CN104311616A - Method for extracting high-purity esculine and fraxin from Cortex Fraxini - Google Patents
Method for extracting high-purity esculine and fraxin from Cortex Fraxini Download PDFInfo
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- CN104311616A CN104311616A CN201410519725.1A CN201410519725A CN104311616A CN 104311616 A CN104311616 A CN 104311616A CN 201410519725 A CN201410519725 A CN 201410519725A CN 104311616 A CN104311616 A CN 104311616A
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- China
- Prior art keywords
- fraxin
- cortex fraxini
- extract
- ash
- aesculin
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- CRSFLLTWRCYNNX-UHFFFAOYSA-N Fraxin Natural products OC=1C(OC)=CC=2C=CC(=O)OC=2C=1OC1OC(CO)C(O)C(O)C1O CRSFLLTWRCYNNX-UHFFFAOYSA-N 0.000 title claims abstract description 44
- CRSFLLTWRCYNNX-QBNNUVSCSA-N fraxin Chemical compound OC=1C(OC)=CC=2C=CC(=O)OC=2C=1O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O CRSFLLTWRCYNNX-QBNNUVSCSA-N 0.000 title claims abstract description 44
- XHCADAYNFIFUHF-TVKJYDDYSA-N esculin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC(C(=C1)O)=CC2=C1OC(=O)C=C2 XHCADAYNFIFUHF-TVKJYDDYSA-N 0.000 title claims abstract description 39
- PLXMOAALOJOTIY-FPTXNFDTSA-N Aesculin Natural products OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](O)[C@H]1Oc2cc3C=CC(=O)Oc3cc2O PLXMOAALOJOTIY-FPTXNFDTSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000008589 Cortex Fraxini Substances 0.000 title claims abstract description 28
- 239000000284 extract Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 43
- 239000012071 phase Substances 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 15
- 239000008346 aqueous phase Substances 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 7
- 241000565359 Fraxinus chinensis Species 0.000 claims description 6
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000010612 desalination reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 241000537370 Fraxinus bungeana Species 0.000 claims description 2
- 241001098499 Lanceolata Species 0.000 claims description 2
- 241000207834 Oleaceae Species 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 238000010992 reflux Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 5
- 235000019804 chlorophyll Nutrition 0.000 abstract description 4
- 150000004676 glycans Chemical class 0.000 abstract description 3
- 229920001282 polysaccharide Polymers 0.000 abstract description 3
- 239000005017 polysaccharide Substances 0.000 abstract description 3
- 108010082495 Dietary Plant Proteins Proteins 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 150000002772 monosaccharides Chemical class 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 235000019441 ethanol Nutrition 0.000 description 15
- 238000002425 crystallisation Methods 0.000 description 11
- 230000008025 crystallization Effects 0.000 description 9
- QNHQEUFMIKRNTB-UHFFFAOYSA-N aesculetin Natural products C1CC(=O)OC2=C1C=C(O)C(O)=C2 QNHQEUFMIKRNTB-UHFFFAOYSA-N 0.000 description 6
- ILEDWLMCKZNDJK-UHFFFAOYSA-N esculetin Chemical compound C1=CC(=O)OC2=C1C=C(O)C(O)=C2 ILEDWLMCKZNDJK-UHFFFAOYSA-N 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000001953 recrystallisation Methods 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- GMRNMZUSKYJXGJ-UHFFFAOYSA-N Fraxetin Natural products C1=CC(=O)C(=O)C2=C1C=C(OC)C(O)=C2O GMRNMZUSKYJXGJ-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229930002875 chlorophyll Natural products 0.000 description 3
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- HAVWRBANWNTOJX-UHFFFAOYSA-N fraxetin Chemical compound C1=CC(=O)OC2=C1C=C(OC)C(O)=C2O HAVWRBANWNTOJX-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 241000588214 Fraxinus chinensis subsp. rhynchophylla Species 0.000 description 2
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000161265 Fraxinus baroniana Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- FRHBOQMZUOWXQL-UHFFFAOYSA-L ammonium ferric citrate Chemical compound [NH4+].[Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FRHBOQMZUOWXQL-UHFFFAOYSA-L 0.000 description 1
- 230000001166 anti-perspirative effect Effects 0.000 description 1
- 239000003213 antiperspirant Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N benzo-alpha-pyrone Natural products C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 150000004775 coumarins Chemical class 0.000 description 1
- 238000012136 culture method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003889 eye drop Substances 0.000 description 1
- 229960004642 ferric ammonium citrate Drugs 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002523 gelfiltration Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000000011 iron ammonium citrate Nutrition 0.000 description 1
