CN107951921A - A kind of method that flavones is extracted in the powder from eucommia Bark male flower - Google Patents
A kind of method that flavones is extracted in the powder from eucommia Bark male flower Download PDFInfo
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- CN107951921A CN107951921A CN201810028802.1A CN201810028802A CN107951921A CN 107951921 A CN107951921 A CN 107951921A CN 201810028802 A CN201810028802 A CN 201810028802A CN 107951921 A CN107951921 A CN 107951921A
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- flavones
- male flower
- pollen
- eucommia bark
- bark male
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- 229930003944 flavone Natural products 0.000 title claims abstract description 92
- 235000011949 flavones Nutrition 0.000 title claims abstract description 92
- 150000002213 flavones Chemical class 0.000 title claims abstract description 82
- 241000208688 Eucommia Species 0.000 title claims abstract description 70
- 239000000843 powder Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000605 extraction Methods 0.000 claims abstract description 36
- 239000012141 concentrate Substances 0.000 claims abstract description 26
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract description 3
- 235000013305 food Nutrition 0.000 claims abstract description 3
- 230000036541 health Effects 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 238000012545 processing Methods 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 28
- 239000006228 supernatant Substances 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 23
- 238000000874 microwave-assisted extraction Methods 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 20
- 238000003760 magnetic stirring Methods 0.000 claims description 16
- 238000005057 refrigeration Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000005292 vacuum distillation Methods 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 23
- 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 abstract description 10
- 150000002212 flavone derivatives Chemical class 0.000 abstract description 10
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 abstract description 10
- 238000013019 agitation Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000284 extract Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 230000006837 decompression Effects 0.000 description 5
- 238000002137 ultrasound extraction Methods 0.000 description 4
- 229930003935 flavonoid Natural products 0.000 description 3
- 150000002215 flavonoids Chemical class 0.000 description 3
- 235000017173 flavonoids Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- 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
- 241000196324 Embryophyta Species 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000002255 enzymatic effect Effects 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 1
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 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
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000208689 Eucommia ulmoides Species 0.000 description 1
- 241000208686 Eucommiaceae Species 0.000 description 1
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
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- 230000003321 amplification Effects 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000008280 blood Substances 0.000 description 1
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- 210000000170 cell membrane Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 1
- 235000001368 chlorogenic acid Nutrition 0.000 description 1
- 229940074393 chlorogenic acid Drugs 0.000 description 1
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 1
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 235000012041 food component Nutrition 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/46—Eucommiaceae (Eucommia family), e.g. hardy rubber tree
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- 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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Botany (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Biotechnology (AREA)
- Alternative & Traditional Medicine (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Medical Informatics (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention provides a kind of method that flavones is extracted in powder from eucommia Bark male flower, using drying, the eucommia Bark male flower powder to sieve as raw material, heating broken wall treatment is carried out to pollen using tubular heater, using ethanol water as solvent, after pollen and solvent premix, use gradient power microwave method and at the same time with magnetic agitation assisted extraction flavones, extracting solution obtains general flavone extraction concentrate through standing, centrifuging, being concentrated by evaporation.Present invention process has the characteristics that high extraction, quick time saving, inexpensive, environmentally protective, and flavones yield and extraction time be better than soak extraction and ultrasonic extracting method, suitable for the scale extraction of eucommia Bark male flower powder flavones product.Prepared flavones is widely used, can be applied to the fields such as health care, food, industry.
Description
Technical field
The present invention relates to the extracting method of effective component of chinese medicine, more particularly to one kind to use microwave technology from eucommia Bark male flower powder
The method of middle extraction flavones.
Background technology
The bark of eucommia（Scientific name Eucommia ulmoides Oliver）, it is Eucommiaceae plant, is rare traditional Chinese medicine, and country
Second class protection plant, has very high medicinal and edible value.Eucommia pollen is the male sex-cell of the bark of eucommia（Sperm）, it is
There is the part of highest nutritive value in each position of the bark of eucommia.Eucommia Bark male flower powder contain vitamin C, vitamin E, flavones, chlorogenic acid,
The multiple nutritional components such as selenium, wherein flavones are main component, and content is up to 3.36%, far above pollen general flavone content in plant
Average value 2.65%.Flavones is a kind of important bioactive substance, it has anti-aging, suppresses cancer, suppresses thrombus shape
Into, improve blood lipid level and other effects.
