CN103006824A - Method for extracting tritepenoidic acid from jujube leaves - Google Patents
Method for extracting tritepenoidic acid from jujube leaves Download PDFInfo
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Abstract
The invention discloses a method for extracting tritepenoidic acid from jujube leaves and belongs to the technical field of the extraction of tritepenoidic acid. The technical problem to be solved is to provide a method for fully utilizing the resources of jujube leaves and extracting and purifying tritepenoidic acid from the jujube leaves to improve the additional value of jujube products. The technical scheme comprises the following steps: cleaning, drying and smashing the jujube leaves at first, then, extracting the obtained jujube leaf powder with ethanol solution as a solvent by ultrasonic wave, filtering to remove slag to obtain ultrasonic extracting solution; concentrating the ultrasonic extracting solution to remove ethanol to obtain concentrated solution; and purifying the concentrated solution with macroporous resin to obtain tritepenoidic acid solution. The technical research of extracting and producing the tritepenoidic acid from the jujube leaves achieves the comprehensive utilization of the jujube leaves by high technology in a high-additional-value way, and improves the comprehensive economic benefit of planting of jujube tress; and in addition, the planting of the jujube tress is large in scale and high in output of jujube leaves, can implement large scale production and has industrial value and significance.
Description
Technical field
A kind of method of extracting triterpenic acid from Folium Jujubae of the present invention belongs to triterpenic acid extractive technique field.
Background technology
The triterpene acids is the general name that a class has bioactive chemical compound.It is reported and contain more than ten kind of triterpenic acid and triterpene acid esters in the Fructus Jujubae, in jujube, its main forms is belulinic acid Betulinic acid, Crataegolic acid, oleanolic acid and ursolic acid etc.Show that after deliberation the triterpene acid has anticancer, antimutagenic effect.At present, then people mainly by the plantation Chinese herbal medicine, extract wherein that the method for triterpenoids obtains such material, and conventional extracting method is to adopt Hydrolyze method to extract now.
Jujube tree is the Rhamnaceae jujube, and its fruit---Fructus Jujubae is fruit or the dry fruit that the people loves.In China widely cultivated area is arranged.The Fructus Jujubae fruit is edible both, and is pharmaceutically acceptable again, is the nourishing fruit that integrates nutrition and medicinal health care function.Tracing it to its cause, mainly is the biological active substances that contains high-quality in the Fructus Jujubae fruit, such as triterpene acids, alkaloids, saponins, flavonoid and glycoside etc.Yet processing and technical research only are confined to the Fructus Jujubae fruit, the Different Organs such as other product RUGEN of jujube tree, branch, leaf, flower, skin are not developed and utilized, but be left in the basket as a kind of resource such as Folium Jujubae, about 200 kilograms of the bright Folium Jujubae of average yield per mu, annual Fructus Jujubae is really gathered in the crops and is naturally come off afterwards, bioactive substance wherein is not utilized, and causes great waste.
Summary of the invention
The present invention provides a kind of Folium Jujubae resource that takes full advantage of in order to overcome the deficiencies in the prior art, extracts the purification triterpenic acid to improve the method for Fructus Jujubae added value of product from Folium Jujubae.
In order to solve the problems of the technologies described above, a kind of method of extracting triterpenic acid from Folium Jujubae of the technical solution used in the present invention is carried out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction take alcoholic solution as solvent, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of purification by macroporous resin, obtain triterpenic acid solution.
Described ultrasonic extraction is the alcoholic solution of 65%-73% for add weight percent concentration in described Folium Jujubae powder, and at 45-65 ℃ of lower ultrasonic extraction 25-40min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:6-10L.
Described macroporous resin is NKA-9, S-8, AB-8 or D101.
Described purification by macroporous resin step is: a, described concentrated solution is regulated pH value to 4.5-5.6, then with the flow velocity loading of 1.5-3BV/h, the weight part ratio of described concentrated solution and resin bed is 1:3-6, standing adsorption 0.5-1 hour;
The alcoholic solution coutroi velocity 1.5-3BV/h flushing of b, usefulness weight percent concentration 2%-7%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 60%-75% as eluant, described eluant volume is 1.5-3BV, and the control elution flow rate is that 1.5-3BV/h carries out eluting.
Described triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 71%-80%.
