CN105176673A - Method for extracting fat oil in croton by using ionic liquid - Google Patents
Method for extracting fat oil in croton by using ionic liquid Download PDFInfo
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- CN105176673A CN105176673A CN201510687315.2A CN201510687315A CN105176673A CN 105176673 A CN105176673 A CN 105176673A CN 201510687315 A CN201510687315 A CN 201510687315A CN 105176673 A CN105176673 A CN 105176673A
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Abstract
The invention belongs to the technical field of traditional Chinese medicine component extraction, and in particular discloses a method for extracting fat oil in croton by using an ionic liquid. The method comprises the following steps: preparing croton, extracting by using an ionic liquid ethanol solution, performing column chromatography isolation, performing vacuum concentration, and drying in vacuum, thereby obtaining fat oil. The method for extracting fat oil in croton by using the ionic liquid is green and environment-friendly, high in oil yield and simple in whole operation process, waste of traditional Chinese medicine resources can be reduced, the prepared croton fat oil can be directly used in medicines without boiling, and good economic and social benefits can be made.
Description
Technical field
The invention belongs to Chinese medicinal materials Component Extraction field, be specifically related to a kind of method utilizing fatty oil in ionic liquid extract crotons.
Background technology
Many Chinese medicinal materialss contain multiple bioactive compound, have multiple curative effect, have a wide range of applications.Common activeconstituents is as polyphenolic compound, nitrogenous compound, VITAMIN, terpenoid and some other endogenous metabolism thing.The extracting method that these active compounds adopt usually comprises decocting method, ultrasonic circumfluence method, soxhlet extraction etc., but, virulent organic solvent is used and large usage quantity in these methods experiment processes, it is very long to extract the time used, extraction efficiency is low, and experiment operator health is harmful to, environmental pollution is serious.Therefore, for a long time, traditional Chinese medicine extraction activeconstituents replaces traditional organic solvent in the urgent need to finding a kind of nonvolatile solvent that is nontoxic, high-level efficiency extraction.
Chinese patent CN1569204A discloses a kind of extracting method of Oleum Tiglii, get crotons, carry out broken shell, put into the beeswax that heating has been melted, fry to Semen Crotonis coke yellow, then use 60 ~ 80% extraction using alcohol 4 ~ 6 hours, extract reclaims ethanol to most, carry out inclusion with HP-β-CD, obtain crotons inclusion compound.But this method can not abundant extracting effective components Oleum Tiglii, causes the large percentage of crotons in preparation prescription, herb resource can be caused to waste in this patent to the use of crotons.
Summary of the invention
For overcoming above-mentioned defect, the object of the present invention is to provide a kind of method utilizing fatty oil in ionic liquid extract crotons, environmental protection, oil yield is high.
For achieving the above object, the present invention adopts following technical scheme:
Utilize a method for fatty oil in ionic liquid extract crotons, comprise the following steps:
(1) crotons are removed the peel, get kind of a benevolence 10 ~ 20g, concoct, pulverize, obtain crotons processed product;
(2) in step (1) crotons processed product, add ionic liquid ethanolic soln 80 ~ 120mL, mix, under 50 ~ 70 DEG C of conditions, react 5 ~ 10h, obtain mixed solution;
(3) step (2) mixed solution is carried out micro-filtration, collect filtrate, removing ethanol;
(4) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum-drying, obtain fatty oil.
According to the above-mentioned method utilizing fatty oil in ionic liquid extract crotons, described (1) concocting method is: empty pot is burnt heat, the crotons kind that stir-fries benevolence, when stir-fry becomes brown color to crotons Zhong Ren square section from yellow-white, takes out rapidly, cooling.
According to the above-mentioned method utilizing fatty oil in ionic liquid extract crotons, step (2) ionic liquid ethanolic soln intermediate ion strength of fluid is 0.3 ~ 0.6mol/L.