At present since the presence of eucommia Bark male flower flour cell wall, flavones can not be effectively extracted utilization.Eucommia Bark male flower powder
Cell membrane is divided into inner and outer wall, and outer wall is mainly made of cellulose, sporopollenin, and inner wall is mainly by cellulose and pectin element group
Into, it is firm and there is acid-fast alkali-proof, anti-high pressure and anticorrosive, due to the nutrition such as the presence of pollen cell wall, flavones into
Dividing preferably to discharge, so that utilization cannot be fully absorbed, thus constrain the research and development of eucommia Bark male flower powder Related product,
As limiting the major technology bottleneck that it is commercially promoted and applied.Extracting flavonoids method in existing eucommia Bark male flower powder has decocting
Cooking method, enzymatic isolation method, ultrasound assisted extraction method etc..Traditional water decoction cooking method extraction efficiency is relatively low, and long-time, high temperature boiling are easy
The mass degradations such as flavones are caused to inactivate；Enzymatic isolation method is used, though can guarantee that other species activities such as flavones, flavones yield is low,
Only 0.049%, cycle length, and flavones yield is limited by the specificity and dosage of enzyme, is not easy to carry out later stage scale extraction；It is super
The method of sound auxiliary extraction eucommia Bark male flower powder, although general flavone yield is high, about 3.29%, during the technology consumption energy consumption, extraction conditions
Acutely, higher heat and larger noise are produced, and flavones is easily degraded under the high temperature conditions, while this method is limited to carefully
Born of the same parents crush the probe model of instrument, the prospect without large-scale production.Therefore, exploitation extraction efficiency is high, the time is short, extraction conditions
Gently, eucommia Bark male flower powder extracting flavonoids method that is environmentally protective and being easy to industry amplification, has important practical significance and answers
Use prospect.
The content of the invention
The present invention proposes a kind of method that flavones is extracted in powder from eucommia Bark male flower, using tubular heater to eucommia Bark male flower
Powder carries out heating broken wall treatment, using ethanol water as solvent, uses gradient microwave technology and is carried at the same time with magnetic agitation auxiliary
The flavones of eucommia Bark male flower powder is taken, flavones yield can reach 3.34%, be flavones in a kind of efficient, rapid extraction eucommia Bark male flower powder
Method.
Realize the technical scheme is that：A kind of method that flavones is extracted in powder from eucommia Bark male flower, step are as follows：
（1）Fresh eucommia Bark male flower powder is dried to constant weight, sieving at 50 ~ 60 DEG C, obtained eucommia Bark male flower powder is at -20 DEG C
Refrigeration；
（2）By step（1）The eucommia Bark male flower powder of refrigeration, which is placed in tubular heater, carries out heating broken wall treatment；
（3）By step（2）Eucommia Bark male flower powder after broken wall treatment is placed in immersion treatment in ethanol water, obtains pollen ethanol and mixes
Close solution；
（4）By step（3）The pollen alcohol mixed solution of acquisition is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, extraction
0.5 ~ 1 min, obtains pollen extracting liquid；
（5）By step（4）The pollen extracting liquid of acquisition is positioned over 15 ~ 20min of standing in 4 DEG C of refrigerators, is cooled to room temperature；
（6）By step（5）Pollen extracting liquid after standing is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, and extraction 1 ~
2min；
（7）By step（6）Pollen extracting liquid after extraction is placed in 10 ~ 15min of standing in 4 DEG C of refrigerators, is cooled to room temperature；
（8）By step（7）Pollen extracting liquid after cooling is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, and extraction 2 ~
5min；
（9）By step（8）Pollen extracting liquid after extraction stands 2 ~ 5min, cooled to room temperature；
（10）By step（9）Pollen extracting liquid after cooling is placed in a centrifuge, and centrifugation collects supernatant；
（11）By step（10）The supernatant vacuum distillation of collection, obtains flavones concentrate.
The step（1）40 ~ 80 mesh sieves are crossed after middle eucommia Bark male flower powder constant weight.
