CN108553937A - natural eutectic solvent and its application in plant extract - Google Patents
natural eutectic solvent and its application in plant extract Download PDFInfo
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- CN108553937A CN108553937A CN201810463970.3A CN201810463970A CN108553937A CN 108553937 A CN108553937 A CN 108553937A CN 201810463970 A CN201810463970 A CN 201810463970A CN 108553937 A CN108553937 A CN 108553937A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The present invention provides a kind of natural eutectic solvent and its applications in plant extract, including hydrogen bond donor and hydrogen bond receptor;Hydrogen bond donor includes arbitrary two kinds of the combination in glycols, amino acid, carbohydrate or glycitols;Hydrogen bond receptor includes organic salt;Natural eutectic solvent water content is 10~50%.The present invention alleviates tradition with low, of high cost, dangerous, technique the is cumbersome defect of ion solvent or organic solvent extraction plant extracts efficiency;This natural eutectic solvent safety, at low cost, renewable, extraction efficiency is high;In addition, this natural eutectic solvent can be applied in plant extract, the step of also needing to be removed Extraction solvent in traditional handicraft is omitted, saves cost, the used time is short, more efficient.
Description
Technical field
The present invention relates to eutectic solvent technical fields, in particular to a kind of natural eutectic solvent and its are planting
Application in object extraction.
Background technology
Eutectic solvent is as a kind of novel low-melting mixtures solvent, by more and more extensive concern.Eutectic
Solvent is that hydrogen bond receptor by centainly measuring ratio and hydrogen bond donor are composed, the fusing point drop of eutectic solvent compared with pure material
It is much lower.Compared with conventional ion liquid, eutectic solvent, which has, prepares simple, cheap, low melting point, low cost, low
Toxicity, easy the advantages that preparing, capable of regenerating, is biodegradable;And natural eutectic solvent has extensively in foods and cosmetics field
General application prospect.
In view of the plurality of advantages that eutectic solvent technology has, in order to meