CN1554663A - Process for extracting and separating salicin from fresh hranch of red willow - Google Patents
Process for extracting and separating salicin from fresh hranch of red willow Download PDFInfo
- Publication number
- CN1554663A CN1554663A CNA2003101222129A CN200310122212A CN1554663A CN 1554663 A CN1554663 A CN 1554663A CN A2003101222129 A CNA2003101222129 A CN A2003101222129A CN 200310122212 A CN200310122212 A CN 200310122212A CN 1554663 A CN1554663 A CN 1554663A
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- crystallization
- salicyl alcohol
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- alcohol glucoside
- ethanol
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Abstract
The process of extracting and separating salicin from fresh branch of red willow material includes crushing the material, mixing with lime via stirring, letting stand for 30 min, thrice ethanol extraction, recovering ethanol to obtain dilute extractum, diluting with water and filtering to obtain filtrate, elution in macroporous resin, merging effluent and water washing liquid, concentration to crystallize, re-crystallize, suction filtering and vacuum drying. The present invention has simple technological process, low cost, high yield and less 'three waste', and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of from plant the method for extraction separation compound, especially relate to a kind of from the bright branch of purple osier the extraction separation salicyl alcohol glucoside method.
Background technology
Along with the purposes of natural product is increasingly extensive, increasing natural product is paid attention to by domestic and international research institution.Salicyl alcohol glucoside has advantageous advantage the beauty treatment aspect, skin metabolism be can promote, skin skin matter, the colour of skin and smoothness improved, be rich in addition salicyl alcohol glucoside plant milk extract also be much accounted of day by day aspect the fat-reducing with other extract acting in conjunction, to salicyl alcohol glucoside the research of pharmacology aspect more, but report seldom, and several nothings reports over nearly 20 years for the extraction separation aspect.According to studies show that, all contain salicyl alcohol glucoside in the various plants, but how to find a plant that content is high, and can with simple production technology can extraction separation obtain pure salicyl alcohol glucoside the suitability for industrialized production aspect do not appear in the newspapers.
Summary of the invention
The objective of the invention is for overcoming disadvantages of background technology, and provide a kind of from the bright branch of purple osier the extraction separation salicyl alcohol glucoside method.This method is simple and efficient, and by this method extraction separation salicyl alcohol glucoside cost low, productive rate is high.
For achieving the above object, the technical solution used in the present invention is:
The present invention is a raw material with the bright branch of dungarunga purple osier, this raw material powder is broken into 10～20 orders, admix weight percent and be 5～10% unslaked lime, back placement 30 minutes stirs, use 75～85% extraction using alcohols three times then, reclaiming ethanol, to obtain proportion be rare medicinal extract of 1.10～1.15, add 3～4 times of water dilution after-filtration, macroporous adsorbent resin will be gone on the clear liquid, merge effluent liquid and water lotion, being concentrated into proportion is that crystallization is placed in 1.02～1.05 backs, then coarse crystallization is carried out recrystallization again, promptly obtains the salicyl alcohol glucoside crystallization after suction filtration, the vacuum-drying.
Described recrystallization is meant 90～95% ethanol that add 8～12 times of amounts in coarse crystallization, adds 8～12% gac again and carries out reflux decolour, and filtered while hot is placed crystallization.
The present invention compared with prior art has the following advantages: technical process of the present invention is simple, and extraction separation salicyl alcohol glucoside cost is low, productive rate is high, and the little and easy processing of " three wastes " treatment capacity is fit to the suitability for industrialized production salicyl alcohol glucoside.
Embodiment
Embodiment 1
1, the bright branch of the purple osier of gathering is ground into powder about 10 orders, admixes weight percent and be 5% unslaked lime and mix the back thoroughly and placed 30 minutes
2, the raw material of mixing was used 85% alcohol reflux 1 hour for the first time, the alcohol reflux of second and third time usefulness 80%, united extraction liquid, and concentrating under reduced pressure to become proportion be rare medicinal extract of 1.10.
3, this rare medicinal extract is added the dilution of 3 times of water, leave standstill 30 minutes after, filter, go into the D101 macroporous adsorbent resin on the filtrate
4, collect effluent liquid and water lotion, and to be evaporated to proportion be 1.02, needle crystal is promptly arranged after the placement.