The step（2）Middle tubular heater is warming up to 80-100 DEG C with the speed of 15 ~ 20 DEG C/min, processing time for 5 ~
10min, nitrogen is passed through in heating process as protection gas.
The step（3）The volumetric concentration of middle ethanol water is 60% ~ 80%, 1g eucommia Bark male flower powder is added to 30 ~
1 ~ 5 min is soaked in 50ml ethanol waters.
The frequency of the Microwave Extraction Apparatus is 915 ~ 2450MHz, power 200-800W, the stirring speed of magnetic stirring apparatus
Spend for 200 ~ 800rpm.
The step（10）The centrifugal speed of middle centrifuge is 8000 ~ 10000rpm, and centrifugation time is 15 ~ 20min.
The step（11）Middle supernatant is evaporated under reduced pressure using Rotary Evaporators, and rotating evaporation temperature is 40 ~ 60 DEG C, vacuum
It is 20 ~ 60min to spend for 0.08 ~ 0.09MPa, time.
Using rutin as standard items, using aluminum nitrate colorimetric determination step（11）General flavone is dense in the flavones concentrate of acquisition
Degree, flavones yield is calculated according to equation below：
Wherein, k is flavones yield；
C is flavones concentrate concentration, unit mg/mL；
V is the flavones volume of the concentrated liquid, unit mL；
M be eucommia Bark male flower powder raw material quality, unit g.
Application of the flavones in health care, food and industry.
Conventional wall breaking technology needs pollen being prepared into pollen aqueous solution mostly, carries out broken wall on this basis, but
This broken wall treatment can be there are considerable influence, because flavones dissolubility under aqueous solution is poor for follow-up extracting flavonoids.
The beneficial effects of the invention are as follows：The present invention carries out eucommia Bark male flower powder broken wall, mainly profit using tubular heater
Reaction environment is rapidly achieved the temperature of difference Poluo wall with the faster rate of heat addition of the equipment and a height uniformly, stable is provided
Warm environment, can make pollen uniformly effectively be heated broken wall, while add can be to avoid things such as flavones with nitrogen as protective gas
Matter high-temperature oxydation.Microwave assisting method mainly make use of the penetrability of microwave, and microwave can directly act on material solute molecule, make
It is brought rapidly up, and increases its dissolubility, and speed is significantly larger than traditional Convective Heating；At the same time microwave using dipole ion movement and
Ionic conduction two ways, makes eucommia Bark male flower flour cell expand broken wall, the flavones in cell can be come into full contact with solvent and then
Dissolving, can increase substantially extraction efficiency, improve general flavone yield.Compared to traditional microwave extract method, present invention side
Method uses gradient power microwave radiation exaraction operating process, and the three-stage microwave radiation technology progressively to be successively decreased by microwave irradiation power extracts
Take and combine intermittent cooling, on the one hand before extraction the phase using higher microwave irradiation intensity can the flavones Rapid Leaching stage into
Flavones extracts and efficiency in one step lifting pollen, and on the other hand the phase can also be reduced pair using relatively low microwave irradiation intensity after the extraction
The thermal degradation of flavones has been leached in extracting solution；
Present invention extraction general flavone yield is high, and eucommia Bark male flower powder contains general flavone 3.36%, and present invention extraction general flavone yield is
3.34%, better than soak extraction and ultrasonic extracting method.
Embodiment
Below in conjunction with the embodiment of the present invention, technical scheme is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's all other embodiments obtained under the premise of not making the creative labor, belong to this hair
The scope of bright protection.
Embodiment 1
The fresh eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried hero
Pollen crosses 60 mesh sieves, is stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 100
DEG C, heating rate is 20 DEG C/min, heats the 10min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by material
Liquor ratio 1:40g/mL adds the ethanol water of volumetric concentration 70%, soaks 1min, obtains pollen alcohol mixed solution；By pollen
Alcohol mixed solution is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 2450MHz, power 800W,
Under conditions of mixing speed 800rpm, 1min is extracted, obtains pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators,
20min is cooled down to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power
Under conditions of being 800rpm for 500W, mixing speed, 2min is extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
15min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 200W, mixing speed are 800rpm, 5min is extracted；Extracting solution after processing is stood into 5min, is cooled to room temperature；Will
The pollen extracting liquid stand, cooled down is placed in a centrifuge, and 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Will
Supernatant is fitted into round-bottomed flask, is placed in Rotary Evaporators, and under conditions of 40 DEG C of temperature, vacuum are 0.09MPa, decompression is steamed
40min is evaporated, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, flavones yield is calculated
For 3.34%.