According to the above-mentioned method utilizing fatty oil in ionic liquid extract crotons, described step (2) ionic liquid is 1-butyl-3-Methylimidazole hexafluorophosphate (BmimPF
6), 1-hexyl-3-Methylimidazole hexafluorophosphate (HmimPF
6), 1-butyl-3-Methylimidazole hexafluoro antimonate (BmimSbF
6) and 1-butyl-3-Methylimidazole fluoroform sulphonate (BmimCF
3sO
3) middle at least one.
According to the above-mentioned method utilizing fatty oil in ionic liquid extract crotons, described step (4) column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluent is sherwood oil and acetone, and both volume ratios are 1:1 ~ 10:1.
the positive beneficial effect of the present invention:
1. the present invention utilizes the method for fatty oil in ionic liquid extract crotons first through concocting step, remove most of grease, make crotin lose activity simultaneously, further across ionic liquid ethanolic soln extraction step, selective extraction crotons effective constituent fatty oil, fatty oil content loss is few, oil yield is high, composition is basicly stable, decreases the waste of Chinese material medicine resource, and crotons toxicity reduces greatly.
2. ionic liquid liquid state temperature range of the present invention is wide, from lower than or close to room temperature within the scope of 300 DEG C, can stable existence, there is good thermostability, good dissolving power is all shown to a large amount of inorganic and organic substances, fusing point is low, non-combustible, and steam forces down, not volatile, easy recovery, environmental protection, overcomes the problem of environmental pollution that traditional Chinese medicine extracts organic solvent.
3. the present invention utilizes the whole operating process of the method for fatty oil in ionic liquid extract crotons simple, and gained crotons fatty oil can be applied directly in the middle of medicine, does not need decoction process, has good economic benefit and social benefit.
Embodiment
Below in conjunction with some embodiments, the present invention is further described.
Embodiment 1
Utilize a method for fatty oil in ionic liquid extract crotons, comprise the following steps:
(1) crotons are removed the peel, get kind of a benevolence 10g, concoct, pulverize, obtain crotons processed product; Described concocting method is: empty pot is burnt heat, the crotons kind that stir-fries benevolence, when stir-fry becomes brown color to crotons Zhong Ren square section from yellow-white, takes out rapidly, cooling;
(2) in step (1) crotons processed product, add ionic liquid ethanolic soln 80mL, mix, ionic liquid is BmimCF
3sO
3, concentration is 0.3mol/L, reacts 10h, obtain mixed solution under 50 DEG C of conditions;
(3) step (2) mixed solution is carried out micro-filtration, collect filtrate, removing ethanol;
(4) filtrate is adopted column chromatography for separation, 200 ~ 300 order silicagel columns, eluent is sherwood oil and acetone, and both volume ratios are 1:1 ~ 10:1, concentrating under reduced pressure, and vacuum-drying obtains fatty oil 2.6g.
Embodiment 2
Utilize a method for fatty oil in ionic liquid extract crotons, comprise the following steps:
(1) crotons are removed the peel, get kind of a benevolence 12g, concoct, pulverize, obtain crotons processed product; Described concocting method is: empty pot is burnt heat, the crotons kind that stir-fries benevolence, when stir-fry becomes brown color to crotons Zhong Ren square section from yellow-white, takes out rapidly, cooling;
(2) in step (1) crotons processed product, add ionic liquid ethanolic soln 90mL, mix, ionic liquid is BmimPF
6, concentration is 0.4mol/L, reacts 8h, obtain mixed solution under 55 DEG C of conditions;
(3) step (2) mixed solution is carried out micro-filtration, collect filtrate, removing ethanol;
(4) filtrate is adopted column chromatography for separation, 200 ~ 300 order silicagel columns, eluent is sherwood oil and acetone, and both volume ratios are 1:1 ~ 10:1, concentrating under reduced pressure, and vacuum-drying obtains fatty oil 2.3g.
