CN102527085B - 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, particularly relate to a kind of method of magnetic adsorbent auxiliary extraction Chinese herbal medicine effective ingredients.
Background technology
Chinese herbal medicine is as a kind of pure natural plant medicine, containing many effective components, treatment can be permitted various diseases, for realizing these effective components need being extracted from plant tissue effective utilization of Chinese herbal medicine, again through further separation and purification, make Chinese patent drug and various preparation, these Chinese herbal and crude drugs preparationses are because of pure natural, toxic and side effect is few, extremely the liking of people.
Utilize in process at Chinese herbal medicine effective ingredients, extractive technique is crucial.Traditional extracting method adopts organic solvent extraction, and as heat reflow method and soxhlet extraction, it is large that these methods also exist organic solvent consumption, consuming time longer, high temperature cause heat-sensitive ingredients because of degraded the defect such as loss.For addressing these problems, people have developed some new extracting process as supercritical fluid extraction, using microwave-assisted and ultrasound-assisted extraction method in recent years.These new abstraction techniques overcome conventional art defect in achieve good progress: supercritical liquid extraction technique is using the supercritical fluid of green as solvent, there is solvent reusable edible, high extraction, Extracting temperature are low to advantages such as heat-sensitive ingredients frees of losses, be subject to paying attention to widely and a large amount of application in recent years in Chinese herbal medicine effective ingredients extracts, its defect is that energy consumption is large, need extraction equipment costly; Microwave, ultrasound-assisted extraction technology utilize the high energy such as ultrasonic wave, microwave field to organize from external action in Chinese herbal medicine, by disorganize cell and cavitation effect to reduce the stripping that the forms such as resistance to mass tranfer strengthen Chinese herbal medicine effective ingredients, thus improve extraction efficiency shortening extraction time, wherein microwave greatly shortens on extraction time, effect is best, but the two defect is all little on raising recovery rate, and needs corresponding equipment and energy ezpenditure.Therefore develop a kind of not energy requirement, do not need complex appts, simple to operate, at low temperatures can realize to thermal sensitivity Chinese herbal medicine effective ingredients fast and efficiently extractive technique there is important value and significance.
CN 101869581A discloses a kind of process extracting effective ingredient from Chinese herbal medicine, and it comprises the following steps: medium-height grass medicinal solvent is carried out extraction and obtains extract by (1); (2) extract is carried out concentrated obtain concentrate; (3) concentrate is used macroporous adsorbing resin for purification effective components of Chinese medicinal; (4) at supercritical conditions, fully contact with macroporous absorbent resin with supercritical fluid, removing organic molecule remains, and it is separated with macroporous absorbent resin under supercritical fluid liquid condition, and liquid obtains effective component of Chinese herbal medicine after removing high pressure.It is few that it has solvent load, the elution time fast and wash-out advantage such as completely.
The invention provides a kind of new magnetic adsorbent auxiliary extraction technology, this technology causes Chinese herbal medicine matrix with concentration difference larger in extract based on the absorption of magnetic adsorbent to the active ingredient in extract, thus greatly strengthens mass transfer, shortens extraction time; Meanwhile, magnetic adsorbent causes the mass transfer of active ingredient and Chinese herbal medicine matrix in extract to balance constantly be broken because the active ingredient in extract is transferred to continuously, thus obtain very high recovery rate; And Extraction solvent only serves as the effect of a mass transfer medium in extraction process, therefore solvent reusable edible to a great extent; In addition this technology is at room temperature carried out in a very simple way, especially applicable to 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 defect of existing extracting process.The method has simple to operate, the advantage such as rate of extraction is fast, extraction yield is high, carry out under room temperature, solvent reusable edible, is very suitable for the extraction of active ingredient in Chinese herbal medicine.
For reaching this object, the present invention by the following technical solutions:
A method for magnetic adsorbent auxiliary extraction Chinese herbal medicine effective ingredients, first mixes Chinese herbal medicine, magnetic adsorbent with Extraction solvent, carries out adsorbing and extracting under at room temperature constantly stirring; Then Magneto separate reclaims magnetic adsorbent, and desorb obtains stripping liquid is extract.
Preferably, the filtrate that extracted by filtration mixed liquor after Magneto separate can be produced and stripping liquid are together as extract.When magnetic adsorbent is enough, can ignore amount of filtrate, stripping liquid is extract.
