CN105362311A - Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers - Google Patents
Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers Download PDFInfo
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 43
- 229930003944 flavone Natural products 0.000 title claims abstract description 35
- 235000011949 flavones Nutrition 0.000 title claims abstract description 35
- 150000004676 glycans Chemical class 0.000 title claims abstract description 33
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 33
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 33
- 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 23
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 23
- 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 23
- 238000000034 method Methods 0.000 title abstract description 11
- 240000005959 Abelmoschus manihot Species 0.000 title abstract description 9
- 235000001075 Abelmoschus manihot Nutrition 0.000 title abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 241000628997 Flos Species 0.000 claims description 43
- 235000005739 manihot Nutrition 0.000 claims description 43
- 238000002955 isolation Methods 0.000 claims description 17
- 150000002213 flavones Chemical class 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- 239000002893 slag Substances 0.000 claims description 7
- 206010013786 Dry skin Diseases 0.000 claims description 6
- 238000005138 cryopreservation Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 4
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000002879 macerating effect Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 241000221022 Manihot Species 0.000 claims 8
- 239000003814 drug Substances 0.000 abstract description 7
- 229940079593 drug Drugs 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000004821 distillation Methods 0.000 abstract description 2
- 239000011149 active material Substances 0.000 abstract 2
- 238000000926 separation method Methods 0.000 abstract 2
- 240000003183 Manihot esculenta Species 0.000 description 35
- 238000002360 preparation method Methods 0.000 description 9
- 239000013543 active substance Substances 0.000 description 6
- 229930003935 flavonoid Natural products 0.000 description 6
- 150000002215 flavonoids Chemical class 0.000 description 6
- 235000017173 flavonoids Nutrition 0.000 description 6
- 239000012567 medical material Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- OVSQVDMCBVZWGM-SJWGPRHPSA-N Hyperin Natural products O[C@H]1[C@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-SJWGPRHPSA-N 0.000 description 2
- FVQOMEDMFUMIMO-UHFFFAOYSA-N Hyperosid Natural products OC1C(O)C(O)C(CO)OC1OC1C(=O)C2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 FVQOMEDMFUMIMO-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- OVSQVDMCBVZWGM-DTGCRPNFSA-N quercetin 3-O-beta-D-galactopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-DTGCRPNFSA-N 0.000 description 2
- BBFYUPYFXSSMNV-UHFFFAOYSA-N quercetin-7-o-galactoside Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=C2C(=O)C(O)=C(C=3C=C(O)C(O)=CC=3)OC2=C1 BBFYUPYFXSSMNV-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241001573881 Corolla Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000219071 Malvaceae Species 0.000 description 1
- 206010028116 Mucosal inflammation Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 210000005095 gastrointestinal system Anatomy 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- NQYPTLKGQJDGTI-FCVRJVSHSA-N hyperoside Natural products OC[C@H]1O[C@@H](OC2=C(Oc3cc(O)cc(O)c3[C@H]2O)c4ccc(O)c(O)c4)[C@H](O)[C@@H](O)[C@H]1O NQYPTLKGQJDGTI-FCVRJVSHSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 210000003097 mucus Anatomy 0.000 description 1
- 201000008383 nephritis Diseases 0.000 description 1
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 206010039073 rheumatoid arthritis Diseases 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
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- 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)
-
- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- 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
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
-
- 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
-
- 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
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers. The method comprises the following steps: (1) smashing the abelmoschus manihot flowers dried in the shade into 10-80 mesh powder, adding an organic solvent into the powder, and carrying out reflux extraction, thus obtaining an extracting solution and drug dregs; (2) preparing volatile oil, namely, carrying out water distillation on the extracting solution to prepare the volatile oil of the abelmoschus manihot flowers; (3) carrying out extraction on the drug dregs by adopting warm water, and adding ethanol into the liquid obtained after extraction for separation, thus obtaining a supernate and a precipitate; (4) preparing general flavone, namely, concentrating and drying the supernate to obtain the general flavone; and (5) preparing total polysaccharide, namely, drying the precipitate, thus obtaining the total polysaccharide. According to the method for extracting and separating the volatile oil, the flavone and the polysaccharide of abelmoschus manihot flowers, the three-component extraction separation method is adopted, and the three active materials, including the volatile oil, the flavone and the polysaccharide of the abelmoschus manihot flowers are extracted and separated, the active materials of the abelmoschus manihot flower medicinal material are sufficiently utilized, and a foundation is laid for the comprehensive development and application of the abelmoschus manihot flower medicinal material.