Embodiment 3
Utilize a method for fatty oil in ionic liquid extract crotons, comprise the following steps:
(1) crotons are removed the peel, get kind of a benevolence 15g, concoct, pulverize, obtain crotons processed product; Described concocting method is: empty pot is burnt heat, the crotons kind that stir-fries benevolence, when stir-fry becomes brown color to crotons Zhong Ren square section from yellow-white, takes out rapidly, cooling;
(2) in step (1) crotons processed product, add ionic liquid ethanolic soln 100mL, mix, ionic liquid is BmimSbF
6, concentration is 0.42mol/L, reacts 7h, obtain mixed solution under 60 DEG C of conditions;
(3) step (2) mixed solution is carried out micro-filtration, collect filtrate, removing ethanol;
(4) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum-drying, obtain fatty oil 4.3g.
Embodiment 4
Utilize a method for fatty oil in ionic liquid extract crotons, comprise the following steps:
(1) crotons are removed the peel, get kind of a benevolence 17g, concoct, pulverize, obtain crotons processed product; Described concocting method is: empty pot is burnt heat, the crotons kind that stir-fries benevolence, when stir-fry becomes brown color to crotons Zhong Ren square section from yellow-white, takes out rapidly, cooling;
(2) in step (1) crotons processed product, add ionic liquid ethanolic soln 110mL, mix, ionic liquid is HmimPF
6and BmimCF
3sO
3, both are 0.3mol/L at concentration, react 6h, obtain mixed solution under 65 DEG C of conditions;
(3) step (2) mixed solution is carried out micro-filtration, collect filtrate, removing ethanol;
(4) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum-drying, obtain fatty oil 5.0g.
Embodiment 5
Utilize a method for fatty oil in ionic liquid extract crotons, comprise the following steps:
(1) crotons are removed the peel, get kind of a benevolence 20g, concoct, pulverize, obtain crotons processed product; Described concocting method is: empty pot is burnt heat, the crotons kind that stir-fries benevolence, when stir-fry becomes brown color to crotons Zhong Ren square section from yellow-white, takes out rapidly, cooling;
(2) in step (1) crotons processed product, add ionic liquid ethanolic soln 120mL, mix, ionic liquid is HmimPF
6, concentration is 0.6mol/L, reacts 5h, obtain mixed solution under 70 DEG C of conditions;
(3) step (2) mixed solution is carried out micro-filtration, collect filtrate, removing ethanol;
(4) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum-drying, obtain fatty oil 5.2g.
Calculate above-described embodiment 1 ~ 5 fatty oil oil yield, by the extracting method of " Chinese Pharmacopoeia " in contrast, the results are shown in Table 1; Fatty oil GC-MS composition analysis result is in table 2.
The oil yield result of table 1 embodiment of the present invention 1 ~ 5
Fatty oil content result prepared by table 2 embodiment of the present invention 1 ~ 5
From above-mentioned table 1 and table 2, the present invention utilizes the method process crotons of fatty oil in ionic liquid extract crotons, and fatty oil oil yield is high, and fatty oil effective constituent kind and content do not change substantially, shows that crotons fat oil nature does not change; And phorbol ester class toxic chemical do not detected, further across the fatty oil illustrated after the inventive method extraction, toxicity reduces.
Claims (5)
1. utilize a method for fatty oil in ionic liquid extract crotons, it is characterized in that, comprise the following steps:
(1) crotons are removed the peel, get kind of a benevolence 10 ~ 20g, concoct, pulverize, obtain crotons processed product;
(2) in step (1) crotons processed product, add ionic liquid ethanolic soln 80 ~ 120mL, mix, under 50 ~ 70 DEG C of conditions, react 5 ~ 10h, obtain mixed solution;
(3) step (2) mixed solution is carried out micro-filtration, collect filtrate, removing ethanol;
(4) filtrate is adopted column chromatography for separation, concentrating under reduced pressure, vacuum-drying, obtain fatty oil.
2. the method utilizing fatty oil in ionic liquid extract crotons according to claim 1, is characterized in that, described (1) concocting method is: empty pot is burnt heat, the crotons kind that stir-fries benevolence, when stir-fry becomes brown color to crotons Zhong Ren square section from yellow-white, take out rapidly, cooling.
