranfer coefficient strengthening extraction speed greatly; Thereby magnetic adsorbent can optionally adsorb the concentration difference that active ingredient causes active ingredient; Thereby reach the purpose of the strengthening extraction of high selectivity; In addition owing to the concentration of active ingredient in the extraction solution is kept very low concentration all the time; Be equivalent to fresh solvent Chinese herbal medicine matrix extracted all the time, so can obtain very high extraction yield; Because the extractant that is adopted only is equivalent to the mass transfer media, so can recycle.
Therefore the extracting process that the present invention adopted has that technology is simple, extraction rate is very fast, recovery rate is high, extracts temperature low (room temperature), selectivity height, solvent reusable edible, extract the product purity advantages of higher, is very suitable for quick, high selectivity, the high efficiency extraction of thermal sensitivity composition in the tcm product.
Description of drawings
All kinds of extraction process effects compared block diagram when Fig. 1 was 5min.
All kinds of extraction process effects compared block diagram when Fig. 2 was 10min.
Down in the face of further explain of the present invention.But following instance only is a simple and easy example of the present invention, does not represent or limits rights protection scope of the present invention, and interest field of the present invention is as the criterion with claims.
The specific embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical case of the present invention but non-restrictive example is following:
Embodiment 1
Extracting process: add the 30ml n-hexane in the 3g Danshen Root, adding average grain diameter again is the magnetic molecularly imprinted microballoon 100mg of 200nm, then integral container is placed the Extraction by Ultrasound device; Use recirculated cooling water to keep the extraction temperature and be room temperature, under the no stirring action, ultrasonic Extraction 5min; Sample magnetic is separated; Filtering out Chinese herbal medicine matrix must filtrate, with magnetic molecularly imprinted microballoon in methyl alcohol: acetic acid (9: 1, v/v) desorb gets stripping liquid in the mixed solution; Merging filtrate and stripping liquid get extract, and three kinds of content of effective detect with high performance liquid chromatography.
The result: ultrasonic synergistic magnetic adsorbent strengthening extraction method is respectively the content of three kinds of active ingredient Cryptotanshinones, tanshinone 1 and tanshinone 2a in the red sage root: 0.206mg/g, 0.136mg/g and 0.461mg/g.
Comparative example: for further proving the effect of ultrasonic synergistic magnetic adsorbent strengthening extraction; The effect of its effect of extracting and room temperature oscillation extraction and magnetic adsorbent auxiliary extraction is compared; Extraction conditions is respectively: room temperature oscillation extraction condition: add the 30ml n-hexane in the 3g danshen powder, vibration 5min under room temperature, 200rpm; Magnetic adsorbent auxiliary extraction condition: add the 10ml n-hexane in the 1g danshen powder, add the 100mg magnetic adsorbent, vibration 5min under the 200rpm vibration.
The result is as shown in Figure 1, can know: ultrasonic synergistic magnetic adsorbent auxiliary extraction technology three kinds of extraction ratio of effective constituents in the red sage root are all high than corresponding room temperature oscillation extraction and magnetic adsorbent auxiliary extraction.Show: show that ultrasonic wave and magnetic adsorbent have synergy really, greatly the strengthening extraction process.
Embodiment 2
Extracting process: add the 30ml n-hexane in the 3g Danshen Root, adding average grain diameter is the magnetic molecularly imprinted microballoon 100mg of 200nm, then integral container is placed the Extraction by Ultrasound device; Use recirculated cooling water to keep the extraction temperature and be room temperature, under the no stirring action, extract 10min; To sample magnetic Separation and Recovery magnetic microsphere; Filtering out Chinese herbal medicine matrix must filtrate, with magnetic molecularly imprinted microballoon in methyl alcohol: acetic acid (9: 1, v/v) desorb gets stripping liquid in the mixed solution; Merging filtrate and stripping liquid get extract, and three kinds of content of effective detect with high performance liquid chromatography.