Description
Technical field
The present invention relates to Chinese crude drug extractive technique field, particularly relate to a kind of method of three way classification extraction and isolation Flos abelmoschi manihot volatile oil, flavone and polysaccharide.
Background technology
Flos abelmoschi manihot is the dry corolla of Malvaceae plant Abelmoschusmanihot (L.) Medic..2015 editions " Chinese Pharmacopoeias " record, and have eliminating damp-heat, and subduing swelling and detoxicating effect is held back for damp and hot heap soil or fertilizer over and around the roots, stranguria with turbid discharge edema; External treatment swollen ulcer drug, burn due to hot liquid or fire etc.Main containing flavonoid, polysaccharide and volatile oil isoreactivity material in Flos abelmoschi manihot.2015 editions " Chinese Pharmacopoeias " detect control substance of plant drug using hyperin as Flavone content.In recent years the polysaccharide of Flos abelmoschi manihot, volatile oil also there are is further investigation and applied widely.
After current Chinese crude drug usually extracts certain class material, other a large amount of active substances are abandoned with medicinal residues, can not make full use of medical material.Flos abelmoschi manihot is also usually be extracted total flavones, wastes volatile oil; Be extracted total polysaccharides, abandon flavonoid etc. with medicinal residues.For making full use of medical material, the present invention adopts the method for three points of extraction and isolation, and by three class materials of Flos abelmoschi manihot, volatile oil, flavone and Polyose extraction are separated preparation.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method of extraction and isolation Flos abelmoschi manihot volatile oil, flavone and polysaccharide is provided, adopt the method for three points of extraction and isolation, by three class active substances of Flos abelmoschi manihot, volatile oil, flavone and Polyose extraction are separated preparation, make full use of Flos abelmoschi manihot medical material, for the comprehensive exploitation application of Flos abelmoschi manihot medical material is laid a good foundation.
To achieve these goals, the present invention adopts following technical scheme:
A method for extraction and isolation Flos abelmoschi manihot volatile oil, flavone and polysaccharide, comprises the following steps:
(1) Flos abelmoschi manihot dried in the shade is ground into 10-80 order powder, is placed in apparatus,Soxhlet's, adds low boiling point organic solvent, 30-60 DEG C of heating and refluxing extraction, obtains extracting solution and medicinal residues;
(2) volatile oil is prepared: the extracting solution of step (1) is waved most organic solvent, load in volatile oil extractor, add distilled water jolting mixing, connect reflux condensing tube, heating is distilled to volatile oil in volatile oil extractor no longer to be increased, and cooling, collection oil reservoir, then add inorganic salt and dewater in oil reservoir, sealing is preserved, and obtains Flos abelmoschi manihot volatile oil;
(3) in the medicinal residues of step (1), add its weight 10-30 distilled water doubly, 60 DEG C-80 DEG C warm macerating 2-4h, centrifugally to remove slag, lixiviate 1-3 time, merge extractive liquid, extracting solution is concentrated into 1:10-30, add the ethanol that concentration is 95%, make alcohol content reach 60%-80%, staticly settle 12-24h, obtain supernatant and precipitate;
(4) total flavones is prepared: after the supernatant after step (3) precipitate with ethanol being placed in Rotary Evaporators recovery ethanol, water-bath is concentrated into paste, and put vacuum drying oven 80 DEG C of dryings, be ground into fine powder, airtight cryopreservation, obtains total flavones;
(5) total polysaccharides is prepared: the precipitate after step (3) precipitate with ethanol is directly placed in vacuum drying oven 80 DEG C of dryings, be ground into fine powder, airtight cryopreservation, obtains total polysaccharides.