Chinese herbal medicine of the present 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 the contact area with Extraction solvent, thus is conducive to 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 energy; Its average grain diameter is 10nm ~ 500 μm, such as, can select 12nm, 50nm, 100nm, 900nm, 2 μm, 80 μm, 220 μm, 300 μm, 450 μm, and 490 μm of grades are used for the present invention, preferred 30nm ~ 2 μm, preferably 1 μm further; Add 5 ~ 1000mg magnetic adsorbent in every gram of Chinese herbal medicine, such as, in every gram of Chinese herbal medicine, add magnetic adsorbent 20mg, 100mg, 250mg, 380mg, 500mg, 760mg, 880mg, 980mg etc.
Aglucon of the present invention comprises molecularly imprinted polymer aglucon, hydrogen bond type aglucon, solvay-type aglucon, electrostatic aglucon, mixed type aglucon all can be used for implementing 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 for template and suitable monomer are prepared 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 the domain knowledge of technical staff.Described template is active component in the Chinese herbal medicine that will extract or its analog, and technical staff can select flexibly.
Extraction solvent of the present invention is mixture, preferred water and/or the ethanol of water, methyl alcohol, ethanol, n-hexane, acetone, chloroform or at least two kinds.Conventional traditional Chinese medicine extraction solvent has: water, hydrophilic organic solvent, lipophilic organic solvent.Water is a kind of strong polar solvent, hydrophilic composition in Chinese herbal medicine, polysaccharide, tannin, amino acid, protein, acylate, alkaloid salt and glucoside etc. as not too large in inorganic salts, carbohydrate, molecule can by water-soluble go out.Hydrophilic organic solvent namely general said organic solvent miscible with water, as ethanol, methyl alcohol, acetone etc., the most frequently used with ethanol.The solubility property of ethanol is relatively good, stronger to the penetration capacity of Chinese herbal medicine cell.The character of methyl alcohol is similar with ethanol, boiling point lower (64 DEG C), but toxic, should note during use.Lipophilic organic solvent is exactly general said organic solvent not miscible with water, as benzinum, benzene, chloroform, ether, ethyl acetate, dichloroethanes etc.
The consumption of Extraction solvent is 5 ~ 30 times of medium-height grass dose, and such as every gram of Chinese herbal medicine uses Extraction solvent 5.5g, 7g, 10g, 11g, 13.8g, 20g, 24.2g, 28g etc., preferably 5 ~ 15 times, preferably 10 times further.
The described adsorbing and extracting time is 2 ~ 180min, and such as technical staff can select 3min, and 8min, 20min, 85min, 100min, 135min, 160min, 178min equal time is used for the present invention, preferably 2 ~ 90min, further preferred 10min.The adsorbing and extracting time namely stirs or duration of oscillation.Described agitating mode can be paddle and to stir or entirety is placed in shaking table and vibrates.Other stirrings that adsorbing and extracting process can be made more thoroughly to carry out or mode of oscillation all can be selected according to actual conditions by those skilled in the art, and speed is 50 ~ 2000rpm, such as 60rpm, 120rpm, 187rpm, 280rpm, 450rpm, 800rpm, 1250rpm, 1600rpm, 1980rpm etc., be preferably 50 ~ 600rpm, further preferred 200rpm.
Magneto separate process of the present invention magnet used is for having ferromagnetic electromagnet or permanent magnet.
Described solution smoke absorbent for methyl alcohol or ethanol and acetic acid formulated; Its volume ratio is 3: 1 ~ 12: 1, such as 3.5: 1,5: 1,6.8: 1,8: 1,10.4: 1,11: 1,11.8: 1 etc., preferably 6: 1 ~ 10: 1, further preferably 9: 1.
Magneto separate process of the present invention is to be separated with the mixed liquor of extract with Chinese herbal medicine matrix by magnetic adsorbent, concrete operations are: magnet is put into a teat glass, move back and forth fully to catch magnetic adsorbent by this teat glass mixed liquor after the extraction, then magnet is removed, with a small amount of absorbent drip washing test tube outer surface, magnetic adsorbent is split away off, carries out next step desorb.
The invention provides a kind of method of magnetic adsorbent auxiliary extraction Chinese herbal medicine effective ingredients, concrete operations are as follows: first Chinese medicine, magnetic adsorbent are mixed with Extraction solvent, when room temperature, it is constantly stirred or puts into constant temperature oscillator and vibrate, carry out adsorbing and extracting; Then Magneto separate reclaims magnetic adsorbent, and concrete operations are described above.Filter out Chinese herbal medicine matrix and obtain filtrate, magnetic adsorbent desorb in the mixed liquor of methyl alcohol or ethanol and acetic acid is obtained stripping liquid, and merging filtrate and stripping liquid obtain extract, detect by liquid chromatogram.
