CN105237594A - Preparation method for extracting salicin from bamboo-willow bark - Google Patents
Preparation method for extracting salicin from bamboo-willow bark Download PDFInfo
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Abstract
The invention provides a preparation method for extracting salicin from bamboo-willow bark. The method comprises the following steps: Step 1, a raw material is dried and pulverized, wherein the bark of bamboo-willow with age more than 2 years is adopted as a raw material, and is dried and pulverized; the powder is sieved with a mesh with a size of 20-40 meshes, such that bamboo-willow park powder is prepared; the powder is dried with a continuous microwave drying method under a drying temperature of 60-95 DEG C, such that bamboo-willow park powder is obtained, wherein the particle size of the powder is 20-40 meshes. The raw material adopted by the method has the advantages of low solvent consumption and low cost. The extraction separation method is simple to operate, and has low equipment requirement, such that the method is suitable for large-scale popularization. In a product 1, salicin content is stabilized at 80-85%, and a yield is approximately 2.0%.
Description
Technical field
The present invention relates to genus technical field of chemical engineering, be specifically related to a kind of extract prepared for raw material with bamboo willow bark or bamboo willow withy, and extract the preparation method of high-purity water benzasalicin from bamboo willow bark or bamboo willow withy.
Background technology
Bamboo willow is Salicaceae sallow.Arbor, growth potential is large, and height can reach more than 20 meters.Green, smooth during bark children.Apical dominance is obvious, and axillary bud sprouting power is strong, and branch is morning comparatively, side shoot and trunk angle 30-45 °.Tree crown turriform, branch is even.Leaf lanceolar, single leaf alternate, blade reaches 15-22cm, and the long gradually point of wide 3.5-6.2cm tip, base portion wedge shape, there is obvious serrulation at edge, and face of blade is green, and back side canescence, petiole is micro-red, shorter.Owing to having strong adaptability, fast-growing, cold-resistant high temperature resistant, waterlogging Salt And Alkali Tolerance, management is simple, vegetative propagation is easy, output is high, the excellent feature of material.
Saligenin is white crystals; Bitter; Fusing point 199 ~ 202 DEG C, specific rotatory power [α]-45.6 ° (0.6 gram/100 centimetres
3dehydrated alcohol); Water soluble, is soluble in boiling water, is insoluble in ethanol (1: 90), is insoluble to ether or chloroform, but can be dissolved in alkaline solution, pyridine or Glacial acetic acid.Its aqueous solution is neutral reaction, without free phenolic hydroxyl group in molecule, belongs to phenolic glycoside compounds.Through diluted acid or synaptase hydrolysis, glucose and saligenol can be generated.
Saligenin has antipyretic and analgesic activity, owing to can produce saligenol after its hydrolysis, easily oxidized and produce Whitfield's ointment, is therefore once the main source of salicylate class medicine, present pharmaceutical industry has adopted synthesis method manufacture Whitfield's ointment.
Research shows, saligenin has similar biological activity with acetylsalicylic acid (acetylsalicylic acid), but relative to acetyl salicylic glycosides, saligenin is non-stimulated to stomach, not easily causes gastrorrhagia.New research finds that it is the inhibitor of a kind of oxydase (NADHoxidase), has crease-resistant, increases skin shine and elasticity, reduce pigementation, increase skin beauty water to grade effect, for this reason, develop a kind of preparation method extracting saligenin from bamboo willow bark.
Chinese patent CN1611508A (application number is 200310105868.X) a kind of salicyl alcohol glucoside preparation technology, this invention relates to field of biological extraction, be specifically related to salicyl alcohol glucoside preparation technology.The technical solution of this invention comprises successively: get the raw materials ready, withy leaf is ground into segment raw material; Hydrolysis is extracted, and adds alkaline matter in the feed and is hydrolyzed, and then extracts with extraction agent, removes residue; Concentrated, obtain containing salicyl alcohol glucoside medicinal extract work in-process, through the salicyl alcohol glucoside that purification step obtains purity >=95%.Will consume a large amount of organic solvent in this technique extraction process, cost is higher and be unfavorable for environmental protection, and content can not reach more than 98.45%.
Summary of the invention
The invention discloses a kind of method of extraction and isolation saligenin from bamboo bark of willow, make its stability high, purification degree is high, the feature that cost is low.
