CN108524554A - A kind of method of general flavone in ultrasonic wave assisted extraction common polytrichum herb - Google Patents
A kind of method of general flavone in ultrasonic wave assisted extraction common polytrichum herb Download PDFInfo
- Publication number
- CN108524554A CN108524554A CN201810779583.0A CN201810779583A CN108524554A CN 108524554 A CN108524554 A CN 108524554A CN 201810779583 A CN201810779583 A CN 201810779583A CN 108524554 A CN108524554 A CN 108524554A
- Authority
- CN
- China
- Prior art keywords
- polytrichum
- herb
- common
- general flavone
- extract
- 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.)
- Granted
Links
- 241000195879 Polytrichum Species 0.000 title claims abstract description 137
- 229930003944 flavone Natural products 0.000 title claims abstract description 75
- 235000011949 flavones Nutrition 0.000 title claims abstract description 75
- 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 title claims abstract description 69
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 69
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000000605 extraction Methods 0.000 title claims abstract description 25
- 239000000284 extract Substances 0.000 claims abstract description 49
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000000287 crude extract Substances 0.000 claims abstract description 25
- 239000003960 organic solvent Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000397 disodium phosphate Inorganic materials 0.000 claims abstract description 11
- 235000019800 disodium phosphate Nutrition 0.000 claims abstract description 11
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 90
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 238000002156 mixing Methods 0.000 claims description 31
- 238000010521 absorption reaction Methods 0.000 claims description 27
- 239000000706 filtrate Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 25
- 239000003480 eluent Substances 0.000 claims description 24
- 239000011148 porous material Substances 0.000 claims description 19
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 238000011068 loading method Methods 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000002137 ultrasound extraction Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 7
- 150000002213 flavones Chemical class 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- 230000002745 absorbent Effects 0.000 abstract 1
- 239000002250 absorbent Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 235000008216 herbs Nutrition 0.000 description 6
- ZYURHZPYMFLWSH-UHFFFAOYSA-N octacosane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC ZYURHZPYMFLWSH-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000010828 elution Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- ZPNXTAJKEFNJMW-UHFFFAOYSA-N communin A Natural products C=1C(O)=CC=2OC(C=3C=CC=CC=3)CC(=O)C=2C=1C=CC1=CC=CC=C1 ZPNXTAJKEFNJMW-UHFFFAOYSA-N 0.000 description 4
- 150000002576 ketones Chemical class 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 241000195877 Polytrichum commune Species 0.000 description 3
- 230000000259 anti-tumor effect Effects 0.000 description 3
- 125000005605 benzo group Chemical group 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 241000411851 herbal medicine Species 0.000 description 3
- -1 ketone compounds Chemical class 0.000 description 3
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 2
- ZPNXTAJKEFNJMW-VIOKTNGOSA-N (2s)-7-hydroxy-2-phenyl-5-[(e)-2-phenylethenyl]-2,3-dihydrochromen-4-one Chemical compound C([C@H](OC=1C=C(C=2)O)C=3C=CC=CC=3)C(=O)C=1C=2\C=C\C1=CC=CC=C1 ZPNXTAJKEFNJMW-VIOKTNGOSA-N 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- CJDAIJHZTKDLTJ-UHFFFAOYSA-N Ohioensin F Natural products Oc1ccc2c(c1)C3Oc4ccccc4C5(O)CC(=O)c6c(O)cc(O)c2c6C35 CJDAIJHZTKDLTJ-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 239000002398 materia medica Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- CNNRPFQICPFDPO-UHFFFAOYSA-N octacosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCO CNNRPFQICPFDPO-UHFFFAOYSA-N 0.000 description 2
- CJDAIJHZTKDLTJ-VABKMULXSA-N ohioensin f Chemical compound C([C@]1(O)C2=CC=CC=C2O2)C(=O)C3=C(O)C=C(O)C4=C3[C@H]1[C@@H]2C1=CC(O)=CC=C41 CJDAIJHZTKDLTJ-VABKMULXSA-N 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 2
- 201000008827 tuberculosis Diseases 0.000 description 2
- RQOCXCFLRBRBCS-UHFFFAOYSA-N (22E)-cholesta-5,7,22-trien-3beta-ol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CCC(C)C)CCC33)C)C3=CC=C21 RQOCXCFLRBRBCS-UHFFFAOYSA-N 0.000 description 1
- CZFMLDUNXATLOW-XKZIYDEJSA-N (5z)-5-[[3-(2-hydroxyethoxymethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical compound C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1COCCO CZFMLDUNXATLOW-XKZIYDEJSA-N 0.000 description 1
- QWUWMCYKGHVNAV-UHFFFAOYSA-N 1,2-dihydrostilbene Chemical group C=1C=CC=CC=1CCC1=CC=CC=C1 QWUWMCYKGHVNAV-UHFFFAOYSA-N 0.000 description 1
- 229960002666 1-octacosanol Drugs 0.000 description 1
- HHXYJYBYNZMZKX-PYQRSULMSA-N 22(29)-Hopene Chemical compound C([C@]1(C)[C@H]2CC[C@H]34)CCC(C)(C)[C@@H]1CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@@H]1C(=C)C HHXYJYBYNZMZKX-PYQRSULMSA-N 0.000 description 1
