CN102527085A - Method for extracting effective components of Chinese herbal medicine by magnetic absorbent in an auxiliary way - Google Patents
Method for extracting effective components of Chinese herbal medicine by magnetic absorbent in an auxiliary way Download PDFInfo
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Abstract
The invention relates to a method for extracting effective components of a Chinese herbal medicine by a magnetic absorbent in an auxiliary way. The method comprises the following steps of: firstly mixing the Chinese herbal medicine, the magnetic absorbent and an extraction solvent, and stirring continuously under normal temperature to carry out absorption and extraction; then adopting magnetic separation to recover the magnetic absorbent, and filtering to obtain filtrate; desorbing the magnetic absorbent to obtain desorption solution; and combining the filtrate and the desorption solution to obtain extracting solution. When the magnetic absorbent is enough, the filtrate can be ignored and the desorption solution is the extracting solution. The method has the advantages of simple process, high extraction speed, high extraction rate, mild extraction conditions (room temperature), high selectivity, recycling solvent and high purity of an extracted product and the like, and is very suitable for fast, high-selectivity and high-efficiency extraction of heat-sensitive components in traditional Chinese medicine products.
Description
Technical field
The present invention relates to Chinese herbal medicine purification technique field, relate in particular to a kind of method of magnetic adsorbent auxiliary 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 obtained good progress: supercritical liquid extraction technique with the supercritical fluid of green as solvent; It is low to advantages such as thermal sensitivity composition frees of losses to have solvent reusable edible, high extraction, extraction temperature; In Chinese herbal medicine effective ingredients extracts, receive in recent years and paying attention to widely and number of applications, its defective be energy consumption big, need expensive extraction equipment; Microwave, ultrasonic wave auxiliary extraction technology are to utilize high energy fields such as ultrasonic wave, microwave to organize from external action in Chinese herbal medicine; Strengthen the stripping of Chinese herbal medicine effective ingredients through disorganize cell and cavitation effect to reduce forms such as resistance to mass tranfer; Thereby improve extraction efficiency and shorten the extraction time, wherein microwave shortens on the extraction time greatly, and effect is best; But the two defective is all little on the raising recovery rate, and needs corresponding apparatus and energy consumption.Therefore develop a kind of not energy requirement, do not need complex appts, simple to operate, at low temperatures can realize to the thermal sensitivity Chinese herbal medicine effective ingredients fast and efficiently extractive technique have significant values and meaning.
CN 101869581A discloses a kind of process of from Chinese herbal medicine, extracting effective ingredient, and it may further comprise the steps: (1) is extracted the medium-height grass medicinal solvent and obtained extract; (2) extract is concentrated obtain concentrate; (3) with concentrate with macroporous absorbent resin enrichment effective components of Chinese medicinal; (4) under super critical condition, fully contact with macroporous absorbent resin with supercritical fluid, it is residual to remove organic molecule, under the supercritical fluid liquid condition, it is separated with macroporous absorbent resin, and liquid obtains the Chinese herbal medicine effective ingredient after removing high pressure.It is few that it has a solvent load, and elution time reaches wash-out soon and waits advantage fully.
The invention provides a kind of new magnetic adsorbent auxiliary extraction technology, this technology causes Chinese herbal medicine matrix with concentration difference bigger in the extract based on magnetic adsorbent to the absorption of the active ingredient in the extract, thereby reinforcing mass transfer greatly shortens the extraction time; Simultaneously, owing to the active ingredient in the extract is transferred to continuously and caused in the extract mass transfer balance of active ingredient and Chinese herbal medicine matrix constantly to be broken on the magnetic adsorbent, thereby obtain very high recovery rate; And extract solvent only serves as a mass transfer media in extraction process effect, so solvent reusable edible to a great extent; Should technology at room temperature carry out in addition with very simple mode, especially suitable to the thermal sensitivity Chinese herbal medicine effective ingredients.
Summary of the invention
The object of the present invention is to provide a kind of magnetic adsorbent auxiliary 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 magnetic adsorbent auxiliary extraction Chinese herbal medicine effective ingredients at first with Chinese herbal medicine, magnetic adsorbent and extraction solvent, is carried out adsorbing and extracting under at room temperature constantly stirring; Magnetic Separation and Recovery magnetic adsorbent, and desorb then gets stripping liquid and is extract.
Preferably, can magnetic be separated the back and filter filtrating that the extraction mixed liquor produces and stripping liquid 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 gram 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 adsorbing and extracting time is 2～180min, and for example the technical staff can select 3min, 8min, and 20min, 85min, 100min, 135min, 160min, the 178min equal time is used for the present invention, preferred 2～90min, further preferred 10min.The adsorbing and extracting time just stirs or duration of oscillation.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 magnetic adsorbent auxiliary extraction Chinese herbal medicine effective ingredients; Concrete operations are following: at first with Chinese medicine, magnetic adsorbent and extraction solvent; When room temperature, it is constantly stirred or put into constant temperature oscillator and vibrate, carry out adsorbing and extracting; 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.