5, with behind the crystallization suction filtration, obtain coarse crystallization, again with it 90% ethanol with 10 times of amounts, add 10% gac again and carry out reflux decolour, filtered while hot is placed crystallization, suction filtration, and vacuum-drying promptly gets the salicyl alcohol glucoside crystallization.
Embodiment 2
1, the bright branch of the purple osier of gathering is ground into powder about 15 orders, admixes weight percent and be 8% unslaked lime and mix the back thoroughly and placed 30 minutes
2, the raw material of mixing was used 83% alcohol reflux 1 hour for the first time, the alcohol reflux of second and third time usefulness 78%, united extraction liquid, and concentrating under reduced pressure to become proportion be rare medicinal extract of 1.12.
3, this rare medicinal extract is added the dilution of 3.5 times of water, leave standstill 30 minutes after, filter, go into the D101 macroporous adsorbent resin on the filtrate
4, collect effluent liquid and water lotion, and to be evaporated to proportion be 1.03, needle crystal is promptly arranged after the placement.
5, with behind the crystallization suction filtration, obtain coarse crystallization, again with it 92% ethanol with 8 times of amounts, add 8% gac again and carry out reflux decolour, filtered while hot is placed crystallization, suction filtration, and vacuum-drying promptly gets the salicyl alcohol glucoside crystallization.
Embodiment 3
1, the bright branch of the purple osier of gathering is ground into powder about 20 orders, admixes weight percent and be 10% unslaked lime and mix the back thoroughly and placed 30 minutes
2, the raw material of mixing was used 80% alcohol reflux 1 hour for the first time, the alcohol reflux of second and third time usefulness 75%, united extraction liquid, and concentrating under reduced pressure to become proportion be rare medicinal extract of 1.15.
3, this rare medicinal extract is added the dilution of 4 times of water, leave standstill 30 minutes after, filter, go into the D101 macroporous adsorbent resin on the filtrate
4, collect effluent liquid and water lotion, and to be evaporated to proportion be 1.05, needle crystal is promptly arranged after the placement.
5, with behind the crystallization suction filtration, obtain coarse crystallization, again with it 95% ethanol with 12 times of amounts, add 12% gac again and carry out reflux decolour, filtered while hot is placed crystallization, suction filtration, and vacuum-drying promptly gets the salicyl alcohol glucoside crystallization.
Claims (2)
1, a kind of from the bright branch of purple osier the extraction separation salicyl alcohol glucoside method, with the bright branch of dungarunga purple osier is raw material, it is characterized in that: this raw material powder is broken into 10～20 orders, admix weight percent and be 5～10% unslaked lime, back placement 30 minutes stirs, use 75～85% extraction using alcohols three times then, reclaiming ethanol, to obtain proportion be rare medicinal extract of 1.10～1.15, add 3～4 times of water dilution after-filtration, to go into macroporous adsorbent resin on the clear liquid, merge effluent liquid and water lotion, being concentrated into proportion is that crystallization is placed in 1.02～1.05 backs, then coarse crystallization is carried out recrystallization, suction filtration again, promptly obtain the salicyl alcohol glucoside crystallization after the vacuum-drying.
