CN108299298A - A kind of method of norisoboldine high efficiency extraction - Google Patents
A kind of method of norisoboldine high efficiency extraction Download PDFInfo
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D221/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00
- C07D221/02—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00 condensed with carbocyclic rings or ring systems
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Abstract
A kind of method of norisoboldine high efficiency extraction belongs to plant chemical ingredient extraction and separation technology field.It is comprised the following steps that：（1）Supercritical CO2Degreasing；（2）Ionic liquid aqueous solution extracts；（3）Organic solvent extracts.This method is a kind of new process prepared by norisoboldine ingredient high efficiency extraction, and gained norisoboldine recovery rate is high, purity quality is higher, and ionic liquid can recycle, easy to operate, and technique is environmentally protective, has good popularizing application prospect.
Description
Technical field
The invention belongs to plant chemical ingredient extraction and separation technology fields, go first different more particularly to a kind of high efficiency extraction
The method of boldine.
Background technology
Norisoboldine belongs to benzyl isoquinoline alkaloid, it is one of the main pharmacodynamics ingredient in the Chinese medicine root of three-nerved spicebush,
Studies have shown that norisoboldine there are many pharmacological activity, there is fine curative effect especially for arthritis.Remove the different wave of first
You determine its entitled 1,9- dihydroxy -2,10- dimethoxy glaucine of chemistry, English name Norisoboldine, and molecular formula is
C18H19NO4, molecular weight 313.35, structural formula is as follows：
There are also the patented methods that other extract separation norisoboldines, such as publication date to be September in 2013 25, publication number
For the Chinese patent of 102399186 B of CN, a kind of isolation and purification method of norisoboldine monomer, this method packet are disclosed
Containing following steps：A is extracted：The root of three-nerved spicebush is ground into coarse powder, equivalent extract is extracted to obtain with alcohol reflux；B is extracted：Equivalent extract is with chloroform
Extract to obtain norisoboldine crude product；C is crystallized：With organic solvent solvent crude product, purity >=98% is obtained after filtering, drying
Norisoboldine monomer product.This method is mainly using there is traditional ethyl alcohol solvent extraction, and there are Extraction solvent selections
Property not strong, the problems such as impurity is more and extraction efficiency is not high.
For another example publication date is on May 02nd, 2012, and the Chinese patent of 102432534 A of Publication No. CN discloses one
The method that kind extracts norisoboldine from radix linderae, this method comprise the following steps：Radix linderae is taken, crushes, is added to CO2
In supercritical extract device, for ethyl acetate as entrainer, the percent by volume that entrainer accounts for total extractant is 2-5%, extraction
Pressure 30-40MPa, 50-60 DEG C of temperature, CO2Flow 2-4ml/g crude drug min, extraction time 80-120min must be extracted
Object is added on large pore resin absorption column and adsorbs, 50-70% ethanol elutions, collects 3-8 times and measures column volume eluent, depressurizes back
It receives ethyl alcohol and concentrates, be added on silica gel column chromatography, with ratio for 4：1 dichloromethane-methanol mixed solvent elution, eluent
It is collected by column volume portioning, merges 5-9 parts of eluent, solvent is recovered under reduced pressure and concentrates, acetone crystallization, separation knot is added
Crystalline substance is washed, is drying to obtain.Our experimental study shows that CO is used alone2First cannot be extracted away as supercritical extract agent
Isoboldine, CO in the method2Supercritical extract adds ethyl acetate as entrainer, increases to a certain degree super
Critical fluids extraction scope also increases the impurity content of non-norisoboldine ingredient, there is also extraction efficiencies not high, impurity
More problem；Subsequently use the general skill of routine that macroporous absorbent resin and layer of silica gel column chromatography purify for plant chemical ingredient
Art.
Invention content
In view of the problems of the existing technology, it is an object of the invention to design to provide a kind of use in conjunction supercritical CO2
Extraction and ionic liquid selective extraction prepare the technical method of norisoboldine.It is raw material that this method, which chooses root of three-nerved spicebush root tuber,
Supercritical CO is used first2The liposoluble constituent in the root of three-nerved spicebush is removed, suitable ionic liquid extract preparation is then selected to go first different
Boldine.The method overcome previous methods recovery rates it is relatively low, extract impurity is more the problems such as, this method have efficiently, letter
It is single, environmentally protective, cost is relatively low, is suitble to the advantages of certain scale metaplasia production.
