CN109942528A - A kind of method that ionic liquid separates cynaropicrin in leaf of Cynara scolymus L - Google Patents
A kind of method that ionic liquid separates cynaropicrin in leaf of Cynara scolymus L Download PDFInfo
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- CN109942528A CN109942528A CN201910279634.8A CN201910279634A CN109942528A CN 109942528 A CN109942528 A CN 109942528A CN 201910279634 A CN201910279634 A CN 201910279634A CN 109942528 A CN109942528 A CN 109942528A
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Abstract
The invention discloses the methods of cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L, comprising the following steps: selecting leaf of Cynara scolymus L and being placed in baking oven dry, pulverize；Leaf of Cynara scolymus L powder is added in certain density ionic liquid solution by certain solid-liquid ratio, stirs 30-90min at a certain temperature, keeps its extraction abundant；Suspension is centrifuged 15min at 1000-1500r/min, is added ionic liquid cycling extraction 3 times；Merge above-mentioned supernatant, be added a certain proportion of ethanol water, static 12 hours at 5 DEG C, cynaropicrin precipitating, filtering is precipitated；Filter vacuum concentration can be recycled after removing ethanol water, and filter cake is dried in vacuo to obtain cynaropicrin after cold water washs.The present invention uses ionic liquid aqueous solution selective extraction cynaropicrin, and extraction yield reaches 90% or more.Present device less investment will not generate the volatile materials being harmful to the human body, environmental protection, meet sustainable development idea.
Description
Technical field
The present invention relates to cynaropicrin extractive technique fields, and in particular to cynara scolymus in a kind of ionic liquid separation leaf of Cynara scolymus L
The method of bitter principle.
Background technique
Globe artichoke alias chrysanthemum Ji, cynara scolymus, French lily, lotus lily etc., scientific name (CynarascolymusL) belongs to composite family
Herbaceos perennial, likes moist climate, and resistance to light frost is avoided xeothermic.Globe artichoke is a kind of health-care vegetable with high nutrition, both may be used
Fresh food can also be used for extracting various useful compounds, such as polyphenol, flavones, terpenoid several functions compound.Court
The nutritive value of fresh Ji has: can reduce blood pressure, the generation of prevention of arterial atherosis；It can treat abdominal pain, abdominal distension and nausea
Equal disease of digestive tracts.The leaf of globe artichoke is often considered herbal medicine application, can treat indigestion, promotes bile secretion etc..
Contain cynaropicrin in the leaf of globe artichoke, stem skin and vein, wherein the cynaropicrin content in leaf of Cynara scolymus L
Compared with horn of plenty, therefore leaf of Cynara scolymus L is the desirable feedstock for extracting cynaropicrin.Cynaropicrin is mainly a kind of guaiaci lignum alkanes times
Half terpenoid has anti-spasm, promotees apoptosis, anti-inflammatory effect, to a variety of physiology function such as Helazzq cancer cell toxic action
Energy.Currently, globe artichoke is currently in the primary process segment in China, foreign countries are mainly carried out using the functional components of globe artichoke
The research and development of heath-function product and herbal medicine.The country is less to the effective component extraction process research in globe artichoke, therefore studies
The cynaropicrin extraction process of globe artichoke is of great importance to its further development and utilization.Cynaropicrin separation and Extraction is come out
It can be made to play bigger medical value, economic value, provided for the exploitation of multifunctional food and the exploitation of newtype drug
More selections.
Currently, cynaropicrin mainly uses the organic solvents such as methanol, ethyl alcohol, acetone, methylene chloride to extract, this method is organic
Solvent usage amount is big, and so as to cause some security risks and environmental pollution, impurity content is higher and recovery rate is low, needs subsequent
Separation.As patent CN201811457222.0 report prepares cynara scolymus hardship in globe artichoke by AB-8 macroporous resin adsorption gradient elution
Element, macroporous adsorption resin technology generate a large amount of elution waste water, and industrialization environmental protection pressure is larger.For this purpose, being badly in need of developing a kind of green
The isolation technics that colour circle is protected.