- 239000004313 iron ammonium citrate Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/075—Benzo[b]pyran-2-ones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a method for extracting high-purity esculine and fraxin from Cortex Fraxini, which comprises the following steps: pulverizing a Cortex Fraxini raw material and extracting under hot reflux by a conventional process, preparing a dual-water phase, dissolving, extracting, concentrating, desalinizing and crystallizing. The method mainly comprises the following steps: 1) preparing a dual-water phase system, and separating to obtain an upper phase and a lower phase for later use, and dissolving a Cortex Fraxini extract in the upper phase solvent; 2) centrifugating or filtering the solution containing the Cortex Fraxini extract, adding a right amount of lower phase solvent, sufficiently stirring and mixing, standing, separating the upper phase solution, and concentrating, thereby effectively removing inorganic substances, monosaccharides, polysaccharides. vegetable proteins, chlorophyl and other solid impurities in the Cortex Fraxini extract and enhancing the contents of esculine and fraxin; and removing salts and other impurities from the solution by conventional processes, and concentrating to a proper concentration, thereby sequentially obtaining the esculine and fraxin crystals. The method solves the problems of low crystallizing tendency, high production cost, complex operation and the like in the existing process of preparing esculine and fraxin from Cortex Fraxini, and has the characteristics of simple production equipment, environment friendliness and the like.
Description
Technical field
The present invention relates to a kind of upper and lower phase solubilize of the double-aqueous phase system adopting the organic solvent of inorganic salt/can dissolve each other with water to be formed, extract the method for aesculin in Cortex Fraxini extract and fraxin, belong to technical field of biochemical industry.
Background technology
At present, the main application of highly purified aesculin has 1. as biochemistry detection reagent: utilize the structure enzyme of the active bacterium of some metabolism that aesculin can be made fast to be hydrolyzed and generate aesculetin and glucose, the aesculetin of generation can decompose with Ferric Ammonium Citrate in substratum or ironic citrate the Fe produced again
2+reaction, generate black-and-blue material, substratum is made to present black-and-blue spot, with this can intuitive and accurate discriminating some containing kind of oxygen bacterium, the soonest can 15 ?can draw detected result in 30 minutes, compared with detecting with the general culture method of traditional employing microorganism, be a kind of novel reagent of microorganism checking fast and effectively.2. for the effect of whitening, sun-proof, antiperspirant can be played in makeup, as important natural cosmetics raw material, existing century-old applicating history.
In addition, aesculin, fraxin have been made eye drop, mouthwass etc. as essential substance basis and have been applied to HUMAN HEALTH adjustment.
At present, the method being separated the highly purified aesculin of preparation and fraxin from the bark of ash can be divided into column chromatography and organic solvent extraction two kinds of methods.Wherein the form of column chromatography mainly contains: the employing gel-filtration filler Superose 12 that the method for separation and purification monomeric compound " from the Barks of Fraxinus chinensis Roxb " (Chinese patent CN102924416B) proposes is carrier of separating, with 10 ?80% Jia Chun ?water for elutriant, fraction collection target components, through concentrating the aesculin, aesculetin, fraxin and the Fraxetin that obtain more than 98%.In addition, " high purity cortex fraxini and preparation method thereof " (Chinese patent CN1955173B) proposes to adopt macroporous resin for absorption and carrier of separating, take deionized water as eluent, after being washed till clarification, collect the elute soln of 10 ~ 15 times of column volumes, concentrated, filtration, recrystallization can obtain the aesculin of purity more than 97%.Aforesaid method adopts gel and macroporous resin as carrier of separating; production cost is high; the adsorptive capacity of carrier is limited; the pre-treatment of carrier and the manipulation of regeneration complexity after using; after repeatedly using, its adsorptive capacity must decline; process repeatability is poor, be unfavorable for operate carry out continuously prepare aesculin and fraxin with mass-producing.The implementation process of organic solvent extractionprocess is, after adopting the oil-soluble impurities such as resin, chlorophyll in chloroform extraction removing bark of ash extracting solution, be extracted with ethyl acetate the impurity such as removing aesculetin wherein again, the concentrated Cortex Fraxini extract liquid through 2 extraction treatment is to suitable volumes, place, crystallization or recrystallization obtain aesculin.The subject matter that the method mainly exists is, containing a large amount of vegetable polysaccharides and monose, albumen etc. in solution to be crystallized, viscosity is high, not easily crystallization.