Described triterpenic acid extractum makes triterpenic acid dry powder after super-dry, pulverizing.
The present invention compared with prior art has following beneficial effect.
1, the present invention is on the basis of analysing in depth the Folium Jujubae trophic component; for the characteristics that are rich in the triterpenic acid functional factor in the Folium Jujubae; proposition utilizes Folium Jujubae to extract the technical research of producing triterpenic acid; not only high added value, carried out the comprehensive utilization of Folium Jujubae to high-tech; improved the overall economic efficiency of jujube tree plantation, and because the jujube tree planting scale is large, the Folium Jujubae quantum of output is large; can accomplish scale production, have industrialization value and meaning.
2, the present invention's method to the process using orthogonal test of ultrasonic extraction triterpenic acid in extracting purge process is optimized, and in purifying process, purification condition is optimized, so that the content of triterpenic acid and purity have reached a higher level, and carried out the researchs such as preservation and effect, the standardization of products, formed ripe process route.
Extract triterpenic acid technique and parameter study thereof in the Folium Jujubae
This part research has been carried out the test of four factors, three horizontal quadratures under ul-trasonic irradiation.The design of orthogonal experiment gauge outfit is such as table 1, and extraction time is the ul-trasonic irradiation time.Experimental result and variance analysis see Table 2, table 3.Get dry Folium Jujubae and pulverize, cross 30 mesh sieves.Get 2g Folium Jujubae powder, by the orthogonal experiment requirement, by the different requirements of solid-liquid ratio, add respectively the alcoholic solution of variable concentrations, carry out the ultrasonic extraction of different time.
Above experimental result shows that alcohol concentration and solid-liquid ratio affect significantly extracting the result.In the experimentation, alcohol concentration three gradients are decided to be respectively 90%, 70% and 50%, and alcohol concentration is too high, may cause the cell surface protein degeneration, the material that extracts is stopped and difficult effusion cell, and concentration is excessively low, and possible extract can not be dissolved in the solvent as far as possible.In this experiment, it is 6 solid-liquid ratio that factor solid-liquid ratio significance is mainly derived from level, and namely solid-liquid ratio is that 6 o'clock extraction efficiencies are minimum, and solid-liquid ratio be 8 or 10 o'clock difference not remarkable.Consider that from economic angle can select solid-liquid ratio is 8 to extract.The extraction time impact of factor is not remarkable.Time horizon was respectively 15,30 and 45 minutes, because 15 minutes are shorter, was unfavorable for equipment and manually-operated, and 45 minutes are compared and caused waste, and therefore, extraction time selected be advisable in 30 minutes.
The research of Folium Jujubae triterpenic acid process for refining
Macroporous resin claims again full porous resin, is a present class adsorbent advanced, that have the market competitiveness, and Organic substance is had extremely strong concentrated, centrifugation.Macroporous resin is generally the spherical particle of white, and granularity is 20～60 orders, is the cross linked polymer that a class contains ion exchange group, and its physicochemical property is stable, is insoluble to acid, alkali and organic solvent, is not subjected to the impact of inorganic salts and strong ion low molecular compound.The resin absorption effect is the Van der Waals force that relies between it and the molecule (adsorbate) that is adsorbed, carry out physical absorption by its huge specific surface and work, the organifying compound is according to having absorption affinity and molecular size range thereof separately to reach separation, purification, remove impurity through certain solvent elution, the different purposes such as concentrating.Macroporous adsorbent resin needs to carry out pretreatment before use, namely to commercially available macroporous adsorbent resin with alcohol heating reflux eluting (or heat eluting with the improvement apparatus,Soxhlet's), be washed till noresidue behind the eluent evaporate to dryness.After flinging to solvent, preserves the resin that ethanol is cleaned, and for subsequent use.Need to fill post when using macroporous resin to carry out adsorption bleaching, with ethanol wet method dress post, continue to use ethanol to flow at post and clean during the dress post, frequently check and the ethanol that flows out extremely mix till the muddiness that is not white in color with water.Then with a large amount of distilled water flush away ethanol, for subsequent use.Should be noted that there is the absorption affinity that will greatly reduce resin in a small amount of ethanol.For any depigmenting agent, the regenerative process process that is absolutely necessary.If can not regenerate, mean the increase of depigmenting agent consumption.Macroporous resin column is behind Reusability, and resin surface and inner residual many non-adsorptivity compositions or impurity darken post, and the post effect reduces, thereby also needs regeneration, generally with 95% ethanol be washed till colourless rear go to refine with massive laundering get final product.Deepen available diluted acid or diluted alkaline eluting after washing such as color of resin.Having float available water, alcohol to carry out backwash under the post such as post top can wash out float; affect flow velocity through repeatedly using sometimes post bed extruding tension or resin particle to pulverize; can from post, take out resin, be contained in the larger container and to remove granule or float with water rinse and again fill again post and use.