Ion liquid abstraction is a kind of novel extraction mode, can be used to extract various organic compounds, bioactivity
Molecule and metal ion etc. have many advantages, such as that nontoxic, green, use scope is wide, extraction yield is high.Ionic liquid is one kind by organic
Cationic, inorganic or organic anion composition, be at room temperature the substance of liquid, its excellent property with a series of unique
Matter, such as preferable thermal stability and chemical stability, nonflammable, stronger electric conductivity, difficult volatilization, extremely low vapour pressure.By
In ionic liquid plurality of advantages and the performance of ionic liquid can be regulated and controled by changing the structure of ionic liquid, so sharp
It is also more and more come the application of extracting of organic compounds with ionic liquid.
Summary of the invention
The purpose of the present invention is to provide the methods of cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L, and this method is more
Add safely, effectively, it is economical, environmentally protective.
To achieve the above object, the invention provides the following technical scheme:
A kind of method that ionic liquid separates cynaropicrin in leaf of Cynara scolymus L, comprising the following steps:
1) it picks out and is placed in drying in baking oven without mildew, without lesion, clean leaf of Cynara scolymus L, drying temperature is 50-65 DEG C,
Drying time is 60-120min, then crushes dried leaf of Cynara scolymus L with pulverizer, and be sieved 40-60 mesh；
2) that the resulting leaf of Cynara scolymus L powder of step 1) is added to certain density ionic liquid by certain solid-liquid ratio is molten
In liquid, 30-90min is stirred at a certain temperature, keeps its extraction abundant；
3) the resulting suspension of step 2) is centrifuged at 1000-1500r/min 15min, added fresh or recycling
Ionic liquid cycling extraction 3 times；
4) merge above-mentioned steps 3) resulting supernatant, a certain proportion of ethanol water is added, static 12 is small at 5 DEG C
When, cynaropicrin precipitating, filtering is precipitated；
5) it can be recycled after taking the concentration of step 4) filter vacuum to remove ethanol water, filter cake vacuum after cold water washs
Dry cynaropicrin.
Be as further scheme of the invention: the ionic liquid in the step 2) is 1- alkyl -3- methylimidazole
Close object；1- alkyl -3- the methylimidazole compound mainly includes [C2Min]Cl、[C4Min]Cl、[C8Min]Cl、[C10Min]
Cl、[C12Min]Cl、[C14Min] one of Cl or a variety of.
It is as further scheme of the invention: the quality of leaf of Cynara scolymus L powder and ionic liquid solution in the step 2)
Volume ratio is leaf of Cynara scolymus L powder: ionic liquid solution=1:10~50.
Be as further scheme of the invention: step 2) the intermediate ion liquid solution is ionic liquid and deionized water
It reconciles by a certain percentage, the molal volume concentration of the ionic liquid is 50-1000mM/L.
Be as further scheme of the invention: step 2) the intermediate ion liquid solution extraction temperature is 20-50 DEG C.
It is as further scheme of the invention: the ethanol water volumetric concentration being added in the step 4) is 0~
10%, the supernatant and ethanol water volume ratio are 1:5~100.
Be as further scheme of the invention: filtrate is water-soluble through being concentrated in vacuo and obtained ionic liquid in the step 5)
Liquid can be with cycling extraction 8 times or more.
Be as further scheme of the invention: the step 5) cynaropicrin is quantitatively divided using high performance liquid chromatography
Analysis, specifically: high performance liquid chromatography detection, eluant, eluent used are the mixture of water and acetonitrile, and the ratio between mixture is 75:
25；Flow velocity is 0.5ml/min, and sample volume is 10 μ L, Detection wavelength 198nm.
Compared with prior art, the present invention have it is following the utility model has the advantages that
The present invention provides the methods of cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L, implement to have by this technology
Have following the utility model has the advantages that (1) present invention is using ionic liquid aqueous solution selective extraction cynaropicrin, ionic liquid passes through vacuum
Concentration can be recycled after removing water, and extraction yield reaches 90% or more；(2) water-soluble using ionic liquid, and cynaropicrin
The characteristics of solubility in water low (774.6mg/L, 25 DEG C of Chemspider, 2017), by adding in the supernatant to centrifugation
Enter a certain proportion of water, obtain cynaropicrin precipitating, then by ethyl alcohol water washing, purifies cynaropicrin, cynaropicrin yield
Reach 80% or more, purity reaches 90% or more；(3) present device less investment, process flow it is simple, it is easy to operate, will not
The volatile materials, free from environmental pollution being harmful to the human body is generated, sustainable development idea is met.
