CN107722079A - The method that Stibene-glucoside is extracted from the fleece-flower root - Google Patents

The method that Stibene-glucoside is extracted from the fleece-flower root Download PDF

Info

Publication number
CN107722079A
CN107722079A CN201711053788.2A CN201711053788A CN107722079A CN 107722079 A CN107722079 A CN 107722079A CN 201711053788 A CN201711053788 A CN 201711053788A CN 107722079 A CN107722079 A CN 107722079A
Authority
CN
China
Prior art keywords
glucoside
stibene
ethanol
fleece
flower root
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.)
Pending
Application number
CN201711053788.2A
Other languages
Chinese (zh)
Inventor
谢冬养
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guilin Newtel Biological Technology Co Ltd
Original Assignee
Guilin Newtel Biological Technology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Guilin Newtel Biological Technology Co Ltd filed Critical Guilin Newtel Biological Technology Co Ltd
Priority to CN201711053788.2A priority Critical patent/CN107722079A/en
Publication of CN107722079A publication Critical patent/CN107722079A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/203Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses the method that Stibene-glucoside is extracted from the fleece-flower root, comprise the following steps:1) fleece-flower root is crushed, adds alcohol reflux extraction, obtain ethanol extract;2) ethanol extract is recovered under reduced pressure to the medicinal extract that relative density at 40 DEG C is 1.0~1.5, medicinal extract is dissolved in water, filtered, take filtrate standby;3) by the upper S 8+ macroreticular resins of filtrate, water elution is first distilled, then with 50% ethanol elution, collects ethanol eluate;4) solvent is recovered under reduced pressure in ethanol eluate, be freeze-dried, as Stibene-glucoside.Present invention process is simple, and cost is cheap, obtained Stibene-glucoside high purity more than 99%.