The macroporous resin of selling on the market is a lot, selects which kind of resin can make work simplification, and the impurity good separating effect is crucial.According to documents and materials, project team has selected four kinds of resins to be analyzed, such as table 4
What at first carry out is the static adsorption reconciliation adsorption test of macroporous resin.Take by weighing in the table 4 four kinds of after pretreatment each 2g of macroporous resin, place triangular flask, then respectively add the certain density triterpenic acid concentrated solution of 20ml, sealing, under the room temperature, the 80r/min 12h that vibrates.Measure triterpenic acid concentration in the solution, the triterpenic acid concentration of original solution deducts the triterpenic acid concentration in the solution behind the vibration 12h, is the adsorbance of resin.Then, remove unnecessary solution, remaining resin carries out desorption with 20ml95% ethanol, and desorption process also is at room temperature, the 80r/min 12h that vibrates.Measure the triterpenic acid content in the alcoholic solution, draw desorption efficiency.In conjunction with adsorption rate, determine optimum resinous type, result such as table 5
As can be seen from Table 5, no matter be adsorption rate, or desorption efficiency, AB-8 is optimum selection.
Secondly, the manufacture and research of AB-8 type resin absorption isotherm.Accurately take by weighing 5 parts of each 2.5g of AB-8 type resin, place respectively 100ml triangular flask and numbering, according to number order add 3,6,9,12, the triterpenic acid solution 20ml of 15mg/g, sealing, under the room temperature, the 80r/min 12h that vibrates.Measure triterpenic acid concentration remaining in the solution, according to adsorbance and corresponding triterpenic acid solution concentration mapping, see Fig. 1.
As shown in Figure 1, under isothermy, AB-8 type resin increases and increases progressively gradually along with concentration the adsorption process of triterpenic acid, and such process meets the Langmuir adsorption isotherm, can think that substantially the AB-8 resin is monolayer adsorption to the absorption of triterpenic acid.
Again, AB-8 type resin dynamic adsorption research.Take by weighing a certain amount of AB-8 type resin, fill after pretreatment 20mm * 300mm chromatographic column, with the triterpenic acid solution loading of concentration 2.00mg/ml, loading speed is 2BV/h, the fraction collection effluent, and survey the concentration of its triterpenic acid.After absorption reaches capacity, calculate the dynamic adsorption saturation capacity, and mapping, see Fig. 2.
Can find out among Fig. 2 that when loading to the 2BV, just can detect the effusion of triterpenic acid in the effluent, the resin saturation can reach 6 BV.Subsequently, tested again reduction loading speed, the time that effluent can detect triterpenic acid prolongs to some extent, but may have influence on the work efficiency of resin, and therefore, this experiment determines that loading speed still is 2BV/h.But suggestion can be used the macroporous resin column series connection, can raise the efficiency, and reduces simultaneously the loss of triterpenic acid.
Alcohol concentration when at last, determining loading pH value and eluting.The triterpenic acid concentrated solution of equivalent is transferred to different pH value with HCl, advances respectively the AB-8 post, then, carry out eluting with 70% ethanol, collect eluent, and survey wherein triterpenic acid concentration, the result sees Table 6.Get a certain amount of triterpenic acid concentrated solution, upper prop carries out eluting with 60%～90% alcoholic solution respectively, collects eluent, measures wherein triterpenic acid concentration, the results are shown in Table 7
Triterpenoids is under acid condition, and its dissolubility can reduce, and may affect the absorption in resin.In the experimental result of table 6, pH value is that 4 o'clock product purity is the highest, but eluting rate not as good as pH value be 5 o'clock high, and find have floccule to occur in the post upper end in the process, may be triterpenic acid at pH value be precipitation under 4 conditions.Compare the result under other pH value condition, pH value is that 5 o'clock eluting rate and product purity all is optimal.