In desorption process of the present invention, how many direct relations of desorption efficiency the size of extraction yield, and therefore need to smoke absorbent to adopted solution and be optimized, desorb is complete as far as possible.
Mass transfer can be strengthened based on concentration difference, the present invention proposes and adopt magnetic adsorbent to produce larger mass transfer concentration difference thus the extraction of strengthening Chinese herbal medicine effective ingredients, because the magnetic adsorbent made can optionally adsorb specific active ingredient thus cause the concentration difference of active ingredient, thus reach the object of the strengthening extraction of high selectivity.In addition because the concentration of active ingredient in extraction solution maintains very low concentration all the time, be equivalent to extract Chinese herbal medicine matrix with fresh solvent all the time, therefore very high extraction yield can be obtained; Because adopted extractant is only equivalent to mass transfer medium, therefore can recycle.
Extracting process of the present invention at room temperature carries out, and do not need to consume any energy, be particularly useful for the extraction of the high selectivity of the active ingredient of thermal sensitivity in Chinese herbal medicine.
Accompanying drawing explanation
Fig. 1 is that the extraction effect of different extraction mode compares block diagram.
Fig. 2 is the extraction kinetics curve map of magnetic molecularly imprinted microballoon strengthening extraction tanshinone 2a.
Fig. 3 is that magnetic molecularly imprinted microballoon auxiliary extraction contrasts figure with solvent extraction extract spectrogram
Fig. 4 is the liquid phase spectrogram comparison diagram that three kinds of magnetic adsorbent auxiliary extractions and shaken at room temperature extract.
Fig. 5 is variety classes magnetic adsorbent strengthening extraction effectiveness comparison block diagram.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, does not represent or limits the scope of the present invention, and interest field of the present invention is as the criterion with claims.
Detailed description of the invention
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1 adopts three kinds of tanshinones in the magnetic molecularly imprinted polymer microballoon auxiliary extraction red sage root
Extraction conditions: add 10ml n-hexane in 1g Danshen Root, for carrying out extraction kinetics mensuration, average grain diameter is that the magnetic molecularly imprinted polymer microballoon of 200nm adds and measures three parameters: 0, 100mg and 200mg, then at room temperature integral container is placed in constant temperature oscillator to vibrate, hunting speed is 200rpm, when different duration of oscillation, Magneto separate is carried out to sample, filter out Chinese herbal medicine matrix and obtain filtrate, by magnetic molecularly imprinted microballoon in methyl alcohol: acetic acid (9: 1, v/v) in, desorb obtains stripping liquid, merging filtrate and stripping liquid obtain extract, detect by liquid chromatogram.
Result: as shown in Figure 2, the extraction kinetics not adding magnetic particle under magnetic molecularly imprinted microballoon addition is the magnetic auxiliary extraction of 100mg and 200mg and the same terms carries out contrasting (using the extraction yield of tanshinone 2a as reference), known: magnetic microsphere auxiliary extraction can strengthening extraction efficiency greatly.Show: along with adding of magnetic microsphere, the extraction yield of tanshinone 2a significantly improves, extraction rate is accelerated greatly, reach extraction equilibrium required time when not adding magnetic adsorbent and need 1h, and to reach equilibration time when adding 100mg magnetic adsorbent be 10min, reach equilibration time when adding 200mg magnetic adsorbent and shorten to 5min, show that the more extraction rates of added magnetic absorption dosage are faster.Whether have selective for investigating magnetic adsorbent strengthening extraction in addition, the extract of magnetic auxiliary extraction and organic solvent extraction extract high-efficient liquid phase chromatogram are contrasted, as shown in Figure 3, visible magnetic adsorbent auxiliary extraction has the effect of high selectivity strengthening extraction, and this figure also shows that the purity of magnetic auxiliary extraction gained active ingredient is higher than shaken at room temperature extraction simultaneously.For proving whether magnetic adsorbent auxiliary extraction solvent can reuse, and is extracted under the same conditions by this solvent and contrast with former solvent extraction effect the red sage root, and experiment finds almost constant to the extraction yield of three kinds of tanshinones.
