CN104689600B - The extraction of Folium Kaki total flavones and purification process - Google Patents
The extraction of Folium Kaki total flavones and purification process Download PDFInfo
- Publication number
- CN104689600B CN104689600B CN201510104876.5A CN201510104876A CN104689600B CN 104689600 B CN104689600 B CN 104689600B CN 201510104876 A CN201510104876 A CN 201510104876A CN 104689600 B CN104689600 B CN 104689600B
- Authority
- CN
- China
- Prior art keywords
- extraction
- folium kaki
- organic solvent
- purification process
- total flavones
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 244000236655 Diospyros kaki Species 0.000 title claims abstract description 74
- 235000008597 Diospyros kaki Nutrition 0.000 title claims abstract description 73
- 238000000605 extraction Methods 0.000 title claims abstract description 62
- 229930003944 flavone Natural products 0.000 title claims abstract description 43
- 235000011949 flavones Nutrition 0.000 title claims abstract description 43
- 150000002213 flavones Chemical class 0.000 title claims abstract description 42
- 238000000746 purification Methods 0.000 title claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 35
- 239000000287 crude extract Substances 0.000 claims abstract description 27
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 238000003809 water extraction Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 10
- 239000012467 final product Substances 0.000 claims description 9
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 7
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 7
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 7
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims 3
- 239000008346 aqueous phase Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004945 emulsification Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 20
- 239000000843 powder Substances 0.000 description 11
- 239000002904 solvent Substances 0.000 description 10
- 230000033228 biological regulation Effects 0.000 description 8
- 230000006837 decompression Effects 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 238000005086 pumping Methods 0.000 description 8
- 238000011084 recovery Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 238000007670 refining Methods 0.000 description 5
- 239000008280 blood Substances 0.000 description 4
- 210000004369 blood Anatomy 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229930003935 flavonoid Natural products 0.000 description 3
- 150000002215 flavonoids Chemical class 0.000 description 3
- 235000017173 flavonoids Nutrition 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 2
- 230000001093 anti-cancer Effects 0.000 description 2
- 230000017531 blood circulation Effects 0.000 description 2
- 230000036772 blood pressure Effects 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- -1 triterpenoid compound Chemical class 0.000 description 2
- 206010065559 Cerebral arteriosclerosis Diseases 0.000 description 1
- 206010008570 Chloasma Diseases 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- OVSQVDMCBVZWGM-IDRAQACASA-N Hirsutrin Natural products O([C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1)C1=C(c2cc(O)c(O)cc2)Oc2c(c(O)cc(O)c2)C1=O OVSQVDMCBVZWGM-IDRAQACASA-N 0.000 description 1
- FVQOMEDMFUMIMO-UHFFFAOYSA-N Hyperosid Natural products OC1C(O)C(O)C(CO)OC1OC1C(=O)C2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 FVQOMEDMFUMIMO-UHFFFAOYSA-N 0.000 description 1
- 208000003351 Melanosis Diseases 0.000 description 1
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 1
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 201000005851 intracranial arteriosclerosis Diseases 0.000 description 1
- GXMWXESSGGEWEM-UHFFFAOYSA-N isoquercitrin Natural products OCC(O)C1OC(OC2C(Oc3cc(O)cc(O)c3C2=O)c4ccc(O)c(O)c4)C(O)C1O GXMWXESSGGEWEM-UHFFFAOYSA-N 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- OVSQVDMCBVZWGM-QSOFNFLRSA-N quercetin 3-O-beta-D-glucopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-QSOFNFLRSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses the extraction of a kind of Folium Kaki total flavones and purification process, comprise the following steps: (1) Folium Kaki water extraction, obtain Folium Kaki crude extract；(2) Folium Kaki crude extract adds extractant, multistage centrifugal extraction equipment carries out multistage centrifugal extraction, it is thus achieved that organic solvent phase；(3) adopt the mode of one-stage centrifugal back extraction remove organic solvent mutually in impurity, collect and remove the organic solvent phase after impurity, concentration, dry, obtain highly purified Folium Kaki total flavones.The extraction of the present invention and purification process overcome Emulsification effect existing in existing Folium Kaki total flavones extraction process, significantly reduce the consumption of organic solvent, effectively reduce production cost, shorten the production cycle, and prouctiveness is high.Detecting through HPLC method, the inventive method is obtained in that highly purified Folium Kaki total flavones, and product total flavones purity reaches as high as 99.3%.
Description
Technical field
The present invention relates to the extracting method of a kind of total flavones, particularly relate to extraction and the purification process of Folium Kaki total flavones, belong to extraction and the purification art of Folium Kaki total flavones.