Description

The method that Stibene-glucoside is extracted from the fleece-flower root
Technical field
The invention belongs to bioactive ingredients extractive technique field, and in particular to Stibene-glucoside is extracted from the fleece-flower root Method.
Background technology
The fleece-flower root is clinical Chinese medicine, the dried root of polygonaceae plant, and China's plant resources enriches, be distributed in northeast, it is Central-South, East China, southwestern each province.The fleece-flower root after processing has the effect of filling liver kidney, benefiting essence-blood, black beard and hair, strengthening the bones and muscles, change turbid lipid-loweringing, For under blood deficiency chlorosis, dizziness and tinnitus, poliosis, soreness and weakness of waist and knees, extremity numbness, uterine bleeding band, hyperlipidemia etc..Modern study It was found that the fleece-flower root has promotion hematopoiesis containing Multiple components, main pharmacological activity such as Anthraquinones, talan glycoside and flavonoids Function, enhancing immunologic function, reducing blood lipid and antiatherosclerosis, antitumor, liver protection, anti-aging, regulation endocrine, ease constipation Defaecation etc..Anthraquinone analog compound has the effects such as Adjust-blood lipid, cardiac stimulant, antibacterial, anticancer, raising immunologic function, anthracene contained by the fleece-flower root Quinones is secondly Rhein, Physcion and rheochrysin based on rheum emodin, Chrysophanol.The trip of Radix Polygoni Multiflori It is respectively 2.51% and 2.05% from property anthraquinone and associativity anthraquinone, the free property anthraquinone and associativity anthraquinone of prepared fleece flower root are distinguished For 2.63% and 0.87%.Stibene-glucoside have anti-aging, reduce cholesterol, improve immunologic function, preventing and treating artery sclerosis and The functions such as liver protection.Most important diphenylethylene compounds are 2,3,5,4 '-tetrahydroxystilbene -2-O- β-D- in the fleece-flower root Glucoside, abbreviation Stibene-glucoside.The content Radix Polygoni Multiflori of Stibene-glucoside is higher than prepared fleece flower root.Raw content reaches as high as 1.396%.Temperature and humidity influences Stibene-glucoside stability, is raised with temperature, and Stibene-glucoside content drops in prepared fleece flower root It is low.Currently available technology is typically first extracted with organic solvent, then Stibene-glucoside is purified using macroreticular resin, such as AB-8, S-8, X-5, NKA-9, but macroporous resin purification effect is poor, purity is only 70~80%.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of method that Stibene-glucoside is extracted from the fleece-flower root, this method The purity of Stibene-glucoside can be greatly improved.
Technical scheme provided by the invention is the method that Stibene-glucoside is extracted from the fleece-flower root, is comprised the following steps:
1) fleece-flower root is crushed, adds alcohol reflux extraction, obtain ethanol extract;
2) ethanol extract is recovered under reduced pressure to the medicinal extract that relative density at 40 DEG C is 1.0~1.5, by medicinal extract plus water-soluble Solution, filtering, takes filtrate standby;
3) by the upper S-8+ macroreticular resins of filtrate, water elution is first distilled, then with 50% ethanol elution, collects ethanol elution Liquid;
4) solvent is recovered under reduced pressure in ethanol eluate, be freeze-dried, as Stibene-glucoside.
In step 1), ethanol volumetric concentration is 60~80%, and the solid-liquid ratio of the fleece-flower root and ethanol is 1g:10~20ml;Return It is 30~45 DEG C to flow Extracting temperature, and extraction time is 1~3h.
In step 2), the addition of water is 10~15 times of medicinal extract volume.
In step 3), loading flow velocity is 1~3BV/h, and the elution flow rate of distilled water is 2~5BV/h, and ethanol elution flow velocity is 1~2BV/h.
In step 3), the S-8+ resins are polystyrene type Polar Adsorbent Resin, and quality index is as follows:
Outward appearance:The opaque spherical particle of milky;
Moisture content:66~72%;
Pore volume:0.78~0.82ml/g;
Particle size range:0.315~1.25mm >=90%;
Specific surface area:130~150 ㎡/g;
Average pore size:25~27nm;
Apparent density:0.42~0.46g/ml;
Skeletal density:1.20~1.24g/ml;
Wet apparent density:0.60~0.70g/ml;
Wet true density:1.00~1.06g/ml.
S-8+ macroreticular resins are applicants according to produce reality demand, are found by substantial amounts of experiment by former S-8 types macropore Resin average pore size change it is smaller, make its preferably by and adsorb Stibene-glucoside, and the flavones of macromolecule, polysaccharide and egg White matter class material then cannot be introduced into resin, and these macromolecular substances flow directly out without absorption;And the Anthraquinones thing that molecular weight is small Matter is then because the too small speed by resin of molecular weight is faster by the speed of resin than Stibene-glucoside so that the macropore after improvement Resin can be very good to adsorb Stibene-glucoside.In addition, after H103+ macroreticular resins aperture diminishes, specific surface area accordingly increases, energy Increase adsorption area, adsorption and desorption power increases so that Stibene-glucoside separates more thoroughly with other impurities, improves pure Degree.
Compared with prior art, the present invention can be by Stibene-glucoside from Radix Polygoni Multiflori using the H103 types resin after improvement In, high purity more than 99.0%.And present invention process is simple, cost is cheap, is adapted to large-scale industrial production.
Embodiment
The present invention is further elaborated for specific examples below, but not as a limitation of the invention.
Embodiment 1
1) fleece-flower root is crushed to 80 mesh, is 1g by solid-liquid ratio:It is that 60% ethanol is molten that 10ml ratio, which adds volumetric concentration, Liquid, refluxing extraction 1h, obtains ethanol extract at 30 DEG C;
2) ethanol extract is recovered under reduced pressure to the medicinal extract that relative density at 40 DEG C is 1.0, medicinal extract is added into its volume 10 times of water dissolving, filtering, takes filtrate standby;
3) by the upper S-8+ macroreticular resins of filtrate, loading flow velocity is 1BV/h, first distills water elution, the elution flow rate of distilled water For 2BV/h, then eluted with volumetric concentration for 50% ethanol solution, ethanol elution flow velocity is 1BV/h, collects ethanol eluate;
The S-8+ resins are polystyrene type Polar Adsorbent Resin, and quality index is as follows:
Outward appearance:The opaque spherical particle of milky;
Moisture content:66~72%;
Pore volume:0.78~0.82ml/g;
Particle size range:0.315~1.25mm >=90%;
Specific surface area:130~150 ㎡/g;
Average pore size:25~27nm;
Apparent density:0.42~0.46g/ml;
Skeletal density:1.20~1.24g/ml;
Wet apparent density:0.60~0.70g/ml;
Wet true density:1.00~1.06g/ml.
4) solvent is recovered under reduced pressure in ethanol eluate, be freeze-dried, as Stibene-glucoside.
Stibene-glucoside finished product is detected using high performance liquid chromatography, its purity is 99.09%.
Embodiment 2
1) fleece-flower root is crushed to 80 mesh, is 1g by solid-liquid ratio:It is that 80% ethanol is molten that 20ml ratio, which adds volumetric concentration, Liquid, refluxing extraction 3h, obtains ethanol extract at 45 DEG C;
2) ethanol extract is recovered under reduced pressure to the medicinal extract that relative density at 40 DEG C is 1.5, medicinal extract is added into its volume 15 times of water dissolving, filtering, takes filtrate standby;
3) by the upper S-8+ macroreticular resins of filtrate, loading flow velocity is 3BV/h, first distills water elution, the elution flow rate of distilled water For 5BV/h, then eluted with volumetric concentration for 50% ethanol solution, ethanol elution flow velocity is 2BV/h, collects ethanol eluate;
The S-8+ resins are polystyrene type Polar Adsorbent Resin, and quality index is as follows:
Outward appearance:The opaque spherical particle of milky;
Moisture content:66~72%;
Pore volume:0.78~0.82ml/g;
Particle size range:0.315~1.25mm >=90%;
Specific surface area:130~150 ㎡/g;
Average pore size:25~27nm;
Apparent density:0.42~0.46g/ml;
Skeletal density:1.20~1.24g/ml;
Wet apparent density:0.60~0.70g/ml;
Wet true density:1.00~1.06g/ml.
4) solvent is recovered under reduced pressure in ethanol eluate, be freeze-dried, as Stibene-glucoside.
Stibene-glucoside finished product is detected using high performance liquid chromatography, its purity is 99.18%.
Embodiment 3
1) fleece-flower root is crushed to 80 mesh, is 1g by solid-liquid ratio:It is that 70% ethanol is molten that 15ml ratio, which adds volumetric concentration, Liquid, refluxing extraction 2h, obtains ethanol extract at 40 DEG C;
2) ethanol extract is recovered under reduced pressure to the medicinal extract that relative density at 40 DEG C is 1.2, medicinal extract is added into its volume 12 times of water dissolving, filtering, takes filtrate standby;
3) by the upper S-8+ macroreticular resins of filtrate, loading flow velocity is 2BV/h, first distills water elution, the elution flow rate of distilled water For 4BV/h, then eluted with volumetric concentration for 50% ethanol solution, ethanol elution flow velocity is 1.5BV/h, collects ethanol elution Liquid;
The S-8+ resins are polystyrene type Polar Adsorbent Resin, and quality index is as follows:
Outward appearance:The opaque spherical particle of milky;
Moisture content:66~72%;
Pore volume:0.78~0.82ml/g;
Particle size range:0.315~1.25mm >=90%;
Specific surface area:130~150 ㎡/g;
Average pore size:25~27nm;
Apparent density:0.42~0.46g/ml;
Skeletal density:1.20~1.24g/ml;
Wet apparent density:0.60~0.70g/ml;
Wet true density:1.00~1.06g/ml.
4) solvent is recovered under reduced pressure in ethanol eluate, be freeze-dried, as Stibene-glucoside.
Stibene-glucoside finished product is detected using high performance liquid chromatography, its purity is 99.11%.
Embodiment 4
1) fleece-flower root is crushed to 80 mesh, is 1g by solid-liquid ratio:It is that 80% ethanol is molten that 10ml ratio, which adds volumetric concentration, Liquid, refluxing extraction 3h, obtains ethanol extract at 30 DEG C;
2) ethanol extract is recovered under reduced pressure to the medicinal extract that relative density at 40 DEG C is 1.0, medicinal extract is added into its volume 15 times of water dissolving, filtering, takes filtrate standby;
3) by the upper S-8+ macroreticular resins of filtrate, loading flow velocity is 1BV/h, first distills water elution, the elution flow rate of distilled water For 5BV/h, then eluted with volumetric concentration for 50% ethanol solution, ethanol elution flow velocity is 1BV/h, collects ethanol eluate;
The S-8+ resins are polystyrene type Polar Adsorbent Resin, and quality index is as follows:
Outward appearance:The opaque spherical particle of milky;
Moisture content:66~72%;
Pore volume:0.78~0.82ml/g;
Particle size range:0.315~1.25mm >=90%;
Specific surface area:130~150 ㎡/g;
Average pore size:25~27nm;
Apparent density:0.42~0.46g/ml;
Skeletal density:1.20~1.24g/ml;
Wet apparent density:0.60~0.70g/ml;
Wet true density:1.00~1.06g/ml.
4) solvent is recovered under reduced pressure in ethanol eluate, be freeze-dried, as Stibene-glucoside.
Stibene-glucoside finished product is detected using high performance liquid chromatography, its purity is 99.02%.