Comparative example: for proving the performance of magnetic auxiliary extraction further, the effect of its effect of extracting and conventional extracting process contrasted, shaken at room temperature extraction conditions is: add 10ml n-hexane in 1g danshen powder, and vibrate 4h under room temperature, 200rpm; Hot reflux extraction conditions: add 10ml n-hexane in 1g danshen powder, reflux 45min at 80 DEG C; Ultrasound-assisted extraction condition: add 10ml n-hexane in 1g danshen powder, ultrasonic 1.5h in ultrasonic washer.
Result shows: as shown in Figure 1, and the reflux extraction of magnetic adsorbent auxiliary extraction 20min specific heat, ultrasound-assisted extraction, shaken at room temperature extraction have the highest extraction yield and the shortest extraction time to three kinds of tanshinones.
Be there is by the present embodiment sufficient proof magnetic adsorbent auxiliary extraction the advantages such as technique is simple, high extraction, high extraction rate, solvent reusable edible, high selectivity.
Three kinds of tanshinones in the embodiment 2 magnetic absorption resin auxiliary extraction red sage root
Extraction conditions: add 10ml absolute ethyl alcohol in 1g salvia piece, for carrying out different magnetic adsorbent auxiliary extraction and shaken at room temperature effect of extracting contrasts, average grain diameter is respectively 1 μm, the magnetic hydroxyethyl meth acrylate crosslinked microsphere of 1 μm and 150nm, magnetic methacrylic acid crosslinked microsphere and magnetic silica, addition all gets 500mg, then at room temperature integral container is placed in constant temperature oscillator to vibrate, hunting speed is 200rpm, under vibration different time, to sample Magneto separate, filter out Chinese herbal medicine matrix and obtain filtrate, by magnetic adsorbent in ethanol: acetic acid (9: 1, v/v) in, desorb obtains stripping liquid, merging filtrate and stripping liquid obtain extract, detect by liquid chromatogram.
Result shows, as shown in Figure 5, for salvia piece, three kinds of magnetic adsorbents all can strengthening extraction well, all can obtain high extraction yield to three kinds of active ingredients; Fig. 4 is that the liquid phase spectrogram that three kinds of magnetic adsorbent auxiliary extractions and shaken at room temperature extract contrasts, after showing three kinds of magnetic adsorbent extractions, in extract, the purity of three kinds of active ingredients all improves more significantly than having of shaken at room temperature extraction, this further demonstrates the high selectivity of magnetic adsorbent auxiliary extraction in Chinese herbal medicine extracts.
Embodiment 3 adopts active ingredient in the magnetic molecularly imprinted polymer microballoon auxiliary extraction banksia rose
First be that the magnetic molecularly imprinted polymer microballoon of 10nm mixes with 5g ethanol by 1g Common Aucklandia Root, 5mg average grain diameter, constantly stir 2min when room temperature to it, mixing speed is 2000rpm, carries out adsorbing and extracting; Then Magneto separate reclaims magnetic adsorbent, filter out Chinese herbal medicine matrix and obtain filtrate, by magnetic molecularly imprinted polymer microballoon in ethanol: in acetic acid (3: 1, v/v), desorb obtains stripping liquid, merging filtrate and stripping liquid obtain extract, detect by liquid chromatogram.
Embodiment 4 adopts active ingredient in magnetic molecularly imprinted polymer microballoon auxiliary extraction dried orange peel
First be that the magnetic molecularly imprinted polymer microballoon of 500 μm mixes with 15g acetone by 1g Dried Tangerine Peel, 1g average grain diameter, when room temperature, integral container is put into constant temperature oscillator and to vibrate 180min, hunting speed is 50rpm, carries out adsorbing and extracting; Then Magneto separate reclaims magnetic adsorbent, by magnetic molecularly imprinted polymer microballoon in methyl alcohol: in acetic acid (12: 1, v/v), desorb obtains stripping liquid and is extract, detects by liquid chromatogram.
Embodiment 5 adopts active ingredient in magnetic molecularly imprinted polymer microballoon auxiliary extraction dried orange peel
First be that the magnetic molecularly imprinted polymer microballoon of 1 μm mixes with 10g chloroform by 1g Dried Tangerine Peel, 200mg average grain diameter, when room temperature, integral container is put into constant temperature oscillator and to vibrate 10min, hunting speed is 600rpm, carries out adsorbing and extracting; Then Magneto separate reclaims magnetic adsorbent, filter out Chinese herbal medicine matrix and obtain filtrate, by magnetic molecularly imprinted polymer microballoon in methyl alcohol: in acetic acid (9: 1, v/v), desorb obtains stripping liquid, merging filtrate and stripping liquid obtain extract, detect by liquid chromatogram.