Specific embodiment
Combined with specific embodiments below, technical scheme in the embodiment of the invention is clearly and completely described, shows
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1:
A kind of method that ionic liquid separates cynaropicrin in leaf of Cynara scolymus L, comprising the following steps:
1) it picks out and is placed in drying in baking oven without mildew, without lesion, clean leaf of Cynara scolymus L, drying temperature is 50 DEG C, is done
The dry time is 120min, then crushes dried leaf of Cynara scolymus L with pulverizer, and be sieved 40-60 mesh；
2) 10g leaf of Cynara scolymus L powder is taken to be added to [the C that 300mL concentration is 500mM/L14Min] in Cl aqueous solution, at 25 DEG C
30min is stirred, keeps its extraction abundant；
3) the resulting suspension of step 2) is centrifuged 15min at 1000r/min, it is spare to pour out supernatant, filter residue circulation
Extraction 3 times；
4) merge above-mentioned steps 3) resulting supernatant, the ethanol water of 20 times of volumes is added, static 12 is small at 5 DEG C
When, cynaropicrin precipitating, filtering is precipitated；
5) it can be recycled after taking the concentration of step 4) filter vacuum to remove ethanol water, filter cake is after the washing of 20mL cold water
It is dried in vacuo to obtain cynaropicrin 0.65g.
In step 4) in the present embodiment, obtained quantitative result is corresponding with the average value of at least three independent experiments.
Embodiment 2:
1) it picks out and is placed in drying in baking oven without mildew, without lesion, clean leaf of Cynara scolymus L, drying temperature is 55 DEG C, is done
The dry time is 120min, then crushes dried leaf of Cynara scolymus L with pulverizer, and be sieved 40-60 mesh；
2) 10g leaf of Cynara scolymus L powder is taken to be added to [the C that 300mL concentration is 500mM/L14Min] in Cl aqueous solution, at 25 DEG C
60min is stirred, keeps its extraction abundant；
3) the resulting suspension of step 2) is centrifuged 15min at 1500r/min, it is spare to pour out supernatant, filter residue circulation
Extraction 3 times；
4) merge above-mentioned steps 3) resulting supernatant, the ethanol water of 20 times of volumes is added, static 12 is small at 5 DEG C
When, cynaropicrin precipitating, filtering is precipitated；
5) it can be recycled after taking the concentration of step 4) filter vacuum to remove ethanol water, filter cake is after the washing of 20mL cold water
It is dried in vacuo to obtain cynaropicrin 0.67g.
Embodiment 3:
1) it picks out and is placed in drying in baking oven without mildew, without lesion, clean leaf of Cynara scolymus L, drying temperature is 65 DEG C, is done
The dry time is 60min, then crushes dried leaf of Cynara scolymus L with pulverizer, and be sieved 40-60 mesh；
2) 10g leaf of Cynara scolymus L powder is taken to be added to [the C that 300mL concentration is 500mM/L14Min] in Cl aqueous solution, at 25 DEG C
90min is stirred, keeps its extraction abundant；
3) the resulting suspension of step 2) is centrifuged 15min at 1500r/min, it is spare to pour out supernatant, filter residue circulation
Extraction 3 times；
4) merge above-mentioned steps 3) resulting supernatant, the ethanol water of 20 times of volumes is added, static 12 is small at 5 DEG C
When, cynaropicrin precipitating, filtering is precipitated；
5) it can be recycled after taking the concentration of step 4) filter vacuum to remove ethanol water, filter cake is after the washing of 20mL cold water
It is dried in vacuo to obtain cynaropicrin 0.66g.
In step 4) in the present embodiment, obtained quantitative result is corresponding with the average value of at least three independent experiments.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of method of cynaropicrin in ionic liquid separation leaf of Cynara scolymus L, which comprises the following steps:
1) it picks out and is placed in drying in baking oven without mildew, without lesion, clean leaf of Cynara scolymus L, drying temperature is 50-65 DEG C, dry
Time is 60-120min, then crushes dried leaf of Cynara scolymus L with pulverizer, and be sieved 40-60 mesh；
2) the resulting leaf of Cynara scolymus L powder of step 1) is added in certain density ionic liquid solution by certain solid-liquid ratio,
30-90min is stirred at a certain temperature, keeps its extraction abundant；
3) the resulting suspension of step 2) is centrifuged at 1000-1500r/min 15min, adds fresh or recycling ion
Liquid circulation extracts 3 times；
4) merge above-mentioned steps 3) resulting supernatant, it is added a certain proportion of ethanol water, static 12 hours at 5 DEG C, analysis
Cynaropicrin precipitates out, filtering；
5) it can be recycled after taking the concentration of step 4) filter vacuum to remove ethanol water, filter cake is dried in vacuo after cold water washs
Obtain cynaropicrin.