Preferably, in step (1), the Flos abelmoschi manihot dried in the shade is ground into 60 order powder.
Preferably, the low boiling point organic solvent described in step (1) is one or both in ether, petroleum ether.
Preferably, the inorganic salt described in step (2) is anhydrous sodium sulfate.
Preferably, centrifugal described in step (3) is removed slag, and centrifuge speed is 3500r/min, centrifugation time 20min.
Compared with the prior art, beneficial effect of the present invention is as follows:
(1) method of extraction and isolation Flos abelmoschi manihot volatile oil of the present invention, flavone and polysaccharide, characteristic for Flos abelmoschi manihot adopts the method for three points of extraction and isolation, by three class active substances of Flos abelmoschi manihot, volatile oil, flavone and Polyose extraction are separated preparation, take full advantage of the active substance of Flos abelmoschi manihot medical material.
(2) the present invention first uses oil substances in organic solvent continuous circumfluence extraction Flos abelmoschi manihot, distilling with water prepares volatile oil, one is the problem solving the distillation of Flos abelmoschi manihot unsuitable directly water, and two is eliminate the low polar impurity of part, is more conducive to the extraction of flavonoid, polysaccharose substance;
(3) medicinal residues of the present invention adopt 60 DEG C-80 DEG C warm water lixiviates, are beneficial to flavonoid and polysaccharose substance leaching; Then centrifugally to remove slag, because Flos abelmoschi manihot contains a large amount of mucus colloids, soup thickness after warm water lixiviate, adopt the method for " centrifugal remove slag ", it is difficult to filter after solving Flos abelmoschi manihot water extraction, wastes large problem; Utilize the size of flavonoid and polysaccharose substance polarity and molecular weight, adopt precipitate with ethanol to be separated, the flavonoid being dissolved in ethanol, in supernatant, is insoluble to the polysaccharide precipitation of ethanol, then by supernatant with precipitate concentrate drying respectively and prepare total flavones and total polysaccharides; Flos abelmoschi manihot volatile oil yield of the present invention reaches 0.8%, and total flavones yield reaches 38%, and total polysaccharides yield reaches 16%.
(4) the present invention adopts the method for three points of extraction and isolation, by three class materials of Flos abelmoschi manihot, volatile oil, flavone and Polyose extraction are separated preparation, the Flos abelmoschi manihot volatile oil of preparation, all has effect in the many-side such as cardio-cerebrovascular, central nervous system, respiratory system, gastrointestinal system, antibacterial, antiinflammatory, anticancer, antiviral, promotion drug absorption; The Flos abelmoschi manihot total flavones of preparation has analgesic activity, prevention of osteoporosis, is used for the treatment of the disease such as nephritis, rheumatoid arthritis; The Flos abelmoschi manihot total polysaccharides of preparation can be used as thickening agent and stabilizing agent in the food industry, or for the lubricant of mucosal inflammation, play protection, abirritant effect, polysaccharide prepared by this law also can adopt removing protein, decolouring or column chromatography separating purification technique to prepare comparatively holosaccharide; The present invention is that the comprehensive exploitation application etc. of Flos abelmoschi manihot medical material is laid a good foundation.
Accompanying drawing explanation
Fig. 1 is flow chart of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but the present invention is not limited only to these embodiments, and under the prerequisite not departing from present inventive concept, any improvement done all drops within protection scope of the present invention.