The method of a kind of norisoboldine high efficiency extraction, it is characterised in that comprise the following steps that：
（1）Degreasing：The root of three-nerved spicebush root tuber powder to have pulverized and sieved is put into supercritical CO2Supercritical CO is carried out in extraction equipment2Extraction
It takes, obtains root of three-nerved spicebush extract remainder after extraction from extraction equipment, extract is obtained from separating still receiving bottle；
（2）Extraction：It will the above overcritical object CO2Ionic liquid aqueous solution is added in root of three-nerved spicebush extract remainder, and ultrasound assisted extraction is carried
Take liquid, extracting solution that filtrate and solid material is obtained by filtration；
（3）Extraction：Organic solvent extraction is added in ionic liquid extract filtrate, stratification obtains upper organic phase extract liquor
With lower layer's aqueous, upper layer organic extract liquid is concentrated under reduced pressure to get norisoboldine.
A kind of method of high efficiency extraction norisoboldine, it is characterised in that the step（1）In it is overcritical
CO2Extraction conditions is：Temperature is 40~60 DEG C, and pressure is 20~30MPa, and the static retention time is 30~60 minutes, is dynamically carried
It is 30~120 minutes to take the time.
A kind of method of high efficiency extraction norisoboldine, it is characterised in that the step（2）Described in
Ionic liquid aqueous solution intermediate ion liquid is 1- butyl -3- methylimidazole bromides, and ion concentration is 0.25~2.5mol/L, the root of three-nerved spicebush
Extract remainder is 1: 10~100 with ionic liquid aqueous solution mass volume ratio, and ultrasound assisted extraction condition is：Extraction time be 15~
120 minutes；300~500W of ultrasonic power.
A kind of method of high efficiency extraction norisoboldine, it is characterised in that the step（3）In it is organic molten
Agent is ethyl acetate or n-butanol.
A kind of method of high efficiency extraction norisoboldine, it is characterised in that the step（3）Middle lower layer's extraction
Extraction raffinate is diluted with water to debita spissitudo, is continuing with removing upper layer residual organic solvents are concentrated under reduced pressure；Or by lower layer's raffinate
Liquid reduced pressure completely removes water and organic solvent, after dry, obtains recycling ionic liquid, is preserved in dry environment, afterwards
It is recycled in extraction separation.
According to the method for the present invention, supercritical CO is utilized2The liposoluble constituent in root of three-nerved spicebush root tuber is removed, and is taken full advantage of
Ionic liquid designability has filtered out ionic liquid 1-butyl-3-methyl imidazolium bromide and has removed the different bohr of first for high efficiency extraction
It is fixed.It, should compared with the yield that used methanol in 2015 editions pharmacopeia-hydrochloric acid reflux method extracts root of three-nerved spicebush norisoboldine
Norisoboldine obtained by method can reach 100% or more with respect to recovery rate, while purity is more than 70%, can greatly simplify follow-up
Purification process step is conducive to large-scale production；Meanwhile ionic liquid used can be recycled again by appropriate method.It should
Method is a kind of new process prepared by norisoboldine ingredient high efficiency extraction, gained norisoboldine recovery rate height, purity
Quality is higher, and ionic liquid can recycle, easy to operate, and technique is environmentally protective, has good popularizing application prospect.
Description of the drawings
Fig. 1 is the HPLC collection of illustrative plates of 1 norisoboldine of the embodiment of the present invention；12.1 minutes chromatographic peaks of retention time are
Norisoboldine.
Specific implementation mode
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
The preparation method of the root of three-nerved spicebush root tuber powder is：Root of three-nerved spicebush root tuber raw material used first dehydrate to moisture 10% with
Under, it crushes crusher machine and crosses 20 mesh with upper screen cloth, after gained powder-tight, store in a dry environment.