- HHXYJYBYNZMZKX-UHFFFAOYSA-N 3,4:15,16-diepoxy-7-oxo-13(16),14-clerodadien-20,12-olide-(3alpha,4alpha)-form Natural products C12CCC3C4(C)CCCC(C)(C)C4CCC3(C)C1(C)CCC1C2(C)CCC1C(=C)C HHXYJYBYNZMZKX-UHFFFAOYSA-N 0.000 description 1
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 1
- DANYIYRPLHHOCZ-UHFFFAOYSA-N 5,7-dihydroxy-4'-methoxyflavone Chemical compound C1=CC(OC)=CC=C1C1=CC(=O)C2=C(O)C=C(O)C=C2O1 DANYIYRPLHHOCZ-UHFFFAOYSA-N 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000195940 Bryophyta Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241001478240 Coccus Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- LKDRXBCSQODPBY-JDJSBBGDSA-N D-allulose Chemical compound OCC1(O)OC[C@@H](O)[C@@H](O)[C@H]1O LKDRXBCSQODPBY-JDJSBBGDSA-N 0.000 description 1
- DNVPQKQSNYMLRS-NXVQYWJNSA-N Ergosterol Natural products CC(C)[C@@H](C)C=C[C@H](C)[C@H]1CC[C@H]2C3=CC=C4C[C@@H](O)CC[C@]4(C)[C@@H]3CC[C@]12C DNVPQKQSNYMLRS-NXVQYWJNSA-N 0.000 description 1
- 208000034507 Haematemesis Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- ASXHBGJHAMJACK-UHFFFAOYSA-N OOC1(CC=C(C(=O)O)C=C1)OC Chemical compound OOC1(CC=C(C(=O)O)C=C1)OC ASXHBGJHAMJACK-UHFFFAOYSA-N 0.000 description 1
- 240000007817 Olea europaea Species 0.000 description 1
- 241000195883 Polytrichales Species 0.000 description 1
- 241001310017 Polytrichum pallidisetum Species 0.000 description 1
- 208000012287 Prolapse Diseases 0.000 description 1
- ZONYXWQDUYMKFB-UHFFFAOYSA-N SJ000286395 Natural products O1C2=CC=CC=C2C(=O)CC1C1=CC=CC=C1 ZONYXWQDUYMKFB-UHFFFAOYSA-N 0.000 description 1
- 241000191940 Staphylococcus Species 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- HZYXFRGVBOPPNZ-UHFFFAOYSA-N UNPD88870 Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)=CCC(CC)C(C)C)C1(C)CC2 HZYXFRGVBOPPNZ-UHFFFAOYSA-N 0.000 description 1
- 206010046788 Uterine haemorrhage Diseases 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 206010051373 Wound haemorrhage Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- RZJRJXONCZWCBN-UHFFFAOYSA-N alpha-octadecene Natural products CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- OTAFHZMPRISVEM-UHFFFAOYSA-N chromone Chemical compound C1=CC=C2C(=O)C=COC2=C1 OTAFHZMPRISVEM-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- DNVPQKQSNYMLRS-SOWFXMKYSA-N ergosterol Chemical compound C1[C@@H](O)CC[C@]2(C)[C@H](CC[C@]3([C@H]([C@H](C)/C=C/[C@@H](C)C(C)C)CC[C@H]33)C)C3=CC=C21 DNVPQKQSNYMLRS-SOWFXMKYSA-N 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229930003949 flavanone Natural products 0.000 description 1
- 150000002208 flavanones Chemical class 0.000 description 1
- 235000011981 flavanones Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002475 indoles Chemical class 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 208000003747 lymphoid leukemia Diseases 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 206010029410 night sweats Diseases 0.000 description 1
- 230000036565 night sweats Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229940038384 octadecane Drugs 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 150000003431 steroids Chemical class 0.000 description 1
- HCXVJBMSMIARIN-PHZDYDNGSA-N stigmasterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)/C=C/[C@@H](CC)C(C)C)[C@@]1(C)CC2 HCXVJBMSMIARIN-PHZDYDNGSA-N 0.000 description 1
- 229940032091 stigmasterol Drugs 0.000 description 1
- BFDNMXAIBMJLBB-UHFFFAOYSA-N stigmasterol Natural products CCC(C=CC(C)C1CCCC2C3CC=C4CC(O)CCC4(C)C3CCC12C)C(C)C BFDNMXAIBMJLBB-UHFFFAOYSA-N 0.000 description 1
- 235000016831 stigmasterol Nutrition 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 230000008736 traumatic injury Effects 0.000 description 1
- 210000004291 uterus Anatomy 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/10—Bryophyta (mosses)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Chemical & Material Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Biotechnology (AREA)
- Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Epidemiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Alternative & Traditional Medicine (AREA)
- Mycology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a kind of methods of general flavone in ultrasonic wave assisted extraction common polytrichum herb, are specifically implemented according to the following steps：Step 1, common polytrichum herb cleaned, dry, obtain common polytrichum herb coarse powder after crushing；Step 2, common polytrichum herb coarse powder is extracted using ultrasonic wave secondary organic solvent, obtains common polytrichum herb extract；Step 3, common polytrichum herb extract is handled using disodium phosphate soln, obtains common polytrichum herb general flavone crude extract；Step 4, common polytrichum herb general flavone crude extract is isolated and purified using macroporous absorbent resin, obtains common polytrichum herb general flavone.Extracting method of the present invention can in short-term, in high efficiency extraction common polytrichum herb general flavone, and easy to operate, resulting product quality is good, and content is high.