Embodiment 1:
A method for extraction and isolation Flos abelmoschi manihot volatile oil, flavone and polysaccharide, comprises the following steps:
(1) Flos abelmoschi manihot dried in the shade is ground into 60 order powder, is placed in apparatus,Soxhlet's, adds petroleum ether, 30-60 DEG C of heating and refluxing extraction, obtains extracting solution and medicinal residues;
(2) volatile oil is prepared: the extracting solution of step (1) is waved most organic solvent, load in volatile oil extractor, add distilled water jolting mixing, connect reflux condensing tube, heating is distilled to volatile oil in volatile oil extractor no longer to be increased, and cooling, collection oil reservoir, then add anhydrous sodium sulfate and dewater in oil reservoir, sealing is preserved, and obtains Flos abelmoschi manihot volatile oil;
(3) in the medicinal residues of step (1), first time adds the distilled water of its weight 20 times, and second time adds the distilled water of its weight 10 times, 70 DEG C of warm macerating 3h, centrifugally to remove slag, centrifuge speed is 3500r/min, centrifugation time 20min, lixiviate 2 times, merge extractive liquid, extracting solution is concentrated into 1:30, adds the ethanol that concentration is 95%, makes alcohol content reach 80%, staticly settle 20h, obtain supernatant and precipitate;
(4) total flavones is prepared: after the supernatant after step (3) precipitate with ethanol being placed in Rotary Evaporators recovery ethanol, water-bath is concentrated into paste, and put vacuum drying oven 80 DEG C of dryings, be ground into fine powder, airtight cryopreservation, obtains total flavones;
(5) total polysaccharides is prepared: the precipitate after step (3) precipitate with ethanol is directly placed in vacuum drying oven 80 DEG C of dryings, be ground into fine powder, airtight cryopreservation, obtains total polysaccharides.
The obtaining ratio and content of the present embodiment 1 extraction and isolation Flos abelmoschi manihot three class active substance is as following table 1:
The obtaining ratio and content of table 1 extraction and isolation Flos abelmoschi manihot three class active substance
Flos abelmoschi manihot volatile oil yield prepared by the present embodiment 1 is 0.8%; Total flavones yield is 38%; Total polysaccharides yield is 16%.By 2015 editions " Chinese Pharmacopoeia " detection methods, the general flavone content of preparation reaches 42.3%, and the sugared content adopting phenol-sulfuric acid and colorimetric method to measure this polysaccharide is 72.2%, and adopting HPLC to detect Determination of Hyperoside in the total flavones of preparation is 2.13%.
Claims (5)
1. a method for extraction and isolation Flos abelmoschi manihot volatile oil, flavone and polysaccharide, is characterized in that: comprise the following steps:
(1) Flos abelmoschi manihot dried in the shade is ground into 10-80 order powder, is placed in apparatus,Soxhlet's, adds low boiling point organic solvent, 30-60 DEG C of heating and refluxing extraction, obtains extracting solution and medicinal residues;
(2) volatile oil is prepared: the extracting solution of step (1) is waved most organic solvent, load in volatile oil extractor, add distilled water jolting mixing, connect reflux condensing tube, heating is distilled to volatile oil in volatile oil extractor no longer to be increased, and cooling, collection oil reservoir, then add inorganic salt and dewater in oil reservoir, sealing is preserved, and obtains Flos abelmoschi manihot volatile oil;
(3) in the medicinal residues of step (1), add its weight 10-30 distilled water doubly, 60 DEG C-80 DEG C warm macerating 2-4h, centrifugally to remove slag, lixiviate 1-3 time, merge extractive liquid, extracting solution is concentrated into 1:10-30, add the ethanol that concentration is 95%, make alcohol content reach 60%-80%, staticly settle 12-24h, obtain supernatant and precipitate;
(4) total flavones is prepared: after the supernatant after step (3) precipitate with ethanol being placed in Rotary Evaporators recovery ethanol, water-bath is concentrated into paste, and put vacuum drying oven 80 DEG C of dryings, be ground into fine powder, airtight cryopreservation, obtains total flavones;
(5) total polysaccharides is prepared: the precipitate after step (3) precipitate with ethanol is directly placed in vacuum drying oven 80 DEG C of dryings, be ground into fine powder, airtight cryopreservation, obtains total polysaccharides.
2. the method for extraction and isolation Flos abelmoschi manihot volatile oil according to claim 1, flavone and polysaccharide, is characterized in that: in step (1), the Flos abelmoschi manihot dried in the shade is ground into 60 order powder.
3. the method for extraction and isolation Flos abelmoschi manihot volatile oil according to claim 1, flavone and polysaccharide, is characterized in that: the low boiling point organic solvent described in step (1) is one or both in ether, petroleum ether.
4. the method for extraction and isolation Flos abelmoschi manihot volatile oil according to claim 1, flavone and polysaccharide, is characterized in that: the inorganic salt described in step (2) is anhydrous sodium sulfate.