The result: ultrasonic synergistic magnetic adsorbent strengthening extraction method is respectively the content of three kinds of active ingredient Cryptotanshinones, tanshinone 1 and tanshinone 2a in the red sage root: 0.249mg/g, 0.157mg/g and 0.475mg/g.
Comparative example: for further proving the effect of ultrasonic synergistic magnetic adsorbent strengthening extraction; The effect of its effect of extracting and room temperature oscillation extraction and magnetic adsorbent auxiliary extraction is compared; Extraction conditions is respectively: room temperature oscillation extraction condition: add the 30ml n-hexane in the 3g danshen powder, vibration 10min under room temperature, 200rpm; Magnetic adsorbent auxiliary extraction condition: add the 10ml n-hexane in the 1g danshen powder, add the 100mg magnetic adsorbent, vibration 10min under the 200rpm vibration.
The result is as shown in Figure 2, can know: ultrasonic synergistic magnetic adsorbent auxiliary extraction technology three kinds of extraction ratio of effective constituents in the red sage root are all high than corresponding room temperature oscillation extraction and magnetic adsorbent auxiliary extraction.This result further shows: ultrasonic wave and magnetic adsorbent have synergy really, can strengthen the extraction process of Chinese herbal medicine effective ingredients greatly.
Embodiment 3
Be that the magnetic molecularly imprinted polymer microballoon of 10nm mixes with 5g ethanol at first with 1g Common Aucklandia Root, 5mg average grain diameter; Place the Extraction by Ultrasound device to carry out ultrasonic Extraction 1min; Ultrasonic power is 500W, uses recirculated cooling water to keep the extraction temperature and is room temperature, and it is constantly stirred; Mixing speed is 2000rpm, carries out adsorbing and extracting; Magnetic Separation and Recovery magnetic adsorbent then, filtering out Chinese herbal medicine matrix must filtrate, with the magnetic molecularly imprinted polymer microballoon in ethanol: acetic acid (3: 1, v/v) in desorb get stripping liquid, merging filtrate and stripping liquid get extract, detect with high performance liquid chromatography.
Embodiment 4
At first be magnetic molecularly imprinted polymer microballoon and the 30g methanol mixed of 500 μ m with 1g rhizoma zingiberis powder, 1000mg average grain diameter; Place the Extraction by Ultrasound device to carry out ultrasonic Extraction 180min; Ultrasonic power is 50W, uses recirculated cooling water to keep the extraction temperature and is room temperature, and it is constantly stirred; Mixing speed is 50rpm, carries out adsorbing and extracting; Magnetic Separation and Recovery magnetic adsorbent then, filtering out Chinese herbal medicine matrix must filtrate, with the magnetic molecularly imprinted polymer microballoon in methyl alcohol: acetic acid (12: 1, v/v) in desorb get stripping liquid, merging filtrate and stripping liquid get extract, detect with high performance liquid chromatography.
Embodiment 5
Be that the magnetic molecularly imprinted polymer microballoon of 2 μ m mixes with 15g acetone at first with 1g rhizoma atractylodis macrocephalae powder, 600mg average grain diameter; Place the Extraction by Ultrasound device to carry out ultrasonic Extraction 40min; Ultrasonic power is 300W, uses recirculated cooling water to keep the extraction temperature and is room temperature, and it is constantly stirred; Mixing speed is 600rpm, carries out adsorbing and extracting; Magnetic Separation and Recovery magnetic adsorbent then, filtering out Chinese herbal medicine matrix must filtrate, with the magnetic molecularly imprinted polymer microballoon in ethanol: acetic acid (10: 1, v/v) in desorb get stripping liquid, merging filtrate and stripping liquid get extract, detect with high performance liquid chromatography.
Embodiment 6
Be that the magnetic molecularly imprinted polymer microballoon of 1 μ m mixes with the 10g n-hexane at first with 1g Common Aucklandia Root, 400mg average grain diameter; Place the Extraction by Ultrasound device to carry out ultrasonic Extraction 20min; Ultrasonic power is 200W, uses recirculated cooling water to keep the extraction temperature and is room temperature, and it is constantly stirred; Mixing speed is 200rpm, carries out adsorbing and extracting; Magnetic Separation and Recovery magnetic adsorbent then, filtering out Chinese herbal medicine matrix must filtrate, with the magnetic molecularly imprinted polymer microballoon in ethanol: acetic acid (9: 1, v/v) in desorb get stripping liquid, merging filtrate and stripping liquid get extract, detect with high performance liquid chromatography.