Description
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, and in particular to general flavone in a kind of ultrasonic wave assisted extraction common polytrichum herb
Method.
Background technology
Common polytrichum herb (Polytrichum commune L.ex Hedw.) belong to moss guiding principle, pigeon-wheat subclass, Polytrichales,
Pigeon-wheat section, Polytrichum plant are a kind of common medicinal mosses, are used as medicine first appeared in the Song Dynasty《Jia Yu after-teeming book on Chinese herbal medicine》, book
In contained " native horse " be pigeon-wheat, can lose that heat scattered poison, relieving bowels, to control bone hot.Written by Ming Dynasty's Li Shizhen《Compendium of Materia Medica》
In also include pigeon-wheat be " native horse-hair ", all herbal medicine is described as to its pharmacological property, it is sweet in flavor, it is cool in nature.Energy nourishing Yin and clearing heat, cool blood are stopped
Sweat, smell is sweet to be dredged, nontoxic.Qing Dynasty Wu its dredge writing《The Illustrated Book on Plants》In also have described below, " native horse to pigeon-wheat
Hair on the neck, good book on Chinese herbal medicine of helping begin to record.Wall clothing is born in person on cob wall head, and performance loses heat toxin ".Modern medicine scholar couple《Compendium of Materia Medica》Again
What deciphering was completed later《This grass Gang Mu ﹒ check and punctuate sheets》Described in pigeon-wheat cure mainly heat long do not move back, tuberculosis cough, night sweat, haematemesis, just
Blood, uterine bleeding, traumatic injury, the prolapse of uterus, knife wound bleeding.And to high husband's kirschner coccus, golden staphylococcus, pneumococcus, tuberculosis
Bacillus is resistant, has certain inhibiting effect to cancers such as lymphocytic leukemias.
Began to be reported in media successively from 1993 to the research of pigeon-wheat plant chemical composition, Zheng Guo-qiang's grinds
Study carefully group the multiform for picking up from Maryland is intended showing in pigeon-wheat Polytrichum ohioense Ren＆Card it is antitumor
Active chloroform is detached at grouping, is identified, 5 benzo coeroxene ketone chemical combination with novel structure skeleton are obtained
Object.Next year, the research group divide the chemical composition for deforming pigeon-wheat Polytrichum pallidisetum Funck
From, identification, get back 3 with novel structure skeleton benzo coeroxene ketone compounds and 2 structure novels benzene second
Olefine aldehydr base and bibenzyl derivative.2008, Chen Sheng et al. follow-up stories were from picking up from Guiyang City, Guizhou Province Qing Yan, high hillside fields area
It detached in common polytrichum herb Polytrichum Commune L.ex Hedw, identify 13 kinds of compounds：Diploptene, octacosane
Sour methyl esters, octacosane acid butyl ester, octocosoic acid pentyl ester, cupreol, octocosoic acid octadecane alcohol ester, 20 acid 19
Alkanol ester, positive inearnatyl alcohol, n-octacosanol, stigmasterol, three octacosane acid glycerides, 5,7- dihydroxy -4'- methoxies
Base -3'- acetyl group flavones, 3- oxo -30- carboxymethyl olive -12,18- diene -28- carboxylic acids., Fu Peng in 2009 et al. from
Divide in the common polytrichum herb Polytrichum Commune L.ex Hedw on Zhejiang Province Longquan City Fengyangshan Nature Reserve crop field level ground
From obtaining 11 kinds of compounds, respectively Communin A, Communin B, Ohioensin F, 6- acetyldihydros indoles, 4-
Hydroxyl-O-Anisic Acid, 5- hydroxyl -7- methoxyl groups chromone, β-D- furans psicose, cupreol, 7 Alpha-hydroxy paddy steroids
Alcohol, 11 times of condensates of ergosterol and ethylene glycol, P-hydroxybenzoic acid, 5,7- dihydroxy -6- methoxy coumarin -7-O- β -
D-Glucose glycosides, sucrose, α-D- furans psicoses.Wherein Communin A and Communin B, which are two, has novel structure
The styryl and flavanone kind composition of skeleton, Ohioensin F are benzo coeroxene ketone derivatives.
In addition, some researches show that anti-tumor active ingredient is mainly Flavonoid substances in common polytrichum herb, but to sum up may be used
Know, at present to the research of active constituent in common polytrichum herb also in the elementary step, and yet there are no related common polytrichum herb
The relevant report of middle flavonoids extraction process of active component, therefore, it is necessary to work out general flavone in a kind of common polytrichum herb
Extracting method, to make up this vacancy, the development for antitumor field provides support.