Therefore, this area needs are a kind of can overcome the problems existed in the production of existing aesculin and fraxin, can reduce production cost, be easy to large-scale production, the high purity cortex fraxini of environmentally friendly type and the method for fraxin.
Summary of the invention
The object of the present invention is to provide a kind of method extracting high purity cortex fraxini and fraxin from the bark of ash, the method easy handling and large-scale production, there is the features such as production cost is low, equipment simple, environmental protection.
The invention provides a kind of method extracting high purity cortex fraxini and fraxin from the bark of ash, it is characterized in that comprising the following steps:
(1) methyl alcohol or water ordinary method is adopted to obtain containing the Cortex Fraxini extract of the different mass such as aesculin, fraxin concentration;
(2) prepare double-aqueous phase system, and be separated the upper and lower phase solution obtaining double water-phase, repeatedly dissolve Cortex Fraxini extract with phase solution, to not containing aesculin and fraxin in Cortex Fraxini extract;
(3) centrifugal or filter above-mentioned containing after the solution of aesculin and fraxin, add the lower phase solution of above-mentioned solution 1 ~ 3 times amount, abundant extraction, supreme mutually in solid substance impurity ratio no longer obviously reduce till, be separated the upper phase solution obtained, the concentrated solution obtained mainly containing aesculin and fraxin;
(4), after adopting conventional means desalination and oil-soluble impurities composition, concentrated, crystallization obtains high purity cortex fraxini and fraxin.
Described double-aqueous phase system adopts Na
2hPO
4, (NH
4)
2sO
4, K
2hPO
4and the inorganic salt that can form double water-phase prepare gained.
Organic solvent in described double-aqueous phase system is methyl alcohol, ethanol.
The solution temperature of described double-aqueous phase system is 20 ° ~ 30 DEG C.
The indication bark of ash of the present invention, refers to the certified products bark of ash medicinal material (comprising Oleaceae fraxinus rhynchophylla Hance Fraxinus rhynchophylla Hance, Chinese ash Fraxinus chinensis Roxb., sharp leaf Chinese ash Fraxinus szaboana Lingelsh. or place post Chinese ash Fraxinus stylosa Lingelsh.) that specifies with version Chinese Pharmacopoeia in 2010 and lanceolata Chinese ash Fraxinus baroniana Diels, the dry branch skin of Fraxinus bungeana Fraxinus bungeana DC. or dry hide.And as raw material, through the powder etc. that ordinary method obtains through to dust etc. through refluxing extraction, concentrated fluid extract or medicinal extract as methyl alcohol, ethanol, water, the mass concentration of aesculin and fraxin is generally respectively 5% ~ 30% and about 3% ~ 20%.
In said extracted thing, principle active component comprises aesculin (Esculin), aesculetin (Aesculetin,), the coumarins composition such as fraxin (Fraxin), Fraxetin (Fraxetin), and a large amount of chlorophyll, carbohydrate and resin etc., wherein the chemical structural formula of aesculin and fraxin is as follows:
Extraction in the inventive method and crystallisation step belong to ordinary method in the art.