Claims (5)

1. the method for Stibene-glucoside is extracted from the fleece-flower root, it is characterised in that:Comprise the following steps:
1) fleece-flower root is crushed, adds alcohol reflux extraction, obtain ethanol extract;
2) ethanol extract is recovered under reduced pressure to the medicinal extract that relative density at 40 DEG C is 1.0~1.5, medicinal extract is dissolved in water, mistake Filter, takes filtrate standby;
3) by the upper S-8+ macroreticular resins of filtrate, water elution is first distilled, then with 50% ethanol elution, collects ethanol eluate;
4) solvent is recovered under reduced pressure in ethanol eluate, be freeze-dried, as Stibene-glucoside.
2. the method according to claim 1 that Stibene-glucoside is extracted from the fleece-flower root, it is characterised in that:In step 1), Ethanol volumetric concentration is 60~80%, and the solid-liquid ratio of the fleece-flower root and ethanol is 1g:10~20ml;Refluxing extraction temperature is 30~45 DEG C, extraction time is 1~3h.
3. the method according to claim 1 that Stibene-glucoside is extracted from the fleece-flower root, it is characterised in that:In step 2), The addition of water is 10~15 times of medicinal extract volume.
4. the method according to claim 1 that Stibene-glucoside is extracted from the fleece-flower root, it is characterised in that:In step 3), Loading flow velocity is 1~3BV/h, and the elution flow rate of distilled water is 2~5BV/h, and ethanol elution flow velocity is 1~2BV/h.
5. the method according to claim 1 that Stibene-glucoside is extracted from the fleece-flower root, it is characterised in that:In step 3), The S-8+ resins are polystyrene type Polar Adsorbent Resin, and quality index is as follows:
Outward appearance:The opaque spherical particle of milky;
Moisture content:66~72%;
Pore volume:0.78~0.82ml/g;
Particle size range:0.315~1.25mm >=90%;
Specific surface area:130~150 ㎡/g;
Average pore size:25~27nm;
Apparent density:0.42~0.46g/ml;
Skeletal density:1.20~1.24g/ml;
Wet apparent density:0.60~0.70g/ml;
Wet true density:1.00~1.06g/ml.
CN201711053788.2A 2017-10-31 2017-10-31 The method that Stibene-glucoside is extracted from the fleece-flower root Pending CN107722079A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711053788.2A CN107722079A (en) 2017-10-31 2017-10-31 The method that Stibene-glucoside is extracted from the fleece-flower root

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711053788.2A CN107722079A (en) 2017-10-31 2017-10-31 The method that Stibene-glucoside is extracted from the fleece-flower root

Publications (1)

Publication Number Publication Date
CN107722079A true CN107722079A (en) 2018-02-23

Family

ID=61202616

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711053788.2A Pending CN107722079A (en) 2017-10-31 2017-10-31 The method that Stibene-glucoside is extracted from the fleece-flower root

Country Status (1)

Country Link
CN (1) CN107722079A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114736109A (en) * 2022-03-02 2022-07-12 华南理工大学 Method for selectively extracting stilbene glycoside component from Polygoni Multiflori radix