Invention content
The present invention provides a kind of methods of general flavone in ultrasonic wave assisted extraction common polytrichum herb, solve in the prior art
There is presently no in common polytrichum herb the problem of total flavone extracting method.
The present invention provides a kind of methods of general flavone in ultrasonic wave assisted extraction common polytrichum herb, specifically according to the following steps
Implement：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, by common polytrichum herb coarse powder and mixed organic solvents according to 1g：The ratio of 40~50mL is uniformly mixed, and is obtained
Mixture；It by mixture ultrasonic extraction, obtains being ultrasonically treated mixture, mixture filtering, concentration will be ultrasonically treated, obtain great Jin
Rodendron extract；
Wherein, the ethyl alcohol that the mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio
It mixes；
Step 3, it is added into the common polytrichum herb extract that step 2 obtains and is equivalent to common polytrichum herb extract weight 5~10
Deionized water again, it is 10~11 then to add alkali, regulation system pH value thereto, and stirring to common polytrichum herb extracts at 60 DEG C
Object is completely dissolved, and obtains common polytrichum herb solution of extract；
The disodium hydrogen phosphate for being equivalent to common polytrichum herb extract weight 10% is added into common polytrichum herb solution of extract
Solution, and a concentration of the 15% of disodium phosphate soln open stirring, until sediment is not further added by system, then mistake
Filter, obtains filtrate A；
Into filtrate A, addition and ethanol solution isometric filtrate A, filter, obtain liquor B, liquor B is subtracted after mixing
Pressure concentration, obtains common polytrichum herb general flavone crude extract；
Step 4, the common polytrichum herb general flavone crude extract obtained in step 3 is crossed into large pore resin absorption column, and by big golden hair
Moss general flavone crude extract and dried resin are according to being 1：30 weight ratio loading, for loading flow control in 2-3BV/h, absorption is complete
Afterwards, it is washed with deionized water and takes off colourless to eluent, then eluted with the ethyl acetate of 50BV, coutroi velocity 2-3BV/h collects second
Acetoacetic ester eluent, and by ethyl acetate eluent concentration, dry to get to general flavone in the common polytrichum herb.
Preferably, ultrasonic power is 120~180W in the step 2.
Preferably, ultrasonic extraction conditions are 45~60min of ultrasonic extraction at 70 DEG C in the step 2.
Preferably, the alkali being added in the step 3 is sodium hydroxide or potassium hydroxide.
Preferably, mixing speed is 500r/min in the step 3.
Preferably, the large pore resin absorption column is using deionized water as solvent wet method dress post, and fills the good macroporous absorption of column
Resin column blade diameter length ratio is 1：15.
Preferably, model M301, the NKA-9 type of big pore adsorption resin in the large pore resin absorption column, AB-8,
One kind in DM130 types.
Compared with prior art, the beneficial effects of the present invention are：
1) present invention is not only substantially reduced and is carried using the general flavone in ultrasonic wave secondary organic solvent extraction common polytrichum herb
The time is taken, the extracted amount of the general flavone in common polytrichum herb is also improved, improves yield.
2) present invention detaches not easy-to-use large pore resin absorption column in common polytrichum herb extract using disodium phosphate soln
Polysaccharose substance and alcohols material precipitation be conducive to total to alleviate the burden of follow-up large pore resin absorption column separation
The purifying of flavones.
3) extracting method of the present invention can in short-term, efficiently extract the general flavone in common polytrichum herb, and easy to operate, gained
Superior product quality, content is high, at low cost, can be widely used to promote.
Specific implementation mode
In order to enable those skilled in the art to more fully understand, technical scheme of the present invention is practiced, with reference to specific
Embodiment is next, and the invention will be further described, but illustrated embodiment is not as a limitation of the invention.
Experimental method described in following each embodiments is unless otherwise specified conventional method；Material therefor is such as without special
Illustrate, can be commercially available on the market.
Embodiment 1
The method of general flavone, is specifically implemented according to the following steps in a kind of ultrasonic wave assisted extraction common polytrichum herb：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, common polytrichum herb coarse powder 100g is weighed, is added it in the mixed organic solvents of 5L, after mixing
To mixture；Ultrasonic extraction 45min under conditions of being 180W in 70 DEG C, ultrasonic power by mixture, obtains being ultrasonically treated mixing
Object；It will be ultrasonically treated mixture filtering, concentration, obtain 18.2g common polytrichum herb extracts；
Wherein, the ethyl alcohol that mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio mixing
It forms；
Step 3,90ml deionized waters are added into the 18.2g common polytrichum herb extracts that step 2 obtains, then add thereto
Sodium hydroxide, regulation system pH value are 10~11, stir at 60 DEG C and are completely dissolved to common polytrichum herb extract, obtain great Jin
Rodendron solution of extract；
The disodium phosphate soln of 18.2g a concentration of 15% is added into common polytrichum herb solution of extract, opens stirring,
Under the mixing speed of 500r/min then stirring is filtered until sediment is not further added by system, is collected filtrate and is depressurized
Concentration, obtains filtrate A；
Into filtrate A, addition and ethanol solution isometric filtrate A, filter, obtain liquor B, liquor B is subtracted after mixing
Pressure concentration, obtains 8.326g common polytrichum herb general flavone crude extracts；
Step 4, the 8.326g common polytrichum herb general flavone crude extracts obtained in step 3 are crossed into large pore resin absorption column, and will
The dried resin of common polytrichum herb general flavone crude extract and model DM130 are according to being 1：30 weight ratio loading, loading flow control
In 2BV/h, after absorption completely, be washed with deionized water take off it is colourless to eluent, then with the ethyl acetate elution of 50BV, coutroi velocity
For 2BV/h, ethyl acetate eluent is collected, and by ethyl acetate eluent concentration, dry to get in 2.081g common polytrichum herbs
General flavone.