The present invention is by the following technical solutions: a kind of preparation method extracting saligenin from bamboo willow bark, is completed by following steps:
Step one, raw material drying are pulverized: it is raw material that the collection age of tree is greater than 2 years bamboo bark of willow, dry, pulverize; Adopt 20-40 eye mesh screen, make bamboo bark of willow skin powder; Adopt continuous microwave drying method, drying temperature 60-95 DEG C, obtained bamboo bark of willow powder after dry, powder particle size 20 order-40 order;
Step 2, extraction and solid-liquid separation: get bamboo bark of willow powder 0.8-1.5 ton by weight, adopt the continuous extraction equipment of ultrasonic adverse current, extract under the condition of 50 DEG C-95 DEG C, centrifugal through horizontal helical type after extraction, rotating speed 2500-3000rpm, then through butterfly centrifugal, rotating speed 7000rpm, obtains after centrifugal extracting filtrate A; Solvent is adopted to be deionized water during extraction;
Step 3, macroporous resin be purifying just: by filtrate A through absorption with macroporous adsorbent resin, flow velocity 1.0-2.0BV/h, uses 30%-95% ethanol elution, elution speed 1.0-3.0BV/h, obtain elutriant B after washing;
Step 4, concentrated: elutriant B is 55 ± 5 DEG C in temperature, under pressure is 0.02-0.095MPa condition, is condensed into condensed cream C;
Step 5, separation: dissolve above-mentioned condensed cream C with the deionized water extracting raw material 2.0-2.7 times weight, add gac 1.0-5.0% insulated and stirred 1h, filtration obtains filtrate D, filtrate D n-butanol extraction 3 times, the volume ratio of organic solvent and filtrate D is 1: 1-2, merge 3 butanol extraction liquids, obtain organic phase E;
Step 6, concentrated and drying: concentrate and adopt vacuum concentration, reclaim organic solvent, temperature 60-80 DEG C, vacuum tightness 0.05-0.095MPa; Adopt vacuum decompression drying means, vacuum tightness 0.05-0.095, temperature 60-80 DEG C, crushed after being dried obtains finished product: pulverize, granularity is 80-100 order, obtains product 1, and product 1 obtains product 2 through twice recrystallization.
Further, a kind of preparation method extracting saligenin from bamboo willow bark, raw material is bamboo bark of willow or bamboo Ramulus Salicis Babylonicae.
Further, a kind of preparation method extracting saligenin from bamboo willow bark, when adopting ultrasonic adverse current to extract continuously, Extracting temperature is 60 DEG C, 70 DEG C, 75 DEG C, 80 DEG C.
Further, a kind of preparation method extracting saligenin from bamboo willow bark, the macroporous adsorbent resin that preliminary purification adopts is HPD-100, HPD-722.
The Materials Solvents consumption that the inventive method uses is little, with low cost, extraction and separation method is simple to operate, low for equipment requirements, be suitable for large-scale promotion application, in product 1, saligenin stable content is at 80-85%, and earning rate is approximately 2.0%, product 2 saligenin stable content is at 96-99%, and earning rate is approximately 1.5%.The method is that saligenin product searches out new raw material, and the low yield of cost is high, practical, is easy to suitability for industrialized production, suitable penetration and promotion application.
Embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.
Embodiment 1
From bamboo willow bark, extract a preparation method for saligenin, it is characterized in that: completed by following steps:
Step one, raw material drying are pulverized: it is raw material that the collection age of tree is greater than 2 years bamboo bark of willow, dry, pulverize, adopts 20 eye mesh screens, make bamboo bark of willow skin powder; Adopt continuous microwave drying method, drying temperature 60 DEG C, obtained bamboo bark of willow powder after dry, powder particle size 20 order;
Step 2, extraction and solid-liquid separation: get 0.8 ton, bamboo bark of willow powder by weight, adopt the continuous extraction equipment of ultrasonic adverse current, extracts under the condition of 60 DEG C, centrifugal through horizontal helical type after extraction, rotating speed 2500rpm, then through butterfly centrifugal, rotating speed 7000rpm, obtains after centrifugal extracting filtrate A; Solvent is adopted to be deionized water during extraction;
Step 3, macroporous resin be purifying just: by filtrate A through absorption with macroporous adsorbent resin, flow velocity 1.0BV/h, uses 30% ethanol elution, elution speed 2.0BV/h, obtain elutriant B after washing;
Step 4, concentrated: elutriant B is 55 ± 5 DEG C in temperature, under pressure is 0.03MPa condition, is condensed into condensed cream C;
Step 5, separation: dissolve above-mentioned condensed cream C with the deionized water extracting raw material 2.2 times of weight, add gac 1.5% insulated and stirred 1h, filtration obtains filtrate D, filtrate D n-butanol extraction 3 times, the volume ratio of organic solvent and filtrate D is 1: 1.4, merge the propyl carbinol of 3 extractions, obtain organic phase E;
Step 6, concentrated and drying: concentrate and adopt vacuum concentration, reclaim organic solvent, temperature 80 DEG C, vacuum tightness 0.09MPa; Employing vacuum decompression is dry, and vacuum tightness is 0.093MPa, temperature 78 DEG C, and crushed after being dried obtains finished product: pulverize, granularity is 80-100 order, obtains product 1, saligenin purity 85.3%, yield 2.0%, product 1 obtains product 2, purity 98.5%, yield 1.5% through twice recrystallization.