Background technology
Folium Kaki is the fresh or dried leaves of plant persimmon (DiospyroskakiThunb.).Modern science analysis finds, Folium Kaki is except containing abundant vitamin C, possibly together with triterpenoid compound, tannins and substantial amounts of flavone compound, such as Quercetin, kaempferol, isoquercitrin etc..Research find Folium Kaki there is antibacterial, antiinflammatory, invigorate blood circulation, blood pressure lowering, blood fat reducing, anticancer, removing chloasma effect, can extensive exploitation for fields such as food, medicine and cosmetics.Wherein, Folium Kaki total flavones has the pharmacological actions such as activating blood circulation to dissipate blood stasis, dredging collateral, hemostasis, antioxidation, anticancer, blood sugar lowering, blood pressure lowering, blood fat reducing, it is clinically used for treatment coronary heart disease, cerebral arteriosclerosis, determined curative effect (Cao Shan etc., Folium Kaki total flavones pharmacological research and clinical practice thereof are inquired into, traditional Chinese medical science journal, the 2012, the 27th volume, total 171st phase, p987-989).
Obtain the most important for guaranteeing Folium Kaki extract performance medical treatment and health-care effect of highly purified Folium Kaki total flavones.Prepare the method for higher degree Folium Kaki total flavones at present to be usually first Folium Kaki and carry precipitate with ethanol or containing alcohol water raises Folium Kaki crude flavonoid powder through water (or aqueous alkali), obtain sterling total flavones by refining further for Folium Kaki crude flavonoid powder.The technique that Folium Kaki crude flavonoid powder is refined mainly has ethyl acetate repeatedly extraction and macroreticular resin absorbing method.Because problems such as emulsifyings, adopt the process for purification that ethyl acetate repeatedly extracts to there is the comparatively serious problems such as production cycle length, product purity are not high, solvent expends greatly, power consumption is high, efficiency-cost ratio is low, seriously constrain industrialized production.When adopting resin adsorption method to carry out refining, owing to resin inevitably deterioration in use causes the uncertainty of technological parameter, ultimately result in product quality shakiness；Additionally, adopt resin adsorption method to carry out the refining problems such as to there is also solvent-oil ratio big, production cycle length, it would be highly desirable to improve.
Summary of the invention
The technical problem to be solved is to provide extraction and the purification process of a kind of new Folium Kaki total flavones, and the method is with short production cycle, it is high to expend few, the prepared total flavones purity of solvent.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The extraction of a kind of Folium Kaki total flavones and purification process, comprise the following steps:
(1) Folium Kaki water extraction, obtains Folium Kaki crude extract；(2) Folium Kaki crude extract adds extractant, adopt the mode that multistage centrifugal extracts to obtain organic solvent phase in multistage centrifugal extraction equipment；(3) adopt the mode of one-stage centrifugal back extraction remove organic solvent mutually in impurity, collect and remove the organic solvent phase after impurity, concentration, dry, obtain high-purity Folium Kaki total flavones.
Preferably, dry Folium Kaki is added 8-12 times of quality water by step (1), decocts 2 times, decoct 0.5-2h every time, merge decoction liquor, be evaporated to the extractum of proportion 1.01-1.15, obtain Folium Kaki crude extract；
In step (2), counting by volume, the ratio of Folium Kaki crude extract and extractant is preferably 1:0.3-1.2；Described extractant include but not limited in ethyl acetate, methyl acetate, butyl acetate, n-butyl alcohol or dichloromethane any or multiple according to arbitrary proportion composition mixture, it is preferred to ethyl acetate；
Multistage centrifugal described in step (2) extracts and is preferably 2-10 level Centrifugical extraction, more preferably 3-6 level Centrifugical extraction, it is particularly preferred to be 5 grades of Centrifugical extractions；Described centrifugal rotational speed is 1000-10000rpm, it is preferred to 1500-8000rpm, and optimum is 2000-3000rpm.
Described in step (3) adopt one-stage centrifugal back extraction mode remove organic solvent mutually in impurity include to organic solvent mutually in add deionized water be centrifuged back extraction；Preferably, counting by volume, the ratio of organic solvent phase and deionized water is 1:0.3-1.2；The preferred 1000-10000rpm of described centrifugal rotational speed, it is preferred to 1500-8000rpm, optimum is 2000-3000rpm.