Embodiment 2
The method of general flavone, is specifically implemented according to the following steps in a kind of ultrasonic wave assisted extraction common polytrichum herb：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, common polytrichum herb coarse powder 100g is weighed, is added it in the mixed organic solvents of 4L, after mixing
To mixture；Ultrasonic extraction 60min under conditions of being 120W in 70 DEG C, ultrasonic power by mixture, obtains being ultrasonically treated mixing
Object；It will be ultrasonically treated mixture filtering, concentration, obtain 20.10g common polytrichum herb extracts；
Wherein, the ethyl alcohol that mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio mixing
It forms；
Step 3,200ml deionized waters are added into the 20.10g common polytrichum herb extracts that step 2 obtains, then thereto
It is 10~11 to add sodium hydroxide, regulation system pH value, stirs at 60 DEG C and is completely dissolved to common polytrichum herb extract, is obtained big
Pigeon-wheat solution of extract；
The disodium phosphate soln of 20.10g a concentration of 15% is added into common polytrichum herb solution of extract, unlatching is stirred
It mixes, stirs until sediment is not further added by system under the mixing speed of 500r/min, then filter, collect filtrate and simultaneously subtract
Pressure concentration, obtains filtrate A；
Into filtrate A, addition and ethanol solution isometric filtrate A, filter, obtain liquor B, liquor B is subtracted after mixing
Pressure concentration, obtains 9.536g common polytrichum herb general flavone crude extracts；
Step 4, the 9.536g common polytrichum herb general flavone crude extracts obtained in step 3 are crossed into large pore resin absorption column, and will
The dried resin of common polytrichum herb general flavone crude extract and model M301 are according to being 1：30 weight ratio loading, loading flow control exist
2BV/h after absorption completely, is washed with deionized water and takes off colourless to eluent, then with the elution of the ethyl acetate of 50BV, coutroi velocity is
2BV/h, collects ethyl acetate eluent, and by ethyl acetate eluent concentration, dry to get to total in 2.025g common polytrichum herbs
Flavones.
Embodiment 3
The method of general flavone, is specifically implemented according to the following steps in a kind of ultrasonic wave assisted extraction common polytrichum herb：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, common polytrichum herb coarse powder 100g is weighed, is added it in the mixed organic solvents of 5L, after mixing
To mixture；Ultrasonic extraction 50min under conditions of being 150W in 70 DEG C, ultrasonic power by mixture, obtains being ultrasonically treated mixing
Object；It will be ultrasonically treated mixture filtering, concentration, obtain 19.3g common polytrichum herb extracts；
Wherein, the ethyl alcohol that mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio mixing
It forms；
Step 3,100ml deionized waters are added into the 19.3g common polytrichum herb extracts that step 2 obtains, then thereto
It is 10~11 to add potassium hydroxide, regulation system pH value, stirs at 60 DEG C and is completely dissolved to common polytrichum herb extract, is obtained big
Pigeon-wheat solution of extract；
The disodium phosphate soln of 19.3g a concentration of 15% is added into common polytrichum herb solution of extract, opens stirring,
Under the mixing speed of 500r/min then stirring is filtered until sediment is not further added by system, is collected filtrate and is depressurized
Concentration, obtains filtrate A；
Into filtrate A, addition and ethanol solution isometric filtrate A, filter, obtain liquor B, liquor B is subtracted after mixing
Pressure concentration, obtains 8.892g common polytrichum herb general flavone crude extracts；
Step 4, the 8.892g common polytrichum herb general flavone crude extracts obtained in step 3 are crossed into large pore resin absorption column, and will
The dried resin of common polytrichum herb general flavone crude extract and model AB-8 are according to being 1：30 weight ratio loading, loading flow control exist
3BV/h after absorption completely, is washed with deionized water and takes off colourless to eluent, then with the elution of the ethyl acetate of 50BV, coutroi velocity is
3BV/h, collects ethyl acetate eluent, and by ethyl acetate eluent concentration, dry to get to total in 2.012g common polytrichum herbs
Flavones.