Based on concentration difference ability reinforcing mass transfer; Adopt magnetic adsorbent to produce the extraction that bigger mass transfer concentration difference is strengthened Chinese herbal medicine effective ingredients thereby the present invention proposes; Because thereby the magnetic adsorbent of making can optionally adsorb the concentration difference that specific active ingredient causes active ingredient, thereby reach the purpose of the strengthening extraction of high selectivity.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, in addition so can obtain very high extraction yield; Because the extractant that is adopted only is equivalent to the mass transfer media, so can recycle.
The extracting process that the present invention adopted is at room temperature to carry out, and need not consume any energy, is particularly useful for the extraction of the high selectivity of the active ingredient of thermal sensitivity in the Chinese herbal medicine.
Description of drawings
Fig. 1 is that the extraction effect of different extraction modes compares block diagram.
Fig. 2 is the extraction kinetics curve map of magnetic molecularly imprinted microballoon strengthening extraction tanshinone 2a.
Fig. 3 is magnetic molecularly imprinted microballoon auxiliary extraction and solvent extraction extract spectrogram map
Fig. 4 is the liquid phase spectrogram comparison diagram of three kinds of magnetic adsorbent auxiliary extractions and room temperature oscillation extraction.
Fig. 5 is a relatively block diagram of variety classes magnetic adsorbent strengthening extraction effect.
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 adopts three kinds of tanshinones in the magnetic molecularly imprinted polymer microballoon auxiliary extraction red sage root
Extraction conditions: add the 10ml n-hexane in the 1g Danshen Root, measure for carrying out extraction kinetics, average grain diameter is that three parameters are measured in the magnetic molecularly imprinted polymer microballoon adding of 200nm: 0; 100mg and 200mg at room temperature place constant temperature oscillator to vibrate integral container then, and hunting speed is 200rpm; When different duration of oscillation, sample is carried out magnetic separate, 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, and merging filtrate and stripping liquid get extract, detect with liquid chromatogram.
Result: as shown in Figure 2; The extraction kinetics that under magnetic auxiliary extraction that magnetic molecularly imprinted microballoon addition is 100mg and 200mg and the same terms, does not add the magnetic particle compare (with the extraction yield of tanshinone 2a as with reference to), can know: the magnetic microsphere auxiliary extraction is strengthening extraction efficient greatly.Show: along with the adding of magnetic microsphere; The extraction yield of tanshinone 2a significantly improves; Extraction rate is accelerated greatly, and reaching the extraction equilibrium required time when not adding magnetic adsorbent needs 1h, is 10min and reach equilibration time when adding the 100mg magnetic adsorbent; Reach equilibration time when adding the 200mg magnetic adsorbent and shorten to 5min, it is fast more to show that institute adds the many more extraction rates of magnetic adsorbent amount.Whether has selectivity for investigating the magnetic adsorbent strengthening extraction in addition; The extract and the organic solvent extraction extract high-efficient liquid phase chromatogram of magnetic auxiliary extraction are compared; As shown in Figure 3; It is thus clear that the magnetic adsorbent auxiliary extraction has the effect of high selectivity strengthening extraction, this figure shows that also the purity of magnetic auxiliary extraction gained active ingredient will be higher than the room temperature oscillation extraction simultaneously.For whether proof magnetic adsorbent auxiliary extraction solvent can reuse, this solvent is extracted the red sage root under the same conditions and compares with former solvent extraction effect, experiment is found almost constant to the extraction yield of three kinds of tanshinones.
Comparative example: be the further performance of proof magnetic auxiliary extraction, the effect of its effect of extracting and extracting process commonly used is compared that room temperature oscillation extraction condition is: add the 10ml n-hexane in the 1g danshen powder, in room temperature, the 200rpm 4h that vibrates down; Hot reflux extraction conditions: add the 10ml n-hexane in the 1g danshen powder, in 80 ℃ of refluxed 45min; Ultrasonic wave auxiliary extraction condition: add 10ml n-hexane, ultrasonic 1.5h in ultrasonic washer in the 1g danshen powder.
The result shows: as shown in Figure 1, the reflux extraction of magnetic adsorbent auxiliary extraction 20min specific heat, ultrasonic wave auxiliary extraction, room temperature oscillation extraction have the highest extraction yield and the shortest extraction time to three kinds of tanshinones.
Prove fully that through present embodiment the magnetic adsorbent auxiliary extraction has advantages such as technology is simple, high extraction, high extraction rate, solvent reusable edible, high selectivity.
