CN104231014A - Method for extracting salicin by virtue of supercritical CO2 - Google Patents
Method for extracting salicin by virtue of supercritical CO2 Download PDFInfo
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- CN104231014A CN104231014A CN201410450524.0A CN201410450524A CN104231014A CN 104231014 A CN104231014 A CN 104231014A CN 201410450524 A CN201410450524 A CN 201410450524A CN 104231014 A CN104231014 A CN 104231014A
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- extraction
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- crude product
- ethanol
- salicin
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for extracting salicin by virtue of supercritical CO2. The method comprises the following steps: soaking tamarisk twig powder in an ethanol solution, extracting by taking supercritical CO2 as an extractant and ethanol as an entrainer in an extraction kettle, analyzing extract, and drying to obtain a crude product; and dissolving the crude product by using alkali liquid, adding chloroform for extraction, and performing reduced pressure concentration on an alkali liquid layer to obtain pure salicin. Obtained salicin is extracted by virtue of supercritical CO2 and is good in quality and high in purity; the whole method is short in operating time, simple in process and suitable for large-scale production.
Description
Technical field
The invention belongs to field of natural product extraction, relate to one and utilize supercritical CO
2the method of extraction water benzasalicin.
Background technology
Saligenin English name Salicin, No. CAS is 138-52-3, molecular formula C
13h
18o
7, molecular weight 286.28.Salicyl alcohol glucoside salicin 15%, 20%, 30% is yellow powder, and more than 90% is white powder, and fusing point 199 ~ 202 DEG C, is dissolved in alkaline solution, pyridine and Glacial acetic acid, is insoluble to ether, chloroform.Saligenin have antipyretic, analgesia and the effect such as anti-inflammatory, rheumatism, there is stomach invigorating and toponarcosis effect in addition, also can be used as biochemical reagents.
As " natural Asprin ", salicyl alcohol glucoside is used to treat slight heating, flu, infection (influenza), acute and chronic rheumatoid is uncomfortable, headache and the pain that causes because of inflammation.Asprin (acetylsalicylic acid), as salicyl alcohol glucoside synthesis substitute, have potential in stomach and intestine dangerous side-effects.As its native configurations, salicyl alcohol glucoside harmlessly can pass through gastrointestinal system, in blood and liver, be converted into Whitfield's ointment.Conversion process needs a few hours, and therefore result can not be arrived by human body sensory immediately, but general effect can continue a few hours.
Salicyl alcohol glucoside is considered to salicis,cortex anti-inflammation and the source of the ability that eases the pain, the pain relieving ability of salicis,cortex comes into force comparatively slow but longer than the time of common Asprin product lasts usually, single test find a class contain 100mg salicyl alcohol glucoside herbal combinations goods taking the pain relieving ability that can effectively improve after two months arthritic continuously, another test finds that taking in 1360mg Salix Babylonica L.P.E every day wherein can have better effect to treatment joint part pain and sacroiliitis containing after 240mg salicyl alcohol glucoside fortnight, high dosage Salix Babylonica L.P.E is used may also to contribute to alleviating lumbar and back pain, the test once continuing for four weeks find containing 240mg salicyl alcohol glucoside Salix Babylonica L.P.E effectively can alleviate the deterioration of lumbar and back pain.
Existing saligenin production technique is completed by operations such as alcohol extracting, extraction, chromatography, crystallizations, and the method pollution is heavy, finished product purity is low, is not suitable for suitability for industrialized production.
Summary of the invention
One is the object of the present invention is to provide to utilize supercritical CO
2the method of extraction water benzasalicin.
The present invention is achieved by the following technical solutions:
One utilizes supercritical CO
2the method of extraction water benzasalicin, is characterized in that: Chinese Tamarisk Twig 4-6 times amount ethanolic soln is infiltrated 0.5-2h to it, puts into extraction kettle, with postcritical CO
2for extraction agent, ethanol is that entrainment agent extracts, and then resolves extract, and dry, obtain crude product, crude product alkali lye dissolves, and adds chloroform extraction, and alkali lye layer concentrating under reduced pressure obtains saligenin sterling.
Described extracting pressure 20-50MPa, temperature are 35-60 DEG C, extraction time is 2-5 hour, parsing pressure is 4-10MPa, resolution temperature 20-40 DEG C, CO
2flow is 0.3-0.5L/min, the flow velocity of entrainment agent ethanol is 1-8ml/min.
The ammonia soln of described alkali lye to be pH be 9.5-11.