Such as, described extraction step can carry out as follows: by the bark of ash meal after pulverizing as in refluxing extraction tank, with the water of raw material weight 5 times amount or methyl alcohol for Extraction solvent, refluxing extraction is after 3 hours, release and filter and obtain extracting solution, normal pressure or vacuum concentration are to the concentrated extract of proportion 1.10 ~ 1.20.
Such as, described crystallisation step can carry out as follows: after the upper phase solution containing aesculin and fraxin is after treatment concentrated, adopt ordinary method, after being added to certain density organic solvent desalination, be concentrated into suitable volumes, add aesculin crystal seed, crystallization, obtain aesculin crude product, add a small amount of ethanol again in mother liquor, place, crystallization, obtain fraxin crude product, the two can obtain more than 98% aesculin and fraxin product with ethyl alcohol recrystallization again.
The present invention adopts the conventional organic solvent such as inorganic salt with low cost and ethanol to prepare double-aqueous phase system, is separated up and down that phase solution is as dissolution solvent and extraction solvent, and industrial scale easily controls, and production cost is low, is easy to crystallization and obtains target component.
The present invention effectively can remove inorganics in Cortex Fraxini extract, monose, polysaccharide and the solid impurity such as vegetable-protein, chlorophyll, improves the content of aesculin and fraxin.
The present invention adopts the cheap chemical industry auxiliary material be easy to get; through dissolving, extracting and routine operation, from the bark of ash, the scale production process of highly purified aesculin and fraxin two kinds of natural products can be obtained simultaneously, easy and simple to handle; technical process is short, can effectively reduce production cost and production difficulty.
In addition, the present invention mainly adopts to the inorganic salt of people and production environment toxicological harmless and organic reagent as extraction carrier, and industrial scale very easily controls.Adopt Ye ?liquid extraction the mode of production make target component lose little, product yield is high.
Accompanying drawing explanation
Fig. 1 is the HPLC collection of illustrative plates of bark of ash raw material.
Fig. 2 is the aesculin HPLC collection of illustrative plates that embodiment obtains.
Fig. 3 is the fraxin HPLC collection of illustrative plates that embodiment obtains.
Embodiment
Below in conjunction with example, the invention will be further described." traditional Chinese chemical contrast workbook " (China Medical Science Press, P129 ?130 in 2000) that in example, TLC and HPLC detection method is edited see Chen Dechang.
Get bark of ash medicinal material (place of production: Shaanxi) 1 kilogram, be ground into meal, add 6 kg ethanol, reflux 1 hour, leaches solution; Add 4 kg ethanol reflux again 1 hour, leach solution, merge twice gained extracting solution, concentrating under reduced pressure reclaims ethanol, obtains the medicinal extract that proportion is 1.15, for subsequent use.
Keep envrionment temperature 20 DEG C, prepare double-aqueous phase system (ammonium sulfate, the ethanol mass concentration in system is respectively 14% and 30%) with ammonium sulfate, ethanol, water, fully after mixing, leave standstill to upper and lower phase volume without considerable change, separate upper and lower phase solution, for subsequent use.
Adopt a small amount of mode repeatedly, fully dissolve medicinal extract with phase solution on above-mentioned gained, detect with TLC or HPLC, in medicinal extract without obvious aesculin, detected resultMerge above-mentioned solution, totally 4.2 liters, this solution of phase solution extraction 2 times under adding 0.5 liter respectively, till in supreme phase solution, solid impurity ratio no longer obviously reduces.Isolate the solution mutually containing aesculin and fraxin, be evaporated to 0.2 liter, add ethanol to alcohol content more than 90%, removing inorganic salt, concentrating under reduced pressure removing ethanol again, gained solution adds suitable quantity of water and heating for dissolving, leaves standstill, crystallization, filter, obtain aesculin crude product 16.8g, with ethyl alcohol recrystallization, obtain the white aesculin 8.6g that purity is 98.6%; Above-mentioned mother liquor is concentrated into 1/2 of original volume again, adds micro-fraxin crystallization and a small amount of ethanol, again places, crystallization, filters, obtains the faint yellow fraxin needle crystal that 6.8g purity is 98.2%.