Experiment use analyze root of three-nerved spicebush extracting solution in norisoboldine liquid phase chromatogram condition for：With octadecylsilane key
Close silica gel C18 chromatographic columns (4.6mm × 250mm, 5 μm) be filler, using acetonitrile as mobile phase, with contain 0.5% formic acid and
0.1% triethylamine solution is Mobile phase B, and gradient elution time-program(me) is：0~13 minute mobile phase A is 10 → 22%, Mobile phase B
It is 90 → 78%；13~25 minutes mobile phase As are 22%, Mobile phase B 78%；Detection wavelength is 280nm.Flow velocity 1.0mL/ minutes,
30 DEG C of column temperature, 10 μ l of sample size.
Embodiment 1
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 60 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 25MPa pressure, starts static holding 60 minutes, then with 3mL/ minutes
Continue dynamic extraction after 120 minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1258 gram）.
2.5mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 200ml is added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：40）, stand and place 30 minutes, be more than to surpass under power 300W
After sound extracts 30 minutes, extracting solution is obtained, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water saturation ethyl acetate and extracts 5 times, each 200ml, merges upper layer acetic acid ethyl acetate extract, uses
Rotary Evaporators reduced pressure is evaporated to get norisoboldine, and the HPLC collection of illustrative plates of norisoboldine is as shown in Figure 1.Go first
It is 0.836% that isoboldine, which extracts yield, opposite recovery rate 110.7%, purity 75.857%.Lower layer's aqueous B Rotary Evaporators
After removing Residual ethyl acetate, it can be continuing with debita spissitudo is deployed into.Such as terminate the extraction process, steaming can be concentrated under reduced pressure
Dry, recycling obtains 1- butyl -3- methylimidazole bromide ionic liquids.
Embodiment 2
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 40 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 30MPa pressure, starts static holding 30 minutes, then with 4mL/ minutes
Continue dynamic extraction after 120 minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1386 gram）.
1.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 200ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：40）, stand and place 30 minutes, be more than to surpass under power 400W
Sound extracts after sixty minutes, obtains extracting solution, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water-saturated n-butanol and extracts 5 times, each 200ml, merges upper layer butanol extraction liquid, with rotation
Evaporation under reduced pressure concentration is evaporated to get norisoboldine.It is 0.818% that norisoboldine, which extracts yield, opposite recovery rate
108.3%, purity 75.659%.After lower layer's aqueous removes residual n-butyl alcohol with Rotary Evaporators, can with being deployed into debita spissitudo,
It is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtains 1- butyl -3- methylimidazole bromide ionic liquids
Body.
Embodiment 3
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 60 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 20MPa pressure, starts static holding 60 minutes, then with 4mL/ minutes
Continue dynamic extraction after 90 minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1390 gram）.
2.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 100ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：20）, stand and place 30 minutes, be more than to surpass under power 300W
Sound extracts after sixty minutes, obtains extracting solution, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water saturation ethyl acetate and extracts 5 times, each 100ml, merges upper layer acetic acid ethyl acetate extract, uses
Rotary Evaporators reduced pressure is evaporated to get norisoboldine.It is 0.806% that norisoboldine, which extracts yield, opposite to extract
Rate 106.8%, purity 74.461%.It, can be appropriate with being deployed into after lower layer's aqueous removes Residual ethyl acetate with Rotary Evaporators
Concentration is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtain 1- butyl -3- methylimidazoles bromide from
Sub- liquid.
Embodiment 4
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 50 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 30MPa pressure, starts static holding 45 minutes, then with 3mL/ minutes
Continue dynamic extraction after 90 minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1246 gram）.
2.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 300ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：60）, stand and place 30 minutes, be more than to surpass under power 300W
Sound extracts after sixty minutes, obtains extracting solution, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water-saturated n-butanol and extracts 5 times, each 300ml, merges upper layer butanol extraction liquid, with rotation
Evaporation under reduced pressure concentration is evaporated to get norisoboldine.It is 0.805% that norisoboldine, which extracts yield, opposite recovery rate
106.6%, purity 79.453%.After lower layer's aqueous removes residual n-butyl alcohol with Rotary Evaporators, can with being deployed into debita spissitudo,
It is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtains 1- butyl -3- methylimidazole bromide ionic liquids
Body.