The extraction of Folium Kaki total flavones of the present invention and purification process, separation efficiency is high, with short production cycle；Overcoming Emulsification effect existing in existing extraction Folium Kaki total flavones process, significantly reduce the consumption of organic solvent, effectively reduce production cost, production efficiency is high；Detecting through HPLC method, the inventive method is obtained in that highly purified Folium Kaki total flavones product, and total flavones purity reaches as high as 99.3%.The refining Folium Kaki total flavones that the present invention extracts may be used for medicine, food, health product, the raw material of cosmetics or additive, of many uses.
Accompanying drawing explanation
Fig. 1 is the process chart of the refining Folium Kaki total flavones of Centrifugical extraction of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment further describe the present invention, advantages of the present invention and feature will be with describe and apparent.It should be understood that described embodiment is only exemplary, the scope of the present invention is not constituted any restriction.It will be understood by those skilled in the art that and the details of technical solution of the present invention and form can be modified or replace lower without departing from the spirit and scope of the present invention, but these amendments or replacement each fall within protection scope of the present invention.
Illustrate: in following example, used Folium Kaki is all same source, the Folium Kaki of same batch, is absent from any substantial differences.
Embodiment 1
Weighing Folium Kaki coarse powder (30 order) 100g, add water 1000ml, micro-decoction 60min that boils, and leaches decoction liquor；Filtering residue add water 800ml micro-boil decoction 35min, merge decoction liquor, be evaporated to the extractum of proportion 1.03, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into isopyknic ethyl acetate solution simultaneously, unlatching centrifugal rotational speed is 2000rpm, carry out 5 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 2000rpm, being centrifuged back extraction, collect the ethyl acetate solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 99.3%.
Embodiment 2
Weighing Folium Kaki coarse powder (30 order) 1000g, add water 12000ml, micro-decoction 50min that boils, and leaches decoction liquor；Filtering residue add water 8000ml micro-boil decoction 30min, merge decoction liquor, be evaporated to proportion 1.09, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into isopyknic ethyl acetate solution simultaneously, unlatching centrifugal rotational speed is 6000rpm, carry out 2 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 6000rpm, being centrifuged back extraction, collect the ethyl acetate solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 89.2%.
Embodiment 3
Weighing Folium Kaki coarse powder (30 order) 100g, add water 1200ml, micro-decoction 90min that boils, and leaches decoction liquor；Filtering residue add water 1000ml micro-boil decoction 45min, merge decoction liquor, be evaporated to proportion 1.08, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into isopyknic butanol solution simultaneously, unlatching centrifugal rotational speed is 5000rpm, carry out 3 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 5000rpm, being centrifuged back extraction, collect the butanol solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 88.6%.
Embodiment 4
Weighing Folium Kaki coarse powder (30 order) 100g, add water 1000ml, micro-decoction 60min that boils, and leaches decoction liquor；Filtering residue add water 800ml micro-boil decoction 35min, merge decoction liquor, be evaporated to the extractum of proportion 1.06, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into isopyknic methyl acetate solution simultaneously, unlatching centrifugal rotational speed is 2000rpm, carry out 3 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 2000rpm, being centrifuged back extraction, collect the methyl acetate solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 87.4%.
Embodiment 5
Weighing Folium Kaki coarse powder (30 order) 100g, add water 1000ml, micro-decoction 60min that boils, and leaches decoction liquor；Filtering residue add water 800ml micro-boil decoction 35min, merge decoction liquor, be evaporated to the extractum of proportion 1.06, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into isopyknic butyl acetate solution simultaneously, unlatching centrifugal rotational speed is 5000rpm, carry out 5 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 5000rpm, being centrifuged back extraction, collect the butyl acetate solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 96.3%.
Embodiment 6
Weighing Folium Kaki coarse powder (30 order) 100g, add water 800ml, micro-decoction 120min that boils, and leaches decoction liquor；Filtering residue add water 800ml micro-boil decoction 30min, merge decoction liquor, be evaporated to the extractum of proportion 1.09, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into the butyl acetate solution of organic solvent 0.3 times of volume mutually simultaneously, unlatching centrifugal rotational speed is 2000rpm, carry out 4 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 2000rpm, being centrifuged back extraction, collect the methyl acetate solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 84.1%.
Embodiment 7
Weighing Folium Kaki coarse powder (30 order) 100g, add water 800ml, micro-decoction 120min that boils, and leaches decoction liquor；Filtering residue add water 800ml micro-boil decoction 30min, merge decoction liquor, be evaporated to the extractum of proportion 1.01, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into the methyl acetate solution of organic solvent 0.3 times of volume mutually simultaneously, unlatching centrifugal rotational speed is 2500rpm, carry out 5 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 2500rpm, being centrifuged back extraction, collect the methyl acetate solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 97.9%.