Embodiment 2
The fresh eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 55 DEG C, untill constant weight；Dried hero
Pollen crosses 80 mesh sieves, is stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 80 DEG C,
Heating rate is 15 DEG C/min, heats the 5min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio
1:50g/mL adds the ethanol water of volumetric concentration 70%, soaks 5min, obtains pollen alcohol mixed solution；By pollen ethanol
Mixed solution is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 2450MHz, power 800W, stirring
Under conditions of speed 600rpm, 38s is extracted, obtains pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
16min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 500W, mixing speed are 600rpm, 1min 20s are extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
12min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 200W, mixing speed are 600rpm, 3min is extracted；Extracting solution after processing is stood into 3min, is cooled to room temperature；Will
The pollen extracting liquid stand, cooled down is placed in a centrifuge, and 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Will
Supernatant is fitted into round-bottomed flask, is placed in Rotary Evaporators, under conditions of temperature 60 C, vacuum 0.08MPa, vacuum distillation
20min, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, calculating flavones yield is
3.11%。
Embodiment 3
The eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried male pollen
40 mesh sieves are crossed, are stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 90 DEG C, heating
Speed is 18 DEG C/min, heats the 8min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio 1:
30g/mL adds the ethanol water of volumetric concentration 60%, soaks 1min, obtains pollen alcohol mixed solution；Pollen ethanol is mixed
Close solution be placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 2450MHz, power 800W, stirring speed
Spend under conditions of 300rpm, extract 35s, obtain pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
16min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 500W, mixing speed are 300rpm, 1min is extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
11min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 200W, mixing speed are 300rpm, 3min is extracted；Extracting solution after processing is stood into 3min, is cooled to room temperature；Will
The pollen extracting liquid stand, cooled down is placed in a centrifuge, and 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Will
Supernatant is fitted into round-bottomed flask, is placed in Rotary Evaporators, and under conditions of temperature 50 C, vacuum 0.085MPa, decompression is steamed
30min is evaporated, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, flavones yield is calculated
For 3.02%.
Embodiment 4
The eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 50 DEG C, untill constant weight；Dried male pollen
80 mesh sieves are crossed, are stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 95 DEG C, heating
Speed is 20 DEG C/min, heats the 10min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio 1:
40g/mL adds the ethanol water of volumetric concentration 80%, soaks 5min, obtains pollen alcohol mixed solution；Pollen ethanol is mixed
Close solution be placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 2450MHz, power 800W, stirring speed
Spend under conditions of 600rpm, extract 45s, obtain pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
18min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 500W, mixing speed are 600rpm, 1min 40s are extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
14min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 200W, mixing speed are 600rpm, 4min is extracted；Extracting solution after processing is stood into 4min, is cooled to room temperature；；
The pollen extracting liquid will stand, cooled down is placed in a centrifuge, and 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；
Supernatant is fitted into round-bottomed flask, is placed in Rotary Evaporators, under conditions of temperature 60 C, vacuum 0.08MPa, decompression is steamed
20min is evaporated, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, flavones yield is calculated
For 3.20%.