Embodiment 5
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 40 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 25MPa pressure, starts static holding 60 minutes, then with 5mL/ minutes
Continue dynamic extraction after 90 minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1442 gram）.
1.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 200ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：40）, stand and place 30 minutes, be more than to surpass under power 300W
Sound extracts after sixty minutes, obtains extracting solution, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water saturation ethyl acetate and extracts 5 times, each 200ml, merges upper layer acetic acid ethyl acetate extract, uses
Rotary Evaporators reduced pressure is evaporated to get norisoboldine.It is 0.846% that norisoboldine, which extracts yield, opposite to extract
Rate 106.6%, purity 73.573%.It, can be appropriate with being deployed into after lower layer's aqueous removes Residual ethyl acetate with Rotary Evaporators
Concentration is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtain 1- butyl -3- methylimidazoles bromide from
Sub- liquid.
Embodiment 6
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 60 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 30MPa pressure, starts static holding 40 minutes, then with 5mL/ minutes
Continue dynamic extraction after sixty minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1420 gram）.
2.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 200ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：40）, stand and place 30 minutes, be more than to surpass under power 300W
After sound extracts 90 minutes, extracting solution is obtained, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water-saturated n-butanol and extracts 5 times, each 200ml, merges upper layer butanol extraction liquid, with rotation
Evaporation under reduced pressure concentration is evaporated to get norisoboldine.It is 0.850% that norisoboldine, which extracts yield, opposite recovery rate
112.6%, purity 75.477%.After lower layer's aqueous removes residual n-butyl alcohol with Rotary Evaporators, can with being deployed into debita spissitudo,
It is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtains 1- butyl -3- methylimidazole bromide ionic liquids
Body.
Embodiment 7
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 40 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 20MPa pressure, starts static holding 60 minutes, then with 3mL/ minutes
Continue dynamic extraction after sixty minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1433 gram）.
1.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 200ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：40）, stand and place 30 minutes, be more than to surpass under power 300W
Sound extracts after sixty minutes, obtains extracting solution, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water saturation ethyl acetate and extracts 5 times, each 200ml, merges upper layer acetic acid ethyl acetate extract, uses
Rotary Evaporators reduced pressure is evaporated to get norisoboldine.It is 0.853% that norisoboldine, which extracts yield, opposite to extract
Rate 112.9%, purity 76.478%.It, can be appropriate with being deployed into after lower layer's aqueous removes Residual ethyl acetate with Rotary Evaporators
Concentration is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtain 1- butyl -3- methylimidazoles bromide from
Sub- liquid.
Embodiment 8
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 50 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 20MPa pressure, starts static holding 30 minutes, then with 5mL/ minutes
Continue dynamic extraction after 120 minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract is obtained from separating still receiving bottle
（0.1327 gram）.
1.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 300ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：60）, stand and place 30 minutes, be more than to surpass under power 300W
After sound extracts 90 minutes, extracting solution is obtained, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water-saturated n-butanol and extracts 5 times, each 300ml, merges upper layer butanol extraction liquid, with rotation
Evaporation under reduced pressure concentration is evaporated to get norisoboldine.It is 0.817% that norisoboldine, which extracts yield, opposite recovery rate
108.2%, purity 74.210%.After lower layer's aqueous removes residual n-butyl alcohol with Rotary Evaporators, can with being deployed into debita spissitudo,
It is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtains 1- butyl -3- methylimidazole bromide ionic liquids
Body.
Embodiment 9
It takes 5g root of three-nerved spicebush root tuber powder to put into supercritical reaction kettle, extraction kettle is respectively heated, when reaching 50 DEG C, open
CO2Gas cylinder pressurizes to system, when reaching 25MPa pressure, starts static holding 60 minutes, then with 4mL/ minutes
Continue dynamic extraction after sixty minutes, root of three-nerved spicebush extract remainder is obtained from extraction equipment, extract B is obtained from separating still receiving bottle
（0.1303 gram）.
1.5 mol/L 1- butyl -3- methylimidazole bromide aqueous solutions 200ml are added in root of three-nerved spicebush extract remainder（Root of three-nerved spicebush extract remainder with
1- butyl -3- methylimidazole bromide aqueous solution mass volume ratios are 1：40）, stand and place 30 minutes, be more than to surpass under power 300W
Sound extracts after sixty minutes, obtains extracting solution, filtrate is obtained by filtration in filter paper.