Three kinds of tanshinones in the embodiment 2 magnetic polymeric adsorbent auxiliary extraction reds sage root
Extraction conditions: add the 10ml absolute ethyl alcohol in the 1g salvia piece, for carrying out different magnetic adsorbent auxiliary extractions and room temperature oscillation extraction effect comparison, average grain diameter is respectively magnetic hydroxyethyl meth acrylate crosslinked microsphere, magnetic methacrylic acid crosslinked microsphere and the magnetic silica of 1 μ m, 1 μ m and 150nm; Addition is all got 500mg; At room temperature place constant temperature oscillator to vibrate integral container then, hunting speed is 200rpm, under the vibration different time; Sample magnetic is separated; Filtering out Chinese herbal medicine matrix must filtrate, with magnetic adsorbent in ethanol: acetic acid (9: 1, v/v) in desorb get stripping liquid; Merging filtrate and stripping liquid get extract, detect with liquid chromatogram.
The result shows, and is as shown in Figure 5, and for salvia piece, three kinds of magnetic adsorbents are strengthening extraction well all, all can obtain high extraction yield to three kinds of active ingredients; Fig. 4 is the liquid phase spectrogram contrast of three kinds of magnetic adsorbent auxiliary extractions and room temperature oscillation extraction; The purity that shows three kinds of active ingredients in three kinds of magnetic adsorbent extraction back extracts all improves than having more significantly of room temperature oscillation extraction, and this has further proved the high selectivity of magnetic adsorbent auxiliary extraction in Chinese herbal medicine extracting.
Embodiment 3 adopts active ingredient in the magnetic molecularly imprinted polymer microballoon auxiliary extraction banksia rose
Be that the magnetic molecularly imprinted polymer microballoon of 10nm mixes with 5g ethanol with 1g Common Aucklandia Root, 5mg average grain diameter at first, when room temperature, it constantly stirred 2min, 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 liquid chromatogram.
Be that the magnetic molecularly imprinted polymer microballoon of 500 μ m mixes with 15g acetone with 1g Dried Tangerine Peel, 1g average grain diameter at first, when room temperature, integral container put into the constant temperature oscillator 180min that vibrates, hunting speed is 50rpm, carries out adsorbing and extracting; Magnetic Separation and Recovery magnetic adsorbent then, with the magnetic molecularly imprinted polymer microballoon in methyl alcohol: acetic acid (12: 1, v/v) in desorb get stripping liquid and be extract, detect with liquid chromatogram.
Be that the magnetic molecularly imprinted polymer microballoon of 1 μ m mixes with the 10g chloroform with 1g Dried Tangerine Peel, 200mg average grain diameter at first, when room temperature, integral container put into the constant temperature oscillator 10min that vibrates, hunting 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 methyl alcohol: acetic acid (9: 1, v/v) in desorb get stripping liquid, merging filtrate and stripping liquid get extract, detect with liquid chromatogram.
Be that the magnetic silica microballoon of 2 μ m mixes with the 30g n-hexane with 1g rhizoma zingiberis medicine materical crude slice, 500mg average grain diameter at first, when room temperature, integral container put into the constant temperature oscillator 90min that vibrates, hunting speed is 500rpm, carries out adsorbing and extracting; Magnetic Separation and Recovery magnetic adsorbent then, filtering out Chinese herbal medicine matrix must filtrate, with magnetic silica microballoon in ethanol: acetic acid (6: 1, v/v) in desorb get stripping liquid, merging filtrate and stripping liquid get extract, detect with liquid chromatogram.
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 (7)
1. the method for a magnetic adsorbent auxiliary extraction Chinese herbal medicine effective ingredients at first with Chinese herbal medicine, magnetic adsorbent and extraction solvent, is carried out adsorbing and extracting under constantly stirring; 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, filtrating that filtration extraction mixed liquor produced after magnetic was separated and stripping liquid are together as extract.
3. according to claim 1 or claim 2 method is characterized in that said Chinese herbal medicine 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.
4. like the described method of one of claim 1-3, 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.
5. like the described method of one of claim 1-4, 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.
6. like the described method of one of claim 1-5, it is characterized in that the said adsorbing and extracting time is 2～180min, preferred 2～90min, further preferred 10min; 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.
7. like the described method of one of claim 1-6, 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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Cited By (2)
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| CN109331783A (en) * | 2018-10-23 | 2019-02-15 | 南京师范大学常州创新发展研究院 | Mechanochemistry Magnetic solid phases extracting process, magnetic Nano material and preparation method thereof |
| CN111744231A (en) * | 2020-06-29 | 2020-10-09 | 漯河医学高等专科学校 | Method for enriching active components for inhibiting growth of candida albicans in mushroom fermentation liquor |
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| CN109331783A (en) * | 2018-10-23 | 2019-02-15 | 南京师范大学常州创新发展研究院 | Mechanochemistry Magnetic solid phases extracting process, magnetic Nano material and preparation method thereof |
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| CN111744231A (en) * | 2020-06-29 | 2020-10-09 | 漯河医学高等专科学校 | Method for enriching active components for inhibiting growth of candida albicans in mushroom fermentation liquor |
| CN111744231B (en) * | 2020-06-29 | 2021-11-19 | 漯河医学高等专科学校 | Method for enriching active components for inhibiting growth of candida albicans in mushroom fermentation liquor |
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