Ethanol is as eluant, and its effect can promote resin swelling, reduces the affinity between triterpenic acid and the resin, and triterpenic acid is dissolved in wherein.In the experiment, be to carry out loading at 5 o'clock at pH value, but carry out eluting with the alcoholic solution of variable concentrations that the result is when alcohol concentration is 70%, the purity of eluting rate and product all is best.
According to above experimental result, the decolouring of the extract triterpenic acid of Chinese date leaf, remove impurity select the AB-8 resin to carry out, and the sample solution pH value is 5 o'clock, and loading speed is 2BV, and the product purity that eluant obtains when being 70% ethanol reaches 75.85%.
Folium Jujubae triterpenic acid product form and preservation and effect research
Can be used as medicine through product that this technique forms and develop and clinical use, the content of total triterpene acid can reach more than 75%.Product characteristics are the brownish black paste, thickness, and density is between 1.25～1.38g/cm
3, this form should not be preserved, and should use as early as possible.Preserve such as need, can pass through microwave, the dry means drying such as infrared, box after, again through pulverizing, the technical process such as sieve makes dry powder.Agglomerate is formed in the easy moisture absorption of this Chinese medical concrete dry powder, therefore should dryly ventilate and preserve.Extract dry powder is compared with above Chinese medical concrete, has easy storage, transportation, the advantages such as long shelf-life.
Description of drawings
Fig. 1 is that the AB-8 resin is to the isothermal adsorption line chart of triterpenic acid.
Fig. 2 is that the AB-8 resin is to the dynamic adsorption figure of triterpenic acid.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment.
A kind of method of from Folium Jujubae, extracting triterpenic acid, carry out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction, ultrasonic extraction is 66% alcoholic solution for adding weight percent concentration in described Folium Jujubae powder, at 50 ℃ of lower ultrasonic extraction 35min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:9L, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of NKA-9 purification, the NKA-9 purification step is: a, described concentrated solution is regulated pH value to 5, then with the flow velocity loading of 2.2BV/h, the weight part ratio of described concentrated solution and resin bed is 1:5, standing adsorption 1 hour; The alcoholic solution coutroi velocity 2BV/h flushing of b, usefulness weight percent concentration 5%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 70% as eluant, described eluant volume is 2.5BV, the control elution flow rate is that 2BV/h carries out eluting, obtains triterpenic acid solution.
Triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 72%.Triterpenic acid extractum makes triterpenic acid dry powder through 60 ℃ of dryings, after pulverizing.
A kind of method of from Folium Jujubae, extracting triterpenic acid, carry out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction, ultrasonic extraction is 72% alcoholic solution for adding weight percent concentration in described Folium Jujubae powder, at 62 ℃ of lower ultrasonic extraction 38min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:7L, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of S-8 purification, the S-8 purification step is: a, described concentrated solution is regulated pH value to 5.2, then with the flow velocity loading of 2.5BV/h, the weight part ratio of described concentrated solution and resin bed is 1:4, standing adsorption 0.5 hour; The alcoholic solution coutroi velocity 2.5BV/h flushing of b, usefulness weight percent concentration 2%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 75% as eluant, described eluant volume is 2.5BV, the control elution flow rate is that 2.5BV/h carries out eluting, obtains triterpenic acid solution.
Triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 75%.
A kind of method of from Folium Jujubae, extracting triterpenic acid, carry out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction, ultrasonic extraction is 68% alcoholic solution for adding weight percent concentration in described Folium Jujubae powder, at 55 ℃ of lower ultrasonic extraction 35min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:8L, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of AB-8 purification, the AB-8 purification step is: a, described concentrated solution is regulated pH value to 4.9, then with the flow velocity loading of 2.5BV/h, the weight part ratio of described concentrated solution and resin bed is 1:5, standing adsorption 0.5 hour; The alcoholic solution coutroi velocity 2.5BV/h flushing of b, usefulness weight percent concentration 7%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 60% as eluant, described eluant volume is 1.8BV, the control elution flow rate is that 1.8BV/h carries out eluting, obtains triterpenic acid solution.
Triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 75.5%.