5. the method for extraction and isolation Flos abelmoschi manihot volatile oil according to claim 1, flavone and polysaccharide, is characterized in that: centrifugal described in step (3) is removed slag, and centrifuge speed is 3500r/min, centrifugation time 20min.
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| CN201510822519.2A CN105362311A (en) | 2015-11-23 | 2015-11-23 | Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105926044A (en) * | 2016-05-26 | 2016-09-07 | 南京中医药大学 | Comprehensive utilization method of natural polysaccharides and plant fiber in abelmoschus manihot waste |
| CN105999022A (en) * | 2016-05-03 | 2016-10-12 | 劲牌生物医药有限公司 | Method for extracting fructus amomi volatile oil, fructus amomi flavone and fructus amomi polysaccharide by utilizing fructus amomi |
| CN109576048A (en) * | 2018-10-30 | 2019-04-05 | 湖南华诚生物资源股份有限公司 | The method extracted volatile oil from sunglo and extract sunglo polysaccharide and usnic acid simultaneously |
| CN109731367A (en) * | 2019-01-26 | 2019-05-10 | 王德明 | A kind of technology of plant extraction freeze-dried powder |
| CN113952368A (en) * | 2021-09-29 | 2022-01-21 | 沈阳化工研究院有限公司 | Method for simultaneously extracting abelmoschus manihot polysaccharide and flavone |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451022A (en) * | 2013-09-02 | 2013-12-18 | 南昌大学 | Method for integrally extracting volatile oil, polysaccharide and flavone from elsholtzia haichowensis sun |
| CN103952240A (en) * | 2014-05-19 | 2014-07-30 | 安徽科技学院 | Preparation method of abelmoschus manihot essential oil |
-
2015
- 2015-11-23 CN CN201510822519.2A patent/CN105362311A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451022A (en) * | 2013-09-02 | 2013-12-18 | 南昌大学 | Method for integrally extracting volatile oil, polysaccharide and flavone from elsholtzia haichowensis sun |
| CN103952240A (en) * | 2014-05-19 | 2014-07-30 | 安徽科技学院 | Preparation method of abelmoschus manihot essential oil |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105999022A (en) * | 2016-05-03 | 2016-10-12 | 劲牌生物医药有限公司 | Method for extracting fructus amomi volatile oil, fructus amomi flavone and fructus amomi polysaccharide by utilizing fructus amomi |
| CN105999022B (en) * | 2016-05-03 | 2019-10-25 | 劲牌生物医药有限公司 | A method of amomum fruit volatile oil, fructus amomi flavones and fructus amomi polysaccharide are extracted using fructus amomi |
| CN105926044A (en) * | 2016-05-26 | 2016-09-07 | 南京中医药大学 | Comprehensive utilization method of natural polysaccharides and plant fiber in abelmoschus manihot waste |
| CN105926044B (en) * | 2016-05-26 | 2018-04-06 | 南京中医药大学 | The method of comprehensive utilization of natural polysaccharide and string in Sunset Abelmoschus Root discarded object |
| CN109576048A (en) * | 2018-10-30 | 2019-04-05 | 湖南华诚生物资源股份有限公司 | The method extracted volatile oil from sunglo and extract sunglo polysaccharide and usnic acid simultaneously |
| CN109576048B (en) * | 2018-10-30 | 2022-06-14 | 湖南华诚生物资源股份有限公司 | Method for extracting volatile oil from usnea and simultaneously extracting usnea polysaccharide and usnic acid |
| CN109731367A (en) * | 2019-01-26 | 2019-05-10 | 王德明 | A kind of technology of plant extraction freeze-dried powder |
| CN113952368A (en) * | 2021-09-29 | 2022-01-21 | 沈阳化工研究院有限公司 | Method for simultaneously extracting abelmoschus manihot polysaccharide and flavone |
| CN113952368B (en) * | 2021-09-29 | 2023-01-24 | 沈阳化工研究院有限公司 | Method for simultaneously extracting abelmoschus manihot polysaccharide and flavone |
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