Claims (5)
1. from the bark of ash, extract a method for high purity cortex fraxini and fraxin, it is characterized in that comprising the following steps:
(1) methyl alcohol or water ordinary method is adopted to obtain containing the Cortex Fraxini extract of the different mass such as aesculin, fraxin concentration;
(2) prepare double-aqueous phase system, and be separated the upper and lower phase solution obtaining double water-phase, repeatedly dissolve Cortex Fraxini extract with phase solution, to not containing aesculin and fraxin in Cortex Fraxini extract;
(3) centrifugal or filter above-mentioned containing after the solution of aesculin and fraxin, add the lower phase solution of above-mentioned solution 1 ~ 3 times amount, abundant extraction, supreme mutually in solid substance impurity ratio no longer obviously reduce till, be separated the upper phase solution obtained, the concentrated solution obtained mainly containing aesculin and fraxin;
(4), after adopting conventional means desalination and oil-soluble impurities composition, condensing crystal obtains high purity cortex fraxini and fraxin.
2. from the bark of ash, extract as claimed in claim 1 the method for high purity cortex fraxini and fraxin, it is characterized in that certified products bark of ash medicinal material that bark of ash raw material used comprises version Chinese Pharmacopoeia in 2010 and specify, lanceolata Chinese ash, Fraxinus bungeana and other contain dry branch skin or the dry hide of the Oleaceae plants of aesculin and fraxin; Wherein the mass concentration of aesculin and fraxin is respectively 5% ~ 30% and 3% ~ 20%.
3. from the bark of ash, extract the method for high purity cortex fraxini and fraxin as claimed in claim 1, it is characterized in that described double-aqueous phase system adopts Na
2hPO
4, (NH
4)
2sO
4, K
2hPO
4and the inorganic salt that can form double water-phase prepare gained.
4. from the bark of ash, extract the method for high purity cortex fraxini and fraxin as claimed in claim 1, it is characterized in that the organic solvent in described double-aqueous phase system is methyl alcohol, ethanol.
5. from the bark of ash, extract the method for high purity cortex fraxini and fraxin as claimed in claim 1, it is characterized in that the solution temperature of described double-aqueous phase system is 20 ° ~ 30 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410519725.1A CN104311616B (en) | 2014-09-30 | 2014-09-30 | A kind of extraction high purity cortex fraxini and method of fraxin from Cortex Fraxini |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410519725.1A CN104311616B (en) | 2014-09-30 | 2014-09-30 | A kind of extraction high purity cortex fraxini and method of fraxin from Cortex Fraxini |
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| Publication Number | Publication Date |
|---|---|
| CN104311616A true CN104311616A (en) | 2015-01-28 |
| CN104311616B CN104311616B (en) | 2016-08-24 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109134562A (en) * | 2018-10-26 | 2019-01-04 | 宁县恒瑞康生物科技有限公司 | A kind of aesculin purification process |
| WO2019225983A1 (en) * | 2018-05-25 | 2019-11-28 | 한국 한의학 연구원 | Composition for preventing, ameliorating, or treating depression and anxiety disorders, comprising fraxin as active ingredient |
| CN111662345A (en) * | 2020-05-14 | 2020-09-15 | 温州医科大学 | Method for extracting chicory glycoside from Fraxinus chinensis Franch leaves |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019225983A1 (en) * | 2018-05-25 | 2019-11-28 | 한국 한의학 연구원 | Composition for preventing, ameliorating, or treating depression and anxiety disorders, comprising fraxin as active ingredient |
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| CN111662345A (en) * | 2020-05-14 | 2020-09-15 | 温州医科大学 | Method for extracting chicory glycoside from Fraxinus chinensis Franch leaves |
| CN111662345B (en) * | 2020-05-14 | 2021-04-06 | 温州医科大学 | A kind of method for extracting cichorin from leaves of ash tree |
| CN114767737A (en) * | 2022-06-21 | 2022-07-22 | 上海中医药大学 | A kind of Qinpi extract, its preparation method and application |
| CN114767737B (en) * | 2022-06-21 | 2022-11-29 | 上海中医药大学 | Cortex fraxini extract, preparation method and application thereof |
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