Embodiment 4
A kind of method of from Folium Jujubae, extracting triterpenic acid, carry out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction, ultrasonic extraction is 70% alcoholic solution for adding weight percent concentration in described Folium Jujubae powder, at 50 ℃ of lower ultrasonic extraction 40min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:7L, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of D101 purification, the D101 purification step is: a, described concentrated solution is regulated pH value to 5, then with the flow velocity loading of 2BV/h, the weight part ratio of described concentrated solution and resin bed is 1:4, standing adsorption 1 hour; The alcoholic solution coutroi velocity 2BV/h flushing of b, usefulness weight percent concentration 4%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 65% as eluant, described eluant volume is 3BV, the control elution flow rate is that 2BV/h carries out eluting, obtains triterpenic acid solution.
Triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 72%.Triterpenic acid extractum makes triterpenic acid dry powder after super-dry, pulverizing.
A kind of method of from Folium Jujubae, extracting triterpenic acid, carry out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction, ultrasonic extraction is 65% alcoholic solution for adding weight percent concentration in described Folium Jujubae powder, at 45 ℃ of lower ultrasonic extraction 40min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:10L, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of AB-8 purification, the AB-8 purification step is: a, described concentrated solution is regulated pH value to 5.6, then with the flow velocity loading of 3BV/h, the weight part ratio of described concentrated solution and resin bed is 1:6, standing adsorption 1 hour; The alcoholic solution coutroi velocity 1.5BV/h flushing of b, usefulness weight percent concentration 6%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 68% as eluant, described eluant volume is 3BV, the control elution flow rate is that 3BV/h carries out eluting, obtains triterpenic acid solution.
Triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 77%, and triterpenic acid extractum makes triterpenic acid dry powder through 70 ℃ of dryings, after pulverizing.
A kind of method of from Folium Jujubae, extracting triterpenic acid, carry out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction, ultrasonic extraction is 73% alcoholic solution for adding weight percent concentration in described Folium Jujubae powder, at 65 ℃ of lower ultrasonic extraction 25min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:6L, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of AB-8 purification, the AB-8 purification step is: a, described concentrated solution is regulated pH value to 4.5, then with the flow velocity loading of 1.5BV/h, the weight part ratio of described concentrated solution and resin bed is 1:3, standing adsorption 0.5 hour; The alcoholic solution coutroi velocity 3BV/h flushing of b, usefulness weight percent concentration 3%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 73% as eluant, described eluant volume is 1.5BV, the control elution flow rate is that 1.5BV/h carries out eluting, obtains triterpenic acid solution.
Triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 78.3%.Triterpenic acid extractum makes triterpenic acid dry powder through 65 ℃ of dryings, after pulverizing.
A kind of method of from Folium Jujubae, extracting triterpenic acid, carry out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction, ultrasonic extraction is 70% alcoholic solution for adding weight percent concentration in described Folium Jujubae powder, at 60 ℃ of lower ultrasonic extraction 30min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:8L, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of AB-8 purification, the AB-8 purification step is: a, described concentrated solution is regulated pH value to 5, then with the flow velocity loading of 2BV/h, the weight part ratio of described concentrated solution and resin bed is 1:4, standing adsorption 0.75 hour; The alcoholic solution coutroi velocity 2BV/h flushing of b, usefulness weight percent concentration 5%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 64% as eluant, described eluant volume is 2BV, the control elution flow rate is that 2BV/h carries out eluting, obtains triterpenic acid solution.
Triterpenic acid solution makes triterpenic acid extractum after concentrated, the total triterpene acid weight percent content of described triterpenic acid extractum is 80%.Triterpenic acid extractum makes triterpenic acid dry powder through 65 ℃ of dryings, after pulverizing.
The present invention can summarize with other the concrete form without prejudice to spirit of the present invention or principal character.Therefore, no matter from that, above-mentioned embodiment of the present invention all can only be thought can not limit invention to explanation of the present invention, claims have been pointed out scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, in the implication suitable with claims of the present invention and any variation in the scope, all should think to be included in the scope of claims.