2, according to claim 1 a kind of from the bright branch of purple osier the extraction separation salicyl alcohol glucoside method, it is characterized in that: described recrystallization is meant 90～95% ethanol that add 8～12 times of amounts in coarse crystallization, add 8～12% gac again and carry out reflux decolour, filtered while hot is placed crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101222129A CN1554663A (en) | 2003-12-29 | 2003-12-29 | Process for extracting and separating salicin from fresh hranch of red willow |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101222129A CN1554663A (en) | 2003-12-29 | 2003-12-29 | Process for extracting and separating salicin from fresh hranch of red willow |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1554663A true CN1554663A (en) | 2004-12-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2003101222129A Pending CN1554663A (en) | 2003-12-29 | 2003-12-29 | Process for extracting and separating salicin from fresh hranch of red willow |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1554663A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079764A (en) * | 2009-12-01 | 2011-06-01 | 汉中秦赢生物科技有限责任公司 | Method for preparing medicinal raw material salicin from white willow branch bark |
| CN101217969B (en) * | 2005-07-14 | 2011-09-28 | 因德纳有限公司 | Salix extract, its use and formulations containing it |
| CN102453061A (en) * | 2010-11-03 | 2012-05-16 | 张守力 | Method for extracting salicin |
| CN102558254A (en) * | 2010-12-30 | 2012-07-11 | 成都华高药业有限公司 | Extract of willow barks or willow branches and method for preparing salicin |
| CN102731587A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting salicin from white willow bark |
| CN106279302A (en) * | 2016-08-18 | 2017-01-04 | 三原金瑞生物工程有限公司 | The method extracting salicoside from Willow bark and the extract obtained |
| CN106957346A (en) * | 2017-01-12 | 2017-07-18 | 南阳理工学院 | The method that salicin is produced using diversiform-leaved poplar leaf |
| CN107488202A (en) * | 2017-07-21 | 2017-12-19 | 安徽龙津生物科技有限公司 | The extracting method in high yield of salicoside in a kind of white willow branches and leaves |
| CN108084235A (en) * | 2018-01-25 | 2018-05-29 | 四川紫灵生物科技有限公司 | A kind of extract of willow bark and preparation method thereof |
| CN109369740A (en) * | 2018-12-24 | 2019-02-22 | 雅安太时生物科技股份有限公司 | A method of using salicoside produce in by-product preparation crystallization salicoside |
| CN111647025A (en) * | 2020-06-18 | 2020-09-11 | 甘肃天顺植物科技有限公司 | Method for extracting, separating and refining salicin from willow |
-
2003
- 2003-12-29 CN CNA2003101222129A patent/CN1554663A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101217969B (en) * | 2005-07-14 | 2011-09-28 | 因德纳有限公司 | Salix extract, its use and formulations containing it |
| CN102079764A (en) * | 2009-12-01 | 2011-06-01 | 汉中秦赢生物科技有限责任公司 | Method for preparing medicinal raw material salicin from white willow branch bark |
| CN102079764B (en) * | 2009-12-01 | 2013-04-17 | 汉中秦赢生物科技有限责任公司 | Method for preparing medicinal raw material salicin from white willow branch bark |
| CN102453061A (en) * | 2010-11-03 | 2012-05-16 | 张守力 | Method for extracting salicin |
| CN102453061B (en) * | 2010-11-03 | 2014-09-10 | 张守力 | Method for extracting salicin |
| CN102558254B (en) * | 2010-12-30 | 2015-05-20 | 成都华高药业有限公司 | Extract of willow barks or willow branches and method for preparing salicin |
| CN102558254A (en) * | 2010-12-30 | 2012-07-11 | 成都华高药业有限公司 | Extract of willow barks or willow branches and method for preparing salicin |
| CN102731587A (en) * | 2011-12-25 | 2012-10-17 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting salicin from white willow bark |
| CN102731587B (en) * | 2011-12-25 | 2015-04-22 | 大兴安岭林格贝有机食品有限责任公司 | Method for extracting salicin from white willow bark |
| CN106279302A (en) * | 2016-08-18 | 2017-01-04 | 三原金瑞生物工程有限公司 | The method extracting salicoside from Willow bark and the extract obtained |
| CN106957346A (en) * | 2017-01-12 | 2017-07-18 | 南阳理工学院 | The method that salicin is produced using diversiform-leaved poplar leaf |
| CN107488202A (en) * | 2017-07-21 | 2017-12-19 | 安徽龙津生物科技有限公司 | The extracting method in high yield of salicoside in a kind of white willow branches and leaves |
| CN108084235A (en) * | 2018-01-25 | 2018-05-29 | 四川紫灵生物科技有限公司 | A kind of extract of willow bark and preparation method thereof |
| CN109369740A (en) * | 2018-12-24 | 2019-02-22 | 雅安太时生物科技股份有限公司 | A method of using salicoside produce in by-product preparation crystallization salicoside |
| CN111647025A (en) * | 2020-06-18 | 2020-09-11 | 甘肃天顺植物科技有限公司 | Method for extracting, separating and refining salicin from willow |
| CN111647025B (en) * | 2020-06-18 | 2023-05-02 | 甘肃天顺植物科技有限公司 | Method for extracting, separating and refining salicin from willow |
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