Embodiment 8
Weighing Folium Kaki coarse powder (30 order) 1000g, add water 12000ml, micro-decoction 50min that boils, and leaches decoction liquor；Filtering residue add water 8000ml micro-boil decoction 30min, merge decoction liquor, be evaporated to proportion 1.02, obtain Folium Kaki crude extract；Folium Kaki crude extract is pumped into plural serial stage centrifugal extractor (purchased from Zhong Wo Machinery Co., Ltd. of Zhangjagang City, CTL50 type centrifugal extractor), pump into isopyknic butyl acetate solution simultaneously, unlatching centrifugal rotational speed is 3000rpm, carry out 6 grades of series connection Centrifugical extractions, collect organic solvent phase；When centrifugal stripping cells, pumping into and the deionized water of organic solvent equal volume, unlatching centrifugal rotational speed is 3000rpm, being centrifuged back extraction, collect the butyl acetate solution after the back extraction removal of impurity, decompression and solvent recovery is to dry, gained dried object is complete at 50 DEG C of drying under reduced pressure further, to obtain final product.
Adopt the Pharmacopoeia of the People's Republic of China 2010 editions regulation HPLC to analyze method and measure the purity of product total flavones；Measurement result: the purity of product total flavones is 90.8%.
Claims (8)
1. the extraction of a Folium Kaki total flavones and purification process, it is characterised in that step is as follows:
(1) Folium Kaki water extraction, obtains Folium Kaki crude extract；(2) Folium Kaki crude extract adds extraction organic solvent, multistage centrifugal extraction equipment carries out multistage centrifugal extraction, it is thus achieved that organic solvent phase；(3) adopt the mode of one-stage centrifugal back extraction remove organic solvent mutually in impurity, collect and remove the organic solvent phase after impurity, concentration, dry, to obtain final product；Wherein, the multistage centrifugal described in step (2) extracts is 5 grades of Centrifugical extractions；Described centrifugal rotational speed is 2000-3000rpm；The centrifugal rotational speed of the one-stage centrifugal back extraction described in step (3) is 2000-3000rpm.
2. extraction described in claim 1 and purification process, it is characterised in that: dry Folium Kaki is added 8-12 times of quality water by step (1), decocts 2 times, decoct 0.5-2h every time, merge decoction liquor, be evaporated to the extractum of proportion 1.01-1.15, obtain Folium Kaki crude extract.
3. extraction described in claim 2 and purification process, it is characterised in that: dry Folium Kaki is added 10 times of quality water by step (1), decocts 2 times, decoct 35-60min every time, merge decoction liquor, be evaporated to the extractum of proportion 1.06, obtain Folium Kaki crude extract.
4. extraction described in claim 1 and purification process, it is characterised in that: in step (2), counting by volume, the ratio of Folium Kaki crude extract and extractant is 1:0.3-1.2.
5. extraction described in claim 1 and purification process, it is characterised in that: described extractant includes but not limited to any or multiple mixture according to arbitrary proportion composition in ethyl acetate, methyl acetate, butyl acetate, n-butyl alcohol or dichloromethane.
6. extraction described in claim 5 and purification process, it is characterised in that: described extractant is ethyl acetate.
7. extraction described in claim 1 and purification process, it is characterised in that: in step (3) to organic solvent mutually in add deionized water and be centrifuged back extraction.