Embodiment 5
The eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 50 DEG C, untill constant weight；Dried male pollen
80 mesh sieves are crossed, are stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 85 DEG C, heating
Speed is 15 DEG C/min, heats the 8min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio 1:
50g/mL adds the ethanol water of volumetric concentration 60%, soaks 2min, obtains pollen alcohol mixed solution；Pollen ethanol is mixed
Close solution be placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 2450MHz, power 800W, stirring speed
Spend under conditions of 200rpm, extract 30s, obtain pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
15min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 500W, mixing speed are 200rpm, 1min is extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
10min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 200W, mixing speed are 200rpm, 2min is extracted；Extracting solution after processing is stood into 2min, is cooled to room temperature；Will
The pollen extracting liquid stand, cooled down is placed in a centrifuge, and 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Will
Supernatant is fitted into round-bottomed flask, is placed in Rotary Evaporators, under conditions of 40 DEG C of temperature, vacuum 0.09MPa, vacuum distillation
60min, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, calculating flavones yield is
3.0%。
Embodiment 6
The fresh eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried hero
Pollen crosses 60 mesh sieves, is stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 98 DEG C,
Heating rate is 20 DEG C/min, heats the 10min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio
1:40g/mL adds the ethanol water of volumetric concentration 70%, soaks 1min, obtains pollen alcohol mixed solution；By pollen ethanol
Mixed solution is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 915MHz, power 800W, stirring speed
Spend under conditions of 700rpm, extract 1min, obtain pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
18min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 915MHz, power are
Under conditions of 500W, mixing speed are 700rpm, 2min is extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
13min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 915MHz, power are
Under conditions of 200W, mixing speed are 700rpm, 5min is extracted；Extracting solution after processing is stood into 4min, is cooled to room temperature；Will
The pollen extracting liquid stand, cooled down is placed in a centrifuge, and 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Will
Supernatant is fitted into round-bottomed flask, is placed in Rotary Evaporators, and under conditions of 55 DEG C of temperature, vacuum are 0.08MPa, decompression is steamed
35min is evaporated, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, flavones yield is calculated
For 3.22%.
Embodiment 7
The fresh eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried hero
Pollen crosses 60 mesh sieves, is stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 98 DEG C,
Heating rate is 20 DEG C/min, heats the 10min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio
1:40g/mL adds the ethanol water of volumetric concentration 70%, soaks 1min, obtains pollen alcohol mixed solution；By pollen ethanol
Mixed solution is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 2400MHz, power 800W, stirring
Under conditions of speed 700rpm, 1min is extracted, obtains pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
19min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2400MHz, power are
Under conditions of 500W, mixing speed are 700rpm, 2min is extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, is cooled down
14min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2400MHz, power are
Under conditions of 200W, mixing speed are 700rpm, 5min is extracted；Extracting solution after processing is stood into 4min, is cooled to room temperature；Will
The pollen extracting liquid stand, cooled down is placed in a centrifuge, and 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Will
Supernatant is fitted into round-bottomed flask, is placed in Rotary Evaporators, and under conditions of 55 DEG C of temperature, vacuum are 0.08MPa, decompression is steamed
35min is evaporated, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, flavones yield is calculated
For 3.32%.
Comparative example 1
The method of soak extraction eucommia Bark male flower powder flavones, comprises the following steps：
The eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried male pollen
80 mesh sieves are crossed, are stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 100 DEG C, is risen
Warm speed is 20 DEG C/min, heats the 10min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio 1:
40g/mL adds the ethanol water of volumetric concentration 70%, and pollen alcohol mixed solution is soaked 4h at room temperature, obtains pollen and carries
Take liquid；Pollen extracting liquid is stood into 30min, cooled to room temperature；It will stand, the pollen extracting liquid of cooling is placed in centrifuge
In, 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Supernatant is loaded into round-bottomed flask, is placed in rotary evaporation
In instrument, under conditions of 40 DEG C of temperature, vacuum 0.09MPa, 56min is evaporated under reduced pressure, removes second alcohol and water, obtain flavones concentration
Liquid；With aluminum nitrate colorimetric determination flavones concentrate, it is 2.7% to calculate flavones yield.
Comparative example 2
The method of ultrasound assisted extraction eucommia Bark male flower powder general flavone, comprises the following steps：
The eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried male pollen
80 mesh sieves are crossed, are stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 100 DEG C, is risen
Warm speed is 20 DEG C/min, heats the 10min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by solid-liquid ratio 1:
25g/mL adds the ethanol water of volumetric concentration 70%；Pollen alcohol mixed solution is placed in shaking table, rotating speed is set
150rpm, mixing time 5min；The pollen alcohol mixed solution of mixing is placed in and is cleaned by ultrasonic in instrument, in power 400W conditions
Under, 100min is extracted, obtains pollen extracting liquid；Pollen extracting liquid is stood into 30min, is cooled to room temperature；Pollen extracting liquid is put
In centrifuge, 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Supernatant is loaded into round-bottomed flask, is placed in
In Rotary Evaporators, under conditions of temperature 45 C, vacuum 0.09MPa, 50min is evaporated under reduced pressure, removes second alcohol and water, is obtained
Flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, it is 3.10% to calculate flavones yield.