Gained filtrate is added water-saturated n-butanol and extracts 5 times, each 200ml, merges upper layer butanol extraction liquid, with rotation
Evaporation under reduced pressure concentration is evaporated to get norisoboldine.It is 0.821% that norisoboldine, which extracts yield, opposite recovery rate
108.8%, purity 75.348%.After lower layer's aqueous removes residual n-butyl alcohol with Rotary Evaporators, can with being deployed into debita spissitudo,
It is continuing with.Such as terminate the extraction process, can be concentrated under reduced pressure and be evaporated, recycling obtains 1- butyl -3- methylimidazole bromide ionic liquids
Body.
Claims (5)
1. a kind of method of norisoboldine high efficiency extraction, it is characterised in that comprise the following steps that：
（1）Degreasing：The root of three-nerved spicebush root tuber powder to have pulverized and sieved is put into supercritical CO2Supercritical CO is carried out in extraction equipment2Extraction
It takes, obtains root of three-nerved spicebush extract remainder after extraction from extraction equipment, extract is obtained from separating still receiving bottle；
（2）Extraction：It will the above overcritical object CO2Ionic liquid aqueous solution is added in root of three-nerved spicebush extract remainder, and ultrasound assisted extraction is carried
Take liquid, extracting solution that filtrate and solid material is obtained by filtration；
（3）Extraction：Organic solvent extraction is added in ionic liquid extract filtrate, stratification obtains upper organic phase extract liquor
With lower layer's aqueous, upper layer organic extract liquid is concentrated under reduced pressure to get norisoboldine.
2. a kind of method of high efficiency extraction norisoboldine as described in claim 1, it is characterised in that the step（1）
Middle supercritical CO2Extraction conditions is：Temperature is 40~60 DEG C, and pressure is 20~30MPa, and the static retention time is 30~60 points
Clock, Dynamic Extraction time are 30~120 minutes.
3. a kind of method of high efficiency extraction norisoboldine as described in claim 1, it is characterised in that the step（2）
Described in ionic liquid aqueous solution intermediate ion liquid be 1- butyl -3- methylimidazole bromides, ion concentration be 0.25~
2.5mol/L, root of three-nerved spicebush extract remainder are 1: 10~100 with ionic liquid aqueous solution mass volume ratio, and ultrasound assisted extraction condition is：
Extraction time is 15~120 minutes；300~500W of ultrasonic power.
4. a kind of method of high efficiency extraction norisoboldine as described in claim 1, it is characterised in that the step（3）
Middle organic solvent is ethyl acetate or n-butanol.
5. a kind of method of high efficiency extraction norisoboldine as described in claim 1, it is characterised in that the step（3）
Middle lower layer's raffinate is diluted with water to debita spissitudo, is continuing with removing upper layer residual organic solvents are concentrated under reduced pressure；Or it will
Lower layer's raffinate reduced pressure completely removes water and organic solvent, after dry, obtains recycling ionic liquid, is protected in dry environment
It deposits, is recycled in extraction separation afterwards.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180584A (en) * | 2018-07-25 | 2019-01-11 | 湖南农业大学 | A method of separating norisoboldine from the root of three-nerved spicebush |
| CN113197934A (en) * | 2021-04-15 | 2021-08-03 | 浙大宁波理工学院 | Lindera aggregata leaf extract and preparation method and application thereof |
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| 杨静: "应用超临界CO2萃取两种天然植物中有效成分的工艺研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109180584A (en) * | 2018-07-25 | 2019-01-11 | 湖南农业大学 | A method of separating norisoboldine from the root of three-nerved spicebush |
| CN113197934A (en) * | 2021-04-15 | 2021-08-03 | 浙大宁波理工学院 | Lindera aggregata leaf extract and preparation method and application thereof |
| CN113197934B (en) * | 2021-04-15 | 2022-03-11 | 浙大宁波理工学院 | Lindera aggregata leaf extract and preparation method and application thereof |
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| CN108299298B (en) | 2021-06-01 |
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