8. extraction described in claim 7 and purification process, it is characterised in that: counting by volume, the ratio of organic solvent phase and aqueous phase is 1:0.3-1.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510104876.5A CN104689600B (en) | 2015-03-10 | 2015-03-10 | The extraction of Folium Kaki total flavones and purification process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510104876.5A CN104689600B (en) | 2015-03-10 | 2015-03-10 | The extraction of Folium Kaki total flavones and purification process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104689600A CN104689600A (en) | 2015-06-10 |
| CN104689600B true CN104689600B (en) | 2016-07-06 |
Family
ID=53337384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510104876.5A Expired - Fee Related CN104689600B (en) | 2015-03-10 | 2015-03-10 | The extraction of Folium Kaki total flavones and purification process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104689600B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111440700B (en) * | 2020-04-17 | 2022-09-23 | 北京化工大学 | Fat-soluble fermentation product online fermentation in-situ separation coupling device and method |
| CN114224933B (en) * | 2022-01-17 | 2023-01-24 | 广州思沛医药科技股份有限公司 | Persimmon leaf flavone extract and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009215253A (en) * | 2008-03-12 | 2009-09-24 | Tama Seikagaku Kk | Carbohydrate metabolism control substance originated from persimmon leaf and persimmon branch |
| CN101637492A (en) * | 2009-08-31 | 2010-02-03 | 陕西师范大学 | Preparation method of total flavonoids in persimmon leaves and application of total flavonoids in liver-protecting drugs and health foods |
| CN101744863A (en) * | 2010-01-29 | 2010-06-23 | 广州白云山和记黄埔中药有限公司 | Persimmon leaf extract preparation, preparing method thereof and application thereof |
| KR20120121684A (en) * | 2011-04-27 | 2012-11-06 | 주식회사 에버미라클 | Antipruritic composition containing astragalin and quercetin |
-
2015
- 2015-03-10 CN CN201510104876.5A patent/CN104689600B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009215253A (en) * | 2008-03-12 | 2009-09-24 | Tama Seikagaku Kk | Carbohydrate metabolism control substance originated from persimmon leaf and persimmon branch |
| CN101637492A (en) * | 2009-08-31 | 2010-02-03 | 陕西师范大学 | Preparation method of total flavonoids in persimmon leaves and application of total flavonoids in liver-protecting drugs and health foods |
| CN101744863A (en) * | 2010-01-29 | 2010-06-23 | 广州白云山和记黄埔中药有限公司 | Persimmon leaf extract preparation, preparing method thereof and application thereof |
| KR20120121684A (en) * | 2011-04-27 | 2012-11-06 | 주식회사 에버미라클 | Antipruritic composition containing astragalin and quercetin |
Non-Patent Citations (2)
| Title |
|---|
| 不同方法提取柿叶总黄酮含量的比较;王晓丹等;《泰山医学院学报》;20080625(第06期);第454-455页 * |
| 黄酮类化合物提取工艺研究;张睿等;《食品与机械》;20030225(第01期);第21-22页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104689600A (en) | 2015-06-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109942380B (en) | Method for preparing cannabidiol by high-speed counter-current chromatography separation and purification | |
| CN102579511B (en) | Method for integrally extracting steroidal compounds, polysaccharides and polyphenols from inonotus obliquus | |
| CN102584766A (en) | Method for simultaneously separating dihydromyricetin and myricetin from ampelopsis plant | |
| CN104689600B (en) | The extraction of Folium Kaki total flavones and purification process | |
| CN104000840B (en) | Preparation method of extractive containing gastrodin and gastrodia elata polysaccharide | |
| CN104098634B (en) | The technique of combined extracting Neosynephrine, hesperidin and PMFs in Fructus Aurantii Immaturus | |
| CN102836194B (en) | Extraction method of affine cudweed total flavonoids | |
| CN111450139A (en) | Eutectic solvent and method for preparing spina gleditsiae total flavonoids by using same | |
| CN109438213B (en) | Isopentenyl chalcone compound and preparation method thereof | |
| CN104606276B (en) | A method of extracting small molecule persimmon leaf flavone from persimmon leaf | |
| CN105884754A (en) | Fine extraction method of silibinin | |
| CN108069930A (en) | A kind of method of combined extracting galangal volatile oil and Galangin from galangal | |
| CN103585424A (en) | Method for extracting total flavone from Chinese chive seeds | |
| CN106138203A (en) | A kind of preparation method of danshen powder | |
| CN104721240B (en) | A kind of technique extracted from leaf of Moringa and separate Moringa flavones and Moringa saponin(e | |
| CN104817601A (en) | Mixture containing three flavone components extracted from Lysimachia capillipes, preparation thereof, and preparation method of mixture and preparation | |
| CN102898411A (en) | Proanthocyanidin extraction technology | |
| CN104211667A (en) | Plant extract applied in taxol preparation and preparation method thereof | |
| CN104262640B (en) | The extracting method of rubber | |
| CN114570058A (en) | Method for comprehensively extracting tea seed components | |
| CN103408522A (en) | Method for extracting high-purity aesculetin from euphorbia lathyris fruit | |
| CN109096076B (en) | Chalcone compound and preparation method thereof | |
| CN101879265A (en) | Process for co-producing total saponins and polysaccharide from star-of-Bethlehem | |
| CN108822067B (en) | Method for preparing tectorigenin from pueraria flower | |
| CN105777922A (en) | Pilose asiabell root polysaccharide extraction method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160830 Address after: 110300 Dongcheng Committee, Dongcheng Street, Xinmin County, Liaoning Patentee after: Shenyang innovation pharmaceutical research and production transformation base Co.,Ltd. Address before: 110300 Xinmin Industrial Development Zone, Liaoning, Shenyang Patentee before: SHENYANG DONGXIN PHARMACEUTICAL CO.,LTD. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160706 |