Raw material is bamboo bark of willow, and when adopting ultrasonic adverse current to extract continuously, Extracting temperature is 60 DEG C, and the macroporous adsorbent resin that preliminary purification adopts is HPD-100.
Embodiment 2
From bamboo willow bark, extract a preparation method for saligenin, completed by following steps:
Step one, raw material drying are pulverized: it is raw material that the collection age of tree is greater than 2 years bamboo bark of willow, dry, pulverize; Adopt 35 eye mesh screens, make bamboo bark of willow skin powder; Adopt continuous microwave drying method, drying temperature 75 DEG C, obtained bamboo bark of willow powder after dry, powder particle size 30 order;
Step 2, extraction and solid-liquid separation: get 1.0 tons, bamboo bark of willow powder by weight, adopt the continuous extraction equipment of ultrasonic adverse current, extracts under the condition of 75 DEG C, centrifugal through horizontal helical type after extraction, rotating speed 2800rpm, then through butterfly centrifugal, rotating speed 7000rpm, obtains after centrifugal extracting filtrate A; Solvent is adopted to be deionized water during extraction;
Step 3, macroporous resin be purifying just: by filtrate A through absorption with macroporous adsorbent resin, flow velocity 1.8BV/h, uses 35% ethanol elution, elution speed 2.0BV/h, obtain elutriant B after washing;
Step 4, concentrated: elutriant B is 55 ± 5 DEG C in temperature, under pressure is 0.06MPa condition, is condensed into condensed cream C;
Step 5, separation: dissolve above-mentioned condensed cream C with the deionized water extracting raw material 2.2 times of weight, add gac 2% insulated and stirred 1h, filters and obtain filtrate D, filtrate D n-butanol extraction 3 times, the volume ratio of organic solvent and filtrate D is 1: 1.5, merges the propyl carbinol of 3 extractions, obtains organic phase E;
Step 6, concentrated and drying: concentrate and adopt vacuum concentration, reclaim organic solvent, temperature 65 DEG C, vacuum tightness 0.090MPa; Employing vacuum decompression is dry, and vacuum tightness is 0.095MPa, temperature 60 C, and crushed after being dried obtains finished product: pulverize, granularity is 80 orders, and obtain product 1, product purity is 84.4%, and yield is 2.05%; Product 1 obtains product 2 through twice recrystallization, and purity is 97.3%, and yield is 1.48%.
Raw material is bamboo Ramulus Salicis Babylonicae, and when adopting ultrasonic adverse current to extract continuously, Extracting temperature is 70 DEG C; The macroporous adsorbent resin that preliminary purification adopts is HPD-100.
Embodiment 3
From bamboo willow bark, extract a preparation method for saligenin, completed by following steps:
Step one, raw material drying are pulverized: it is raw material that the collection age of tree is greater than 2 years bamboo bark of willow, dry, pulverize; Adopt 45 eye mesh screens, make bamboo bark of willow skin powder; Adopt continuous microwave drying method, drying temperature 85 DEG C, obtained bamboo bark of willow powder after dry, powder particle size 32 order;
Step 2, extraction and solid-liquid separation: get 1.5 tons, bamboo bark of willow powder by weight, adopt the continuous extraction equipment of ultrasonic adverse current, extracts under the condition of 75 DEG C, centrifugal through horizontal helical type after extraction, rotating speed 2750rpm, then through butterfly centrifugal, rotating speed 7000rpm, obtains after centrifugal extracting filtrate A; Solvent is adopted to be deionized water during extraction;
Step 3, macroporous resin be purifying just: by filtrate A through absorption with macroporous adsorbent resin, flow velocity 1.8BV/h, uses 65% ethanol elution, elution speed 1.8BV/h, obtain elutriant B after washing;
Step 4, concentrated: elutriant B is 55 ± 5 DEG C in temperature, under pressure is 0.07MPa condition, is condensed into condensed cream C;
Step 5, separation: dissolve above-mentioned condensed cream C with the deionized water extracting raw material 2.35 times of weight, add gac 2.5% insulated and stirred 1h, filtration obtains filtrate D, filtrate D n-butanol extraction 3 times, the volume ratio of organic solvent and filtrate D is 1: 1.5, merge the propyl carbinol of 3 extractions, obtain organic phase E;
Step 6, concentrated and drying: concentrate and adopt vacuum concentration, reclaim organic solvent, temperature 75 DEG C, vacuum tightness 0.075MPa; Employing vacuum decompression is dry, and vacuum tightness is 0.85MPa, temperature 80 DEG C, and crushed after being dried obtains finished product: pulverize, granularity is 90 orders, and obtain product 1, product purity is 83.6%, yield 2.12%; Product 1 obtains product 2 through twice recrystallization, and product purity is 96.2%, and yield is 1.53%.
Raw material is bamboo Ramulus Salicis Babylonicae; When adopting ultrasonic adverse current to extract continuously, Extracting temperature is 75 DEG C; The macroporous adsorbent resin that preliminary purification adopts is HPD-722.
Embodiment 4
From bamboo willow bark, extract a preparation method for saligenin, completed by following steps:
Step one, raw material drying are pulverized: it is raw material that the collection age of tree is greater than 2 years bamboo bark of willow, dry, pulverize; Adopt 55 eye mesh screens, make bamboo bark of willow skin powder; Adopt continuous microwave drying method, drying temperature 95 DEG C, obtained bamboo bark of willow powder after dry, powder particle size 40 order;
Step 2, extraction and solid-liquid separation: get 1.5 tons, bamboo bark of willow powder by weight, adopt the continuous extraction equipment of ultrasonic adverse current, extracts under the condition of 95 DEG C, centrifugal through horizontal helical type after extraction, rotating speed 3000rpm, then through butterfly centrifugal, rotating speed 7000rpm, obtains after centrifugal extracting filtrate A; Solvent is adopted to be deionized water during extraction;
Step 3, macroporous resin be purifying just: by filtrate A through absorption with macroporous adsorbent resin, flow velocity 2.0BV/h, uses 95% ethanol elution, elution speed 3.0BV/h, obtain elutriant B after washing;
Step 4, concentrated: elutriant B is 55 ± 5 DEG C in temperature, under pressure is 0.095MPa condition, is condensed into condensed cream C;
Step 5, separation: dissolve above-mentioned condensed cream C with the deionized water extracting raw material 2.7 times of weight, add gac 5.0% insulated and stirred 1h, filters and obtain filtrate D, filtrate D n-butanol extraction 3 times, the volume ratio of organic solvent and filtrate D is 1: 2, merges the propyl carbinol of 3 extractions, obtains organic phase E;
Step 6, concentrated and drying: concentrate and adopt vacuum concentration, reclaim organic solvent, temperature 80 DEG C, vacuum tightness 0.090MPa; Employing vacuum tightness is 0.095MPa, temperature 75 DEG C, and crushed after being dried obtains finished product; Pulverize, granularity is 100 orders, and obtain product 1, product purity is 82%, and yield is 2.40%; Product 1 obtains product 2 through twice recrystallization, and purity is 96.5%, and yield is 1.48%.
Raw material is bamboo bark of willow, and when adopting ultrasonic adverse current to extract continuously, Extracting temperature is 80 DEG C; The macroporous adsorbent resin that preliminary purification adopts is HPD-722.
Part not in the detailed description of the invention is known technology, and the usual change that those skilled in the art carries out within the scope of technical solution of the present invention or replacement all should be included in protection scope of the present invention.