Comparative example 3
The fresh eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried hero
Pollen crosses 60 mesh sieves, is stored in -20 DEG C of refrigerators；The eucommia Bark male flower powder of refrigeration is taken, by solid-liquid ratio 1:40g/mL adds volumetric concentration
70% ethanol water, soaks 1min, obtains pollen alcohol mixed solution；Pollen alcohol mixed solution is placed in magnetic force
It is 2450MHz, under conditions of power 800W, mixing speed 800rpm in microwave frequency in the Microwave Extraction Apparatus of agitating device, extraction
1min is taken, obtains pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, cooling 20min to room temperature；After cooling down
Pollen extracting liquid be placed in microwave abstracting instrument, microwave frequency 2450MHz, power 500W, mixing speed 800rpm
Under conditions of, extract 2min；Extracting solution after processing is positioned over 4 DEG C of refrigerators, cooling 15min to room temperature；By flower after cooling
Powder extracting solution is placed in microwave abstracting instrument, the bar that microwave frequency 2450MHz, power 200W, mixing speed are 800rpm
Under part, 5min is extracted；Extracting solution after processing is stood into 5min, is cooled to room temperature；It will stand, the pollen extracting liquid of cooling is placed in
In centrifuge, 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Supernatant is loaded into round-bottomed flask, is placed in rotation
Turn in evaporimeter, under conditions of 40 DEG C of temperature, vacuum are 0.08MPa, be evaporated under reduced pressure 50min, remove second alcohol and water, obtain
Flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, it is 2.88% to calculate flavones yield.
Comparative example 4
The fresh eucommia Bark male flower powder of collection is placed in thermostatic drying chamber the drying at 60 DEG C, untill constant weight；Dried hero
Pollen crosses 60 mesh sieves, is stored in -20 DEG C of refrigerators；The pollen of refrigeration is placed in tubular heater, heating-up temperature is set to 100
DEG C, heating rate is 20 DEG C/min, heats the 10min that holds time, is cooled to room temperature；The eucommia Bark male flower powder after processing is taken, by material
Liquor ratio 1:40g/mL adds the ethanol water of volumetric concentration 70%, soaks 1min, obtains pollen alcohol mixed solution；By pollen
Alcohol mixed solution is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, microwave frequency for 2450MHz, power 800W,
Under conditions of mixing speed 0rpm, 1min is extracted, obtains pollen extracting liquid；Extracting solution after processing is positioned over 4 DEG C of refrigerators, it is cold
But 21min is to room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power are
Under conditions of 500W, mixing speed are 0rpm, 2min is extracted；Extracting solution after processing is positioned over 4 DEG C of refrigerators, cools down 17min
To room temperature；Pollen extracting liquid after cooling is placed in microwave abstracting instrument, microwave frequency 2450MHz, power 200W, stir
Speed is mixed under conditions of 0rpm, to extract 5min；Extracting solution after processing is stood into 5min, is cooled to room temperature；It will stand, cooling
Pollen extracting liquid be placed in a centrifuge, 18min is centrifuged under the conditions of 10000rpm, is collected supernatant；Supernatant is filled
Enter round-bottomed flask, be placed in Rotary Evaporators, under conditions of 40 DEG C of temperature, vacuum are 0.085MPa, vacuum distillation
40min, removes second alcohol and water, obtains flavones concentrate；With aluminum nitrate colorimetric determination flavones concentrate, calculating flavones yield is
3.15%。
1 three kinds of extracting method contrasts of table
| Experimental project is numbered | Pollen broken wall | Extracting method | Magnetic agitation | Extraction time（min） | General flavone yield |
| Embodiment 1 | Have | Microwave Extraction | Have | 48 | 3.34% |
| Comparative example 1 | Have | Soak extraction | Nothing | 100 | 2.70% |
| Comparative example 2 | Have | Ultrasonic extraction | Nothing | 240 | 3.10% |
| Comparative example 3 | Nothing | Microwave Extraction | Have | 48 | 2.88% |
| Comparative example 4 | Have | Microwave Extraction | Nothing | 51 | 3.15% |
The result shows that gradient power Microwave Extraction is better than soak extraction and ultrasonic extraction side in flavones yield and extraction time
Method；By the pollen of broken wall treatment, flavones yield is higher than undressed；Magnetic agitation can improve Microwave Extraction bark of eucommia hero
Pollen flavones yield
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.