Embodiment 4
The method of general flavone, is specifically implemented according to the following steps in a kind of ultrasonic wave assisted extraction common polytrichum herb：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, common polytrichum herb coarse powder 100g is weighed, is added it in the mixed organic solvents of 5L, after mixing
To mixture；Ultrasonic extraction 55min under conditions of being 160W in 70 DEG C, ultrasonic power by mixture, obtains being ultrasonically treated mixing
Object；It will be ultrasonically treated mixture filtering, concentration, obtain 19.6g common polytrichum herb extracts；
Wherein, the ethyl alcohol that mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio mixing
It forms；
Step 3,100ml deionized waters are added into the 19.6g common polytrichum herb extracts that step 2 obtains, then thereto
It is 10~11 to add potassium hydroxide, regulation system pH value, stirs at 60 DEG C and is completely dissolved to common polytrichum herb extract, is obtained big
Pigeon-wheat solution of extract；
The disodium phosphate soln of 19.6g a concentration of 15% is added into common polytrichum herb solution of extract, opens stirring,
Under the mixing speed of 500r/min then stirring is filtered until sediment is not further added by system, is collected filtrate and is depressurized
Concentration, obtains filtrate A；
Into filtrate A, addition and ethanol solution isometric filtrate A, filter, obtain liquor B, liquor B is subtracted after mixing
Pressure concentration, obtains 9.218g common polytrichum herb general flavone crude extracts；
Step 4, the 9.218g common polytrichum herb general flavone crude extracts obtained in step 3 are crossed into large pore resin absorption column, and will
The dried resin of common polytrichum herb general flavone crude extract and model NKA-9 types is according to being 1：30 weight ratio loading, loading flow velocity control
System is in 3BV/h, after absorption completely, is washed with deionized water and takes off colourless to eluent, then eluted with the ethyl acetate of 50BV, control is flowed
Speed is 3BV/h, collects ethyl acetate eluent, and by ethyl acetate eluent concentration, dry to get to 2.015g common polytrichum herbs
Middle general flavone.
It should be noted that large pore resin absorption column using deionized water as solvent wet method dress post, fills the good macroporous absorption of column
Resin column blade diameter length ratio is 1：15.
In order to illustrate effect, the present invention is also provided with comparative example, specific as follows：
Comparative example 1
The method of general flavone, is specifically implemented according to the following steps in a kind of ultrasonic wave assisted extraction common polytrichum herb：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, common polytrichum herb coarse powder 100g is weighed, is added it in the mixed organic solvents of 5L, after mixing
To mixture；Ultrasonic extraction 45min under conditions of being 180W in 70 DEG C, ultrasonic power by mixture, obtains being ultrasonically treated mixing
Object；It will be ultrasonically treated mixture filtering, concentration, obtain 18.2g common polytrichum herb extracts；
Wherein, the ethyl alcohol that mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio mixing
It forms；
Step 3, the 18.2g common polytrichum herb general flavone crude extracts obtained in step 2 are crossed into large pore resin absorption column, and will be big
The dried resin of pigeon-wheat general flavone crude extract and model DM130 are according to being 1：30 weight ratio loading, loading flow control exist
2BV/h after absorption completely, is washed with deionized water and takes off colourless to eluent, then with the elution of the ethyl acetate of 50BV, coutroi velocity is
2BV/h, collects ethyl acetate eluent, and by ethyl acetate eluent concentration, dry to get to total in 2.132g common polytrichum herbs
Flavones.
Comparative example 2
The method of general flavone, is specifically implemented according to the following steps in a kind of ultrasonic wave assisted extraction common polytrichum herb：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, common polytrichum herb coarse powder 100g is weighed, is added it in the mixed organic solvents of 5L, 2d is impregnated, has impregnated
Filtering, concentration, obtain 15.6g common polytrichum herb extracts after finishing；
Wherein, the ethyl alcohol that mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio mixing
It forms；
Step 3,80ml deionized waters are added into the 15.6g common polytrichum herb extracts that step 2 obtains, then add thereto
Sodium hydroxide, regulation system pH value are 10~11, stir at 60 DEG C and are completely dissolved to common polytrichum herb extract, obtain great Jin
Rodendron solution of extract；
The disodium phosphate soln of 15.6g a concentration of 15% is added into common polytrichum herb solution of extract, opens stirring,
Under the mixing speed of 500r/min then stirring is filtered until sediment is not further added by system, is collected filtrate and is depressurized
Concentration, obtains filtrate A；
Into filtrate A, addition and ethanol solution isometric filtrate A, filter, obtain liquor B, liquor B is subtracted after mixing
Pressure concentration, obtains 7.658g common polytrichum herb general flavone crude extracts；
Step 4, the 7.658g common polytrichum herb general flavone crude extracts obtained in step 3 are crossed into large pore resin absorption column, and will
The dried resin of common polytrichum herb general flavone crude extract and model DM130 are according to being 1：30 weight ratio loading, loading flow control
In 2BV/h, after absorption completely, be washed with deionized water take off it is colourless to eluent, then with the ethyl acetate elution of 50BV, coutroi velocity
For 2BV/h, ethyl acetate eluent is collected, and by ethyl acetate eluent concentration, dry to get in 1.916g common polytrichum herbs
General flavone.