Claims (4)
1. from bamboo willow bark, extract a preparation method for saligenin, it is characterized in that: completed by following steps:
Step one, raw material drying are pulverized: it is raw material that the collection age of tree is greater than 2 years bamboo bark of willow, dry, pulverize; Adopt 20-40 eye mesh screen, make bamboo bark of willow skin powder; Adopt continuous microwave drying method, drying temperature 60-95 DEG C, obtained bamboo bark of willow powder after dry, powder particle size 20 order-40 order;
Step 2, extraction and solid-liquid separation: get bamboo bark of willow powder 0.8-1.5 ton by weight, adopt the continuous extraction equipment of ultrasonic adverse current, extract under the condition of 50 DEG C-95 DEG C, centrifugal through horizontal helical type after extraction, rotating speed 2500-3000rpm, then through butterfly centrifugal, rotating speed 7000rpm, obtains after centrifugal extracting filtrate A; Solvent is adopted to be deionized water during extraction;
Step 3, macroporous resin be purifying just: by filtrate A through absorption with macroporous adsorbent resin, flow velocity 1.0-2.0BV/h, uses 30%-95% ethanol elution, elution speed 1.0-3.0BV/h, obtain elutriant B after washing;
Step 4, concentrated: elutriant B is 55 ± 5 DEG C in temperature, under pressure is 0.02-0.095MPa condition, is condensed into condensed cream C;
Step 5, separation: dissolve above-mentioned condensed cream C with the deionized water extracting raw material 2.0-2.7 times weight, add gac 1.0-5.0% insulated and stirred 1h, filtration obtains filtrate D, filtrate D n-butanol extraction 3 times, the volume ratio of organic solvent and filtrate D is 1: 1-2, merge 3 butanol extraction liquids, obtain organic phase E;
Step 6, concentrated and drying: concentrate and adopt vacuum concentration, reclaim organic solvent, temperature 60-80 DEG C, vacuum tightness 0.05-0.095MPa; Adopt vacuum decompression drying means, vacuum tightness 0.05-0.095, temperature 60-80 DEG C, crushed after being dried obtains finished product: pulverize, granularity is 80-100 order, obtains product 1, and product 1 obtains product 2 through twice recrystallization.
2. a kind of preparation method extracting saligenin from bamboo willow bark according to claim 1, is characterized in that: raw material is bamboo bark of willow or bamboo Ramulus Salicis Babylonicae.
3. a kind of preparation method extracting saligenin from bamboo willow bark according to claim 1, is characterized in that: when adopting ultrasonic adverse current to extract continuously, Extracting temperature is 60 DEG C, 70 DEG C, 75 DEG C, 80 DEG C.
4. a kind of preparation method extracting saligenin from bamboo willow bark according to claim 1, is characterized in that: the macroporous adsorbent resin that preliminary purification adopts is HPD-100, HPD-722.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106317137A (en) * | 2016-08-19 | 2017-01-11 | 陕西佰瑞生物化工有限责任公司 | Process for processing byproducts of salicin production using Salix babylonica L. bark |
| CN106728252A (en) * | 2016-12-05 | 2017-05-31 | 山东省科学院生物研究所 | A kind of water extraction preparation method and application of bamboo willow antibacterial active constituents |
| CN106728251A (en) * | 2016-12-05 | 2017-05-31 | 山东省科学院生物研究所 | A kind of preparation method and application of bamboo willow antifungal activity component |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102863483A (en) * | 2012-10-12 | 2013-01-09 | 成都乾坤动物药业有限公司 | Preparation process of salicin comparison product |
-
2015
- 2015-10-28 CN CN201510715569.0A patent/CN105237594A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102863483A (en) * | 2012-10-12 | 2013-01-09 | 成都乾坤动物药业有限公司 | Preparation process of salicin comparison product |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106317137A (en) * | 2016-08-19 | 2017-01-11 | 陕西佰瑞生物化工有限责任公司 | Process for processing byproducts of salicin production using Salix babylonica L. bark |
| CN106728252A (en) * | 2016-12-05 | 2017-05-31 | 山东省科学院生物研究所 | A kind of water extraction preparation method and application of bamboo willow antibacterial active constituents |
| CN106728251A (en) * | 2016-12-05 | 2017-05-31 | 山东省科学院生物研究所 | A kind of preparation method and application of bamboo willow antifungal activity component |
| CN106728252B (en) * | 2016-12-05 | 2020-01-17 | 山东省科学院生物研究所 | Water extraction preparation method and application of bamboo willow antibacterial active component |
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Application publication date: 20160113 |