Present method adopts supercritical CO
2extraction, avoid the impact of high temperature on effective constituent during treatment capacity Datong District, the method is simple to operate, security is high, overcome in traditional technology pollute heavy, produce the pure shortcoming such as low, be applicable to scale operation.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
Get 1kg twig and leaf of Juniper Tamarisk to pulverize, add 5kg ethanol and infiltrate 0.5h, put into extraction kettle, with postcritical CO
2for extraction agent, ethanol is that entrainment agent extracts, extracting pressure 20MPa, temperature 35 DEG C, extraction 2h, CO
2flow is 0.3L/min, and ethanol flow velocity is 1ml/min, resolves pressure 4MPa, resolution temperature 20 DEG C, and extraction liquid is dry, and obtain crude product, crude product ammonia soln dissolves, and add equal amounts of chloroform extraction, alkali lye layer concentrating under reduced pressure obtains saligenin sterling, content 91.3%.
Embodiment 2:
Get 5kg twig and leaf of Juniper Tamarisk to pulverize, add 30kg ethanol and infiltrate 2h, put into extraction kettle, with postcritical CO
2for extraction agent, ethanol is that entrainment agent extracts, extracting pressure 50MPa, temperature 60 C, extraction 5h, CO
2flow is 0.5L/min, and ethanol flow velocity is 8ml/min, resolves pressure 10MPa, resolution temperature 40 DEG C, and extraction liquid is dry, and obtain crude product, crude product ammonia soln dissolves, and add equal amounts of chloroform extraction, alkali lye layer concentrating under reduced pressure obtains saligenin sterling, content 92.5%.
Embodiment 3:
Get 1kg twig and leaf of Juniper Tamarisk to pulverize, add 4kg ethanol and infiltrate 1.3h, put into extraction kettle, with postcritical CO
2for extraction agent, ethanol is that entrainment agent extracts, extracting pressure 35MPa, temperature 48 DEG C, extraction 3.5h, CO
2flow is 0.4L/min, and ethanol flow velocity is 4ml/min, resolves pressure 7MPa, resolution temperature 30 DEG C, and extraction liquid is dry, and obtain crude product, crude product ammonia soln dissolves, and add equal amounts of chloroform extraction, alkali lye layer concentrating under reduced pressure obtains saligenin sterling, content 90.8%.
Claims (3)
1. one kind utilizes supercritical CO
2the method of extraction water benzasalicin, is characterized in that comprising the steps: Chinese Tamarisk Twig 4-6 times amount ethanolic soln to infiltrate 0.5-2h to it, puts into extraction kettle, with postcritical CO
2for extraction agent, ethanol is that entrainment agent extracts, and then resolves extract, and dry, obtain crude product, crude product alkali lye dissolves, and adds chloroform extraction, and alkali lye layer concentrating under reduced pressure obtains saligenin sterling.
2. one utilizes supercritical CO as claimed in claim 1
2the method of extraction water benzasalicin, is characterized in that, extracting pressure 20-50MPa, temperature are 35-60 DEG C, extraction time is 2-5min, parsing pressure is 4-10MPa, resolution temperature 20-40 DEG C, CO
2flow is 0.3-0.5L/min, the flow velocity of entrainment agent ethanol is 1-8ml/min.
3. one utilizes supercritical CO as claimed in claim 1
2the method of extraction water benzasalicin, is characterized in that, the ammonia soln of alkali lye to be pH be 9.5-11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410450524.0A CN104231014A (en) | 2014-09-05 | 2014-09-05 | Method for extracting salicin by virtue of supercritical CO2 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410450524.0A CN104231014A (en) | 2014-09-05 | 2014-09-05 | Method for extracting salicin by virtue of supercritical CO2 |
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| Publication Number | Publication Date |
|---|---|
| CN104231014A true CN104231014A (en) | 2014-12-24 |
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|---|---|---|---|
| CN201410450524.0A Pending CN104231014A (en) | 2014-09-05 | 2014-09-05 | Method for extracting salicin by virtue of supercritical CO2 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910110A (en) * | 2015-05-28 | 2015-09-16 | 南京泽朗生物科技有限公司 | Aeginetolide preparation method |
| CN105461766A (en) * | 2015-12-18 | 2016-04-06 | 陕西嘉禾生物科技股份有限公司 | Method for extracting salicin from white willow bark |
-
2014
- 2014-09-05 CN CN201410450524.0A patent/CN104231014A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910110A (en) * | 2015-05-28 | 2015-09-16 | 南京泽朗生物科技有限公司 | Aeginetolide preparation method |
| CN105461766A (en) * | 2015-12-18 | 2016-04-06 | 陕西嘉禾生物科技股份有限公司 | Method for extracting salicin from white willow bark |
| CN105461766B (en) * | 2015-12-18 | 2018-12-21 | 陕西嘉禾生物科技股份有限公司 | A method of extracting salicin from salicis,cortex |
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Application publication date: 20141224 |