3. the method utilizing fatty oil in ionic liquid extract crotons according to claim 1, is characterized in that, step (2) ionic liquid ethanolic soln intermediate ion strength of fluid is 0.3 ~ 0.6mol/L.
4. the method utilizing fatty oil in ionic liquid extract crotons according to claim 1, it is characterized in that, described step (2) ionic liquid is at least one in 1-butyl-3-Methylimidazole hexafluorophosphate, 1-hexyl-3-Methylimidazole hexafluorophosphate, 1-butyl-3-Methylimidazole hexafluoro antimonate and 1-butyl-3-Methylimidazole fluoroform sulphonate.
5. the method utilizing fatty oil in ionic liquid extract crotons according to claim 1, it is characterized in that, described step (4) column chromatography for separation condition is: 200 ~ 300 order silicagel columns, and eluent is sherwood oil and acetone, and both volume ratios are 1:1 ~ 10:1.
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| CN201510687315.2A CN105176673A (en) | 2015-10-22 | 2015-10-22 | Method for extracting fat oil in croton by using ionic liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777541A (en) * | 2016-03-30 | 2016-07-20 | 淮阴师范学院 | Method for preparing 1-stearic acid-2-oleic acid-3-linoleic acid glyceride |
| CN108671582A (en) * | 2018-06-21 | 2018-10-19 | 东北林业大学 | Method that is a kind of while extracting Fructus Schisandrae Polysaccharide and Schisandra chinensis essential oil |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1050990A (en) * | 1989-10-18 | 1991-05-01 | 徐立生 | Anticancer medicine of croton and its preparing process |
| CN1126611A (en) * | 1995-01-11 | 1996-07-17 | 怀化地区第一医院 | Croton oil and beta-cyclodextrin compound and its prepn process |
| CN1569204A (en) * | 2004-05-14 | 2005-01-26 | 北京神农坛医药科技有限公司 | Croton contained medicinal composition for treating tuberculosis and its preparing process |
| CN103725418A (en) * | 2013-12-20 | 2014-04-16 | 茂名市德威圣科技有限责任公司 | Method for extracting jack fruit aromatherapy oil from ionic liquid |
| CN104710502A (en) * | 2015-03-18 | 2015-06-17 | 浙江工商大学 | Method for efficiently extracting triptolide and tripdiolide with ionic liquid |
-
2015
- 2015-10-22 CN CN201510687315.2A patent/CN105176673A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1050990A (en) * | 1989-10-18 | 1991-05-01 | 徐立生 | Anticancer medicine of croton and its preparing process |
| CN1126611A (en) * | 1995-01-11 | 1996-07-17 | 怀化地区第一医院 | Croton oil and beta-cyclodextrin compound and its prepn process |
| CN1569204A (en) * | 2004-05-14 | 2005-01-26 | 北京神农坛医药科技有限公司 | Croton contained medicinal composition for treating tuberculosis and its preparing process |
| CN103725418A (en) * | 2013-12-20 | 2014-04-16 | 茂名市德威圣科技有限责任公司 | Method for extracting jack fruit aromatherapy oil from ionic liquid |
| CN104710502A (en) * | 2015-03-18 | 2015-06-17 | 浙江工商大学 | Method for efficiently extracting triptolide and tripdiolide with ionic liquid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777541A (en) * | 2016-03-30 | 2016-07-20 | 淮阴师范学院 | Method for preparing 1-stearic acid-2-oleic acid-3-linoleic acid glyceride |
| CN105777541B (en) * | 2016-03-30 | 2018-10-26 | 淮阴师范学院 | The preparation method of 1- stearic acid -2- oleic acid -3- glyceryl linoleates |
| CN108671582A (en) * | 2018-06-21 | 2018-10-19 | 东北林业大学 | Method that is a kind of while extracting Fructus Schisandrae Polysaccharide and Schisandra chinensis essential oil |
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Application publication date: 20151223 |