Embodiment 6 adopts active ingredient in magnetic silica microballoon auxiliary extraction rhizoma zingiberis
First be that the magnetic silica microballoon of 2 μm mixes with 30g n-hexane by 1g rhizoma zingiberis medicine materical crude slice, 500mg average grain diameter, when room temperature, integral container is put into constant temperature oscillator and to vibrate 90min, hunting speed is 500rpm, carries out adsorbing and extracting; Then Magneto separate reclaims magnetic adsorbent, filters out Chinese herbal medicine matrix and obtains filtrate, by magnetic silica microballoon in ethanol: in acetic acid (6: 1, v/v), desorb obtains stripping liquid, and merging filtrate and stripping liquid obtain extract, detect by liquid chromatogram.
Applicant states, the present invention illustrates extracting process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned extraction step, does not namely mean that the present invention must rely on above-mentioned extraction step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (19)
1. a method for magnetic adsorbent auxiliary extraction Chinese herbal medicine effective ingredients, first mixes Chinese herbal medicine, magnetic adsorbent with Extraction solvent, carries out adsorbing and extracting under room temperature under constantly stirring; Then Magneto separate reclaims magnetic adsorbent, and desorb obtains stripping liquid is extract;
Described solution smoke absorbent by methyl alcohol or ethanol and acetic acid formulated; Its volume ratio is 3:1 ~ 12:1;
Described magnetic adsorbent is the microballoon with superparamagnetism, the aglucon of the affine absorption effective component of surface-functionalized modification energy; Its average grain diameter is 10nm ~ 500 μm; 5 ~ 1000mg magnetic adsorbent is added in every gram of Chinese herbal medicine; Described aglucon is the one in molecularly imprinted polymer aglucon, hydrogen bond type aglucon, solvay-type aglucon, electrostatic aglucon or mixed type aglucon; Described molecularly imprinted polymer aglucon is for template is prepared with the active component of Chinese herbal medicine or its analog;
The described adsorbing and extracting time is 2 ~ 180min; Described agitating mode is that paddle stirs or entirety is placed in oscillator and vibrates, and its speed is 50 ~ 2000rpm.
2. the method for claim 1, is characterized in that, the filtrate produce extracted by filtration mixed liquor after Magneto separate and stripping liquid are together as extract.
3. method as claimed in claim 1 or 2, it is characterized in that, described Chinese herbal medicine is simple or multi-flavor medicine.
4. method as claimed in claim 3, is characterized in that, described Chinese herbal medicine is the mixture of the red sage root, the banksia rose, rhizoma zingiberis, dried orange peel, rhizoma atractylodis macrocephalae or at least two kinds.
5. method as claimed in claim 3, it is characterized in that, the form of described Chinese herbal medicine is Powdered or graininess.
6. the method for claim 1, is characterized in that, the average grain diameter of described magnetic adsorbent is 30nm ~ 2 μm.
7. method as claimed in claim 6, it is characterized in that, the average grain diameter of described magnetic adsorbent is 1 μm.
8. the method for claim 1, is characterized in that, described template is flavones, polyphenol, steroidal, alkaloid.
9. the method for claim 1, is characterized in that, described Extraction solvent is the mixture of water, methyl alcohol, ethanol, n-hexane, acetone, chloroform or at least two kinds; Its consumption is 5 ~ 30 times of Chinese herbal medicine weight.
10. method as claimed in claim 9, it is characterized in that, described Extraction solvent is water and/or ethanol.
11. methods as claimed in claim 9, is characterized in that, the consumption of described Extraction solvent is 5 ~ 15 times of Chinese herbal medicine weight.
12. methods as claimed in claim 11, the consumption of described Extraction solvent is 10 times of Chinese herbal medicine weight.
13. the method for claim 1, is characterized in that, the described adsorbing and extracting time is 2 ~ 90min.
14. methods as claimed in claim 13, it is characterized in that, the described adsorbing and extracting time is 10min.
15. the method for claim 1, is characterized in that, the speed of described stirring is 50 ~ 600rpm.
16. methods as claimed in claim 15, is characterized in that, the speed of described stirring is 200rpm.
17. the method for claim 1, is characterized in that, described Magneto separate magnet is for having ferromagnetic electromagnet or permanent magnet.
18. the method for claim 1, is characterized in that, the volume ratio of described methyl alcohol or ethanol and acetic acid is 6:1 ~ 10:1.
19. methods as claimed in claim 18, is characterized in that, the volume ratio of described methyl alcohol or ethanol and acetic acid is 9:1.
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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 |
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