Applicant's statement, the present invention explains extracting process of the present invention through the foregoing description, but the present invention is not limited to above-mentioned extraction step, does not mean that promptly the present invention must rely on above-mentioned extraction step and could implement.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of raw material that the present invention selects for use and auxiliary element, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (8)
1. the method for a ultrasonic synergistic magnetic adsorbent strengthening extraction Chinese herbal medicine effective ingredients at first with Chinese herbal medicine, magnetic adsorbent and extraction solvent, places the Extraction by Ultrasound device to carry out ultrasonic Extraction; Magnetic Separation and Recovery magnetic adsorbent, and desorb then gets stripping liquid and is extract.
2. the method for claim 1 is characterized in that, in the ultrasonic Extraction process, uses recirculated cooling water to keep the extraction temperature and is room temperature.
3. according to claim 1 or claim 2 method is characterized in that, magnetic is separated the back filter filtrating that the extraction mixed liquor produces and stripping liquid together as extract.
4. like the described method of one of claim 1-3, it is characterized in that said Chinese herbal medicine is simple or multi-flavor medicine, be preferably the mixture of the red sage root, the banksia rose, rhizoma zingiberis, dried orange peel, rhizoma atractylodis macrocephalae or at least two kinds; Form is preferably Powdered or graininess.
5. like the described method of one of claim 1-4, it is characterized in that described magnetic adsorbent is the microballoon with superparamagnetism, the aglucon of the affine absorption effective component of surface-functionalized modification ability; Its average grain diameter is 10nm～500 μ m, preferred 30nm～2 μ m, further preferred 1 μ m; Add 5～1000mg magnetic adsorbent in every gram Chinese herbal medicine;
Described aglucon comprises molecularly imprinted polymer aglucon, hydrogen bond type aglucon, solvay-type aglucon, electrostatic aglucon, mixed type aglucon;
Described molecularly imprinted polymer aglucon is to be that template prepares with the active component of Chinese herbal medicine or its analog; The preferred flavones of described template, polyphenol, steroidal, alkaloid.
6. like the described method of one of claim 1-5, it is characterized in that said extraction solvent is the mixture of water, methyl alcohol, ethanol, n-hexane, acetone, chloroform or at least two kinds, preferred water and/or ethanol; Its consumption is 5～30 times of Chinese herbal medicine weight, preferred 5～15 times, and further preferred 10 times.
7. like the described method of one of claim 1-6, it is characterized in that the said ultrasonic Extraction time is 1～180min, preferred 1～40min, further preferred 20min;
Said ultrasonic power is 50～500W, preferred 100～300W, further preferred 200W;
In the ultrasonic Extraction process, stir; Said alr mode can be the paddle stirring or integral body places oscillator to vibrate, and its speed is 50～2000rpm, is preferably 50～600rpm, further preferred 200rpm.
8. like the described method of one of claim 1-7, it is characterized in that said magnetic separates use magnet for having ferromagnetic electromagnet or permanent magnet;
Saidly separate that to smoke absorbent formulated by methyl alcohol or ethanol and acetic acid; Its volume ratio is 3: 1～12: 1, preferred 6: 1～10: 1, and further preferred 9: 1.
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| CN104855029A (en) * | 2014-02-25 | 2015-08-26 | 姚明勤 | Simple formula fertilization method for plant prevention and treatment of heavy metal pollution |
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| CN101070555A (en) * | 2006-05-09 | 2007-11-14 | 上海化工研究院 | Method for extracting natural beta-caroetne |
| CN101664668A (en) * | 2009-09-29 | 2010-03-10 | 中国科学院生态环境研究中心 | Preparation method and application of core-shell type Fe3O4/C magnetic nano solid extracting agent |
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