2. the method for cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L according to claim 1, which is characterized in that
Ionic liquid in the step 2) is 1- alkyl -3- methylimidazole compound；1- alkyl -3- methylimidazole compound the master
It to include [C2Min]Cl、[C4Min]Cl、[C8Min]Cl、[C10Min]Cl、[C12Min]Cl、[C14Min] one of Cl or more
Kind.
3. the method for cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L according to claim 1, which is characterized in that
The mass volume ratio of leaf of Cynara scolymus L powder and ionic liquid solution is leaf of Cynara scolymus L powder: ionic liquid solution in the step 2)
=1:10~50.
4. the method for cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L according to claim 1, which is characterized in that
Step 2) the intermediate ion liquid solution is that ionic liquid reconciles by a certain percentage with deionized water, the ionic liquid
Molal volume concentration is 50-1000mM/L.
5. the method for cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L according to claim 1, which is characterized in that
Step 2) the intermediate ion liquid solution extraction temperature is 20-50 DEG C.
6. the method for cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L according to claim 1, which is characterized in that
The ethanol water volumetric concentration being added in the step 4) is 0~10%, and the supernatant is with ethanol water volume ratio
1:5~100.
7. the method for cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L according to claim 1, which is characterized in that
In the step 5) filtrate be concentrated in vacuo and obtained ionic liquid aqueous solution can be with cycling extraction 8 times or more.
8. the method for cynaropicrin in a kind of ionic liquid separation leaf of Cynara scolymus L according to claim 1, which is characterized in that
Step 5) the cynaropicrin carries out quantitative analysis using high performance liquid chromatography, specifically: high performance liquid chromatography detection, it is used
Eluant, eluent be water and acetonitrile mixture, the ratio between mixture be 75:25；Flow velocity is 0.5ml/min, and sample volume is 10 μ L, inspection
Survey wavelength is 198nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113651804A (en) * | 2021-09-18 | 2021-11-16 | 陕西嘉禾生物科技股份有限公司 | Industrialized preparation method of cynaropicrin |
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| JP2006206532A (en) * | 2005-01-31 | 2006-08-10 | Ichimaru Pharcos Co Ltd | NF-kappaB ACTIVATION INHIBITOR |
| CN109180622A (en) * | 2018-11-30 | 2019-01-11 | 中南林业科技大学 | The method of guainane type sesquiterpenoid is extracted from globe artichoke |
| CN109485626A (en) * | 2018-11-30 | 2019-03-19 | 中南林业科技大学 | The method of guainane type sequiterpene is extracted from globe artichoke |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006206532A (en) * | 2005-01-31 | 2006-08-10 | Ichimaru Pharcos Co Ltd | NF-kappaB ACTIVATION INHIBITOR |
| CN109180622A (en) * | 2018-11-30 | 2019-01-11 | 中南林业科技大学 | The method of guainane type sesquiterpenoid is extracted from globe artichoke |
| CN109485626A (en) * | 2018-11-30 | 2019-03-19 | 中南林业科技大学 | The method of guainane type sequiterpene is extracted from globe artichoke |
Non-Patent Citations (2)
| Title |
|---|
| EMANUELLE L. P. DE FARIA ET AL.: "Extraction and recovery processes for cynaropicrin from Cynara cardunculus L. using aqueous solutions of surface-active ionic liquids", 《BIOPHYSICAL REVIEWS》 * |
| HITOMI MIZUNO ET AL.: "Ionic Liquid-Assisted Extraction and Isolation of Cynaropicrin and Cnicin from Artichoke and Blessed thistle", 《CHEMISTRYSELECT》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113651804A (en) * | 2021-09-18 | 2021-11-16 | 陕西嘉禾生物科技股份有限公司 | Industrialized preparation method of cynaropicrin |
| CN113651804B (en) * | 2021-09-18 | 2023-07-14 | 陕西嘉禾生物科技股份有限公司 | Industrial preparation method of cynaropicrin |
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Application publication date: 20190628 |