Claims (8)
1. the method for flavones is extracted in a kind of powder from eucommia Bark male flower, it is characterised in that step is as follows：
（1）Fresh eucommia Bark male flower powder is dried to constant weight, sieving at 50 ~ 60 DEG C, obtained eucommia Bark male flower powder is at -20 DEG C
Refrigeration；
（2）By step（1）The eucommia Bark male flower powder of refrigeration, which is placed in tubular heater, carries out heating broken wall treatment；
（3）By step（2）Eucommia Bark male flower powder after broken wall treatment is placed in immersion treatment in ethanol water, obtains pollen ethanol and mixes
Close solution；
（4）By step（3）The pollen alcohol mixed solution of acquisition is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, extraction
0.5 ~ 1 min, obtains pollen extracting liquid；
（5）By step（4）The pollen extracting liquid of acquisition is positioned over 15 ~ 20min of standing in 4 DEG C of refrigerators, is cooled to room temperature；
（6）By step（5）Pollen extracting liquid after standing is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, and extraction 1 ~
2min；
（7）By step（6）Pollen extracting liquid after extraction is placed in 10 ~ 15min of standing in 4 DEG C of refrigerators, is cooled to room temperature；
（8）By step（7）Pollen extracting liquid after cooling is placed in the Microwave Extraction Apparatus with magnetic stirring apparatus, and extraction 2 ~
5min；
（9）By step（8）Pollen extracting liquid after extraction stands 2 ~ 5min, cooled to room temperature；
（10）By step（9）Pollen extracting liquid after cooling is placed in a centrifuge, and centrifugation collects supernatant；
（11）By step（10）The supernatant vacuum distillation of collection, obtains flavones concentrate.
2. the method for flavones is extracted in the powder according to claim 1 from eucommia Bark male flower, it is characterised in that：The step（1）
40 ~ 80 mesh sieves are crossed after middle eucommia Bark male flower powder constant weight.
3. the method for flavones is extracted in the powder according to claim 1 from eucommia Bark male flower, it is characterised in that：The step（2）
Middle tubular heater is warming up to 80 ~ 100 DEG C with the speed of 15-20 DEG C/min, and processing time is 5 ~ 10min, is led in heating process
Enter nitrogen as protection gas.
4. the method for flavones is extracted in the powder according to claim 1 from eucommia Bark male flower, it is characterised in that：The step（3）
The volumetric concentration of middle ethanol water is 60% ~ 80%, by 1g eucommia Bark male flower powder be added in 30 ~ 50ml ethanol waters immersion 1 ~
5 min。
5. the method for flavones is extracted in the powder according to claim 1 from eucommia Bark male flower, it is characterised in that：The microwave abstracting
The frequency of instrument is 915 ~ 2450MHz, and power is 200 ~ 800W, and the mixing speed of magnetic stirring apparatus is 200 ~ 800rpm.
6. the method for flavones is extracted in the powder according to claim 1 from eucommia Bark male flower, it is characterised in that：The step（10）
The centrifugal speed of middle centrifuge is 8000 ~ 10000rpm, and centrifugation time is 15 ~ 20min.
7. the method for flavones is extracted in the powder according to claim 1 from eucommia Bark male flower, it is characterised in that：The step（11）
Middle supernatant is evaporated under reduced pressure using Rotary Evaporators, and rotating evaporation temperature is 40 ~ 60 DEG C, and vacuum is 0.08 ~ 0.09MPa, when
Between be 20 ~ 60min.
8. application of the flavones in health care, food and industry described in claim 1-7.
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