Examples 1 to 4 and comparative example 1~2 have extracted common polytrichum herb general flavone, using spectrophotometry to embodiment
1~4 and comparative example 1~2 in the performance of general flavone that extracts tested, concrete outcome is shown in Table 1.
1 general flavone testing result of table
| Project | General flavone acquisition amount (g/100g) | General flavone recovery rate (%) | General flavone content (%) |
| Embodiment 1 | 2.081 | 2.08 | 97.87 |
| Embodiment 2 | 2.025 | 2.03 | 96.92 |
| Embodiment 3 | 2.012 | 2.01 | 97.38 |
| Embodiment 4 | 2.015 | 2.02 | 97.26 |
| Comparative example 1 | 2.132 | 2.13 | 83.92 |
| Comparative example 2 | 1.916 | 1.92 | 96.85 |
Note：General flavone recovery rate (%) calculation formula is as follows：The quality of general flavone quality (g)/common polytrichum herb.
As it can be seen from table 1 after method using the present invention extracts general flavone in common polytrichum herb, total Huang of acquisition
Ketone amount is more, can extract to obtain the general flavone of 2g or so in the average common polytrichum herb per 100g, and obtains total yellow in final product
Ketone content is also higher, reaches 96.9% or more, illustrates that the method for the present invention has extraction effect well to general flavone in common polytrichum herb
Rate.
Common polytrichum herb extract does not pass through disodium phosphate soln and handles in documents 1, therefore certain wherein contained
It is a little to be difficult to be maintained in product using the substance of large pore resin absorption column separation, influence the content of general flavone in product.
Without using ultrasonic wave assisted extraction in documents 2, so active ingredient extraction is insufficient in middle common polytrichum herb,
The quality of finally obtained general flavone is low compared with embodiment.
In summary, extracting method of the present invention can in short-term, efficiently extract the general flavone in common polytrichum herb, and operate letter
Just, resulting product quality is good, and content is high, at low cost, can be widely used to promote.
It should be noted that involved in description of the invention when numberical range, it is thus understood that two of each numberical range
Any one numerical value can be selected between endpoint and two endpoints, since the step method of use is identical as Examples 1 to 4,
It repeats in order to prevent, description of the invention preferred embodiment, once a person skilled in the art knows basic wounds
The property made concept, then additional changes and modifications may be made to these embodiments.So the following claims are intended to be interpreted as includes
Preferred embodiment and all change and modification for falling into the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (7)
1. a kind of method of general flavone in ultrasonic wave assisted extraction common polytrichum herb, which is characterized in that specifically real according to the following steps
It applies：
Step 1, common polytrichum herb cleaned, dried, smashing it through 40 mesh sieve, obtaining common polytrichum herb coarse powder；
Step 2, by common polytrichum herb coarse powder and mixed organic solvents according to 1g：The ratio of 40~50mL is uniformly mixed, and is mixed
Object；It by mixture ultrasonic extraction, obtains being ultrasonically treated mixture, mixture filtering, concentration will be ultrasonically treated, obtain common polytrichum herb
Extract；
Wherein, the ethyl alcohol that the mixed organic solvents are 70% by volumetric concentration is with ethyl acetate according to 4：6 volume ratio mixing
It forms；
Step 3, it is added into the common polytrichum herb extract that step 2 obtains and is equivalent to 5~10 times of common polytrichum herb extract weight
Deionized water, it is 10~11 then to add alkali, regulation system pH value thereto, is stirred at 60 DEG C complete to common polytrichum herb extract
Fully dissolved obtains common polytrichum herb solution of extract；
The disodium phosphate soln for being equivalent to common polytrichum herb extract weight 10% is added into common polytrichum herb solution of extract,
And a concentration of the 15% of disodium phosphate soln, stirring is opened, until sediment is not further added by system, then filters, obtains
To filtrate A；
Into filtrate A, addition and ethanol solution isometric filtrate A, filter, obtain liquor B, liquor B is depressurized dense after mixing
Contracting, obtains common polytrichum herb general flavone crude extract；
Step 4, the common polytrichum herb general flavone crude extract obtained in step 3 is crossed into large pore resin absorption column, and common polytrichum herb is total
Flavones crude extract and dried resin are according to being 1：30 weight ratio loading, loading flow control are used after 2-3BV/h, absorption completely
Deionized water is eluted to that eluent is colourless, then is eluted with the ethyl acetate of 50BV, and coutroi velocity 2-3BV/h collects acetic acid second
Ester eluent, and by ethyl acetate eluent concentration, dry to get to general flavone in the common polytrichum herb.
2. the method for general flavone in ultrasonic wave assisted extraction common polytrichum herb according to claim 1, which is characterized in that described
Ultrasonic power is 120~180W in step 2.
3. the method for general flavone in ultrasonic wave assisted extraction common polytrichum herb according to claim 2, which is characterized in that described
Ultrasonic extraction conditions are 45~60min of ultrasonic extraction at 70 DEG C in step 2.
4. the method for general flavone in ultrasonic wave assisted extraction common polytrichum herb according to claim 1, which is characterized in that described
The alkali being added in step 3 is sodium hydroxide or potassium hydroxide.