Claims (6)
1. method of extracting triterpenic acid from Folium Jujubae is characterized in that carrying out according to following steps:
The first step, ultrasonic extraction
After Folium Jujubae cleans, dries, pulverizes, the Folium Jujubae powder that obtains is carried out ultrasonic extraction take alcoholic solution as solvent, pass through again filter cleaner, obtain ultrasonic extraction liquid;
Second step, purification by macroporous resin
With the concentrated ethanol of removing of described ultrasonic extraction liquid, obtain concentrated solution, then use the described concentrated solution of purification by macroporous resin, obtain triterpenic acid solution.
2. a kind of method of from Folium Jujubae, extracting triterpenic acid according to claim 1, it is characterized in that described ultrasonic extraction is the alcoholic solution of 65%-73% for add weight percent concentration in described Folium Jujubae powder, at 45-65 ℃ of lower ultrasonic extraction 25-40min, the proportioning of described Folium Jujubae powder and alcoholic solution is 1Kg:6-10L.
3. a kind of method of extracting triterpenic acid from Folium Jujubae according to claim 1 is characterized in that described macroporous resin is NKA-9, S-8, AB-8 or D101.
4. a kind of method of from Folium Jujubae, extracting triterpenic acid according to claim 3, it is characterized in that described purification by macroporous resin step is: a, described concentrated solution is regulated pH value to 4.5-5.6, then with the flow velocity loading of 1.5-3BV/h, the weight part ratio of described concentrated solution and resin bed is 1:3-6, standing adsorption 0.5-1 hour;
The alcoholic solution coutroi velocity 1.5-3BV/h flushing of b, usefulness weight percent concentration 2%-7%, when effluent stops when being colourless and discards colored solutions, then use the alcoholic solution of weight percent concentration 60%-75% as eluant, described eluant volume is 1.5-3BV, and the control elution flow rate is that 1.5-3BV/h carries out eluting.
5. a kind of method of extracting triterpenic acid from Folium Jujubae according to claim 3 is characterized in that described triterpenic acid solution makes triterpenic acid extractum after concentrated, and the total triterpene acid weight percent content of described triterpenic acid extractum is 71%-80%.
6. a kind of method of extracting triterpenic acid from Folium Jujubae according to claim 5 is characterized in that described triterpenic acid extractum makes triterpenic acid dry powder after super-dry, pulverizing.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103169788A (en) * | 2013-04-16 | 2013-06-26 | 南京中医药大学 | Chinese date leaf extractive and application thereof in preparation of medicament or health food for preventing and treating liver injury |
| CN104146301A (en) * | 2014-08-21 | 2014-11-19 | 天娇红芜湖食品股份有限公司 | Red date whole plant nutrient solution and preparation method thereof |
| CN109498686A (en) * | 2018-12-29 | 2019-03-22 | 河北科技大学 | The preparation method of triterpenic acid in jujube material |
| CN110872337A (en) * | 2019-12-06 | 2020-03-10 | 湖南先伟实业有限公司 | Method for simultaneously preparing different high-purity triterpenic acids from rosemary |
| CN114631545A (en) * | 2022-03-28 | 2022-06-17 | 青岛有为生物科技有限公司 | Plant source rooting agent for promoting plant rooting and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103169788A (en) * | 2013-04-16 | 2013-06-26 | 南京中医药大学 | Chinese date leaf extractive and application thereof in preparation of medicament or health food for preventing and treating liver injury |
| CN104146301A (en) * | 2014-08-21 | 2014-11-19 | 天娇红芜湖食品股份有限公司 | Red date whole plant nutrient solution and preparation method thereof |
| CN109498686A (en) * | 2018-12-29 | 2019-03-22 | 河北科技大学 | The preparation method of triterpenic acid in jujube material |
| CN109498686B (en) * | 2018-12-29 | 2021-07-13 | 河北科技大学 | Preparation method of triterpenic acid in jujube material |
| CN110872337A (en) * | 2019-12-06 | 2020-03-10 | 湖南先伟实业有限公司 | Method for simultaneously preparing different high-purity triterpenic acids from rosemary |
| CN110872337B (en) * | 2019-12-06 | 2022-04-19 | 湖南先伟阳光生物科技有限公司 | Method for simultaneously preparing different high-purity triterpenic acids from rosemary |
| CN114631545A (en) * | 2022-03-28 | 2022-06-17 | 青岛有为生物科技有限公司 | Plant source rooting agent for promoting plant rooting and preparation method thereof |
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| CN103006824B (en) | 2015-04-08 |
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