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61171427A (en) * 1985-01-24 1986-08-02 Osaka Chem Lab Substance for preventing thrombosis or the like
CN1539844A (en) * 2003-10-24 2004-10-27 广州中医药大学热带医学研究所 2,3,5,4'-tetrahydroxy diphenyl ethylene-2-1-beta-D-glucoside
CN101003554A (en) * 2006-12-26 2007-07-25 南京师范大学 Method for preparing tetrahydroxy diphenyl ethylene glycoside separated from fleece-flower root
CN101255180A (en) * 2007-02-27 2008-09-03 江苏正大天晴药业股份有限公司 Diphenyl ethylene glycosides derivatives
CN101560229A (en) * 2008-04-17 2009-10-21 霸王(广州)有限公司 Extracting method of stilbene glycoside of radix-polygoni multiflori extract
CN104945450A (en) * 2015-07-17 2015-09-30 湖南杰萃生物技术有限公司 Method for extracting stibene glucoside from vines of multiflower knotweeds

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61171427A (en) * 1985-01-24 1986-08-02 Osaka Chem Lab Substance for preventing thrombosis or the like
CN1539844A (en) * 2003-10-24 2004-10-27 广州中医药大学热带医学研究所 2,3,5,4'-tetrahydroxy diphenyl ethylene-2-1-beta-D-glucoside
CN101003554A (en) * 2006-12-26 2007-07-25 南京师范大学 Method for preparing tetrahydroxy diphenyl ethylene glycoside separated from fleece-flower root
CN101255180A (en) * 2007-02-27 2008-09-03 江苏正大天晴药业股份有限公司 Diphenyl ethylene glycosides derivatives
CN101560229A (en) * 2008-04-17 2009-10-21 霸王(广州)有限公司 Extracting method of stilbene glycoside of radix-polygoni multiflori extract
CN104945450A (en) * 2015-07-17 2015-09-30 湖南杰萃生物技术有限公司 Method for extracting stibene glucoside from vines of multiflower knotweeds

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张俊娜 等: "何首乌中二苯乙烯苷提取纯化研究进展", 《中国中医药信息杂志》 *
李从军等 主编: "《生物产品分离纯化技术》", 31 August 2009, 华中师范大学出版社 *
相聪坤 等: "大孔吸附树脂纯化何首乌中二苯乙烯苷的工艺研究", 《河北中医》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114736109A (en) * 2022-03-02 2022-07-12 华南理工大学 Method for selectively extracting stilbene glycoside component from Polygoni Multiflori radix

Similar Documents

Publication Publication Date Title
CN103467540B (en) A kind of method extracting rhodioside from Root of Kirilow Rhodiola
CN102423329B (en) A kind of discoloration method of panax notoginsenoside extract
CN102351819A (en) Extraction, purification and preparation method of high-purity salvianolic acid B
CN102746362A (en) Method for extracting refined astragaloside from astragaliradix
CN105131052A (en) Extraction method of crocin I
CN105213441B (en) Technique that is a kind of while preparing glycosides and Sweet tea total polyphenols
CN104610417B (en) A kind of method of extracting ursolic acid and oleanolic acid from hawthorn
CN103360443A (en) Method for extraction and purification of four iridoid glycosides in cornus officinalis
CN107602630A (en) The extracting method of stilbene glucoside in polygonum multiflorum
CN104610401B (en) A kind of method for extracting baicalin, baicalin and wogonin from Radix Scutellariae simultaneously
CN105053952A (en) Processing technology of dried tangerine peel extract without bitter taste
CN102228488A (en) Preparation of Lysimachia capillipes Hemsl total saponin
CN110025677B (en) Preparation method of rhubarb extract
CN107722079A (en) The method that Stibene-glucoside is extracted from the fleece-flower root
CN109021042B (en) Method for extracting high-purity oleuropein from olive leaves
CN111072736A (en) A component rich in liquiritin and glycyrrhizic acid in Glycyrrhrizae radix extract and its preparation method
CN102327325A (en) Method for preparing white mulberry rootbark general flavone
CN102670935B (en) Method for extracting total saponins from allium chinense
CN109134557A (en) The method of phloridzin is extracted from manyspike tanoak leaf piece
CN1272331C (en) Method of extracting effective components in kudzu vine root
CN101422723B (en) Extraction method of flavonoid anti-tumor active ingredient in barbat skullcap
CN108126000A (en) Arasaponin extracts preparation method in fresh Radix Notoginseng
CN103288898B (en) Neomangiferin reference substance extracts method for purifying and separating
CN106946833A (en) A kind of method that high-purity sinensetin is extracted from Mao Xu Cao
CN107582647A (en) The extracting method of fleece-flower root total anthraquinone

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
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20180223