5. the method for general flavone in ultrasonic wave assisted extraction common polytrichum herb according to claim 1, which is characterized in that described
Mixing speed is 500r/min in step 3.
6. the method for general flavone in ultrasonic wave assisted extraction common polytrichum herb according to claim 1, which is characterized in that described
Large pore resin absorption column is using deionized water as solvent wet method dress post, and it is 1 to fill the good large pore resin absorption column blade diameter length ratio of column：15.
7. the method for general flavone in ultrasonic wave assisted extraction common polytrichum herb according to claim 6, which is characterized in that described
One kind in large pore resin absorption column in model M301, the NKA-9 type of big pore adsorption resin, AB-8, DM130 type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810779583.0A CN108524554B (en) | 2018-07-16 | 2018-07-16 | Method for extracting total flavonoids from moss of blossoms by ultrasonic wave assistance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810779583.0A CN108524554B (en) | 2018-07-16 | 2018-07-16 | Method for extracting total flavonoids from moss of blossoms by ultrasonic wave assistance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108524554A true CN108524554A (en) | 2018-09-14 |
| CN108524554B CN108524554B (en) | 2021-04-16 |
Family
ID=63488193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810779583.0A Active CN108524554B (en) | 2018-07-16 | 2018-07-16 | Method for extracting total flavonoids from moss of blossoms by ultrasonic wave assistance |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108524554B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110917225A (en) * | 2019-10-29 | 2020-03-27 | 台州学院 | Preparation method of antioxidant melastoma dodecandrum lour extract |
| CN116444473A (en) * | 2022-11-16 | 2023-07-18 | 河北中医学院 | Novel compound, preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105267275A (en) * | 2015-10-15 | 2016-01-27 | 南阳师范学院 | Extraction method for flavones in chrysanthemum |
-
2018
- 2018-07-16 CN CN201810779583.0A patent/CN108524554B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105267275A (en) * | 2015-10-15 | 2016-01-27 | 南阳师范学院 | Extraction method for flavones in chrysanthemum |
Non-Patent Citations (2)
| Title |
|---|
| 成晓霞: "大金发藓抗癌活性组分分析及其对白血病细胞杀伤机制研究", 《CNKI博士学位论文全文库》 * |
| 陈胜等: "大金发藓的化学成分研究 ", 《贵州化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110917225A (en) * | 2019-10-29 | 2020-03-27 | 台州学院 | Preparation method of antioxidant melastoma dodecandrum lour extract |
| CN116444473A (en) * | 2022-11-16 | 2023-07-18 | 河北中医学院 | Novel compound, preparation method and application thereof |
| CN116444473B (en) * | 2022-11-16 | 2023-09-22 | 河北中医学院 | Compound and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108524554B (en) | 2021-04-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101284022B (en) | Complexation extraction method of plant polyphenols substances | |
| CN108619202A (en) | The method that a kind of extraction of eutectic solvent, macroporous absorbent resin isolate and purify burdock leaf flavonoids | |
| CN102924240B (en) | Method for extracting total magnolol according to alcoholic-alkaline method | |
| CN109053665A (en) | The method and application of dihydromyricetin are extracted in vine tea | |
| CN109157454A (en) | A kind of Camellia combined extracts and its preparation and the application in cosmetics | |
| CN108524554A (en) | A kind of method of general flavone in ultrasonic wave assisted extraction common polytrichum herb | |
| CN105132172A (en) | Method for preparing orris root flavonoid matter for tobaccos from orris roots | |
| CN101361786B (en) | Total-flavone extraction and purification and its monomer separation method from Lespedaza bedysaroides | |
| CN102031116A (en) | New method for preparing rosemary natural antioxidant | |
| CN104523833A (en) | Preparation method of baical skullcap root extract | |
| CN101955479A (en) | Method for extracting orientin from bamboo leaf | |
| CN103830292A (en) | Apocynum flavonoid extract and preparation method thereof | |
| CN103463160A (en) | Preparation method of high-content total flavones of chrysanthemum | |
| CN101757111A (en) | Preparation method of Chinese magnoliavine fruit total lignan | |
| CN108069930A (en) | A kind of method of combined extracting galangal volatile oil and Galangin from galangal | |
| CN106581108A (en) | Method for removing residual pesticide propamocarb in ginseng extractive | |
| CN109453234A (en) | Root bark of white mulberry product and preparation method thereof | |
| CN103183658A (en) | Method for extracting effective component of coleus forskohlii | |
| CN112480053B (en) | Method for extracting and separating baicalin and baicalein | |
| CN107982455B (en) | Natural composite antioxidant | |
| CN107510629A (en) | Extraction process, belamcanda chinensis extract and its application of belamcanda chinensis extract and moisturizing cream | |
| CN109419981A (en) | A kind of preparation method of Sanguis Draxonis flavoniod | |
| CN102836280A (en) | Folium Lycii total flavone extract and preparation method thereof | |
| CN108969580B (en) | Preparation method and application of blue cloth total tannin | |
| CN111329888A (en) | Pseudo-ginseng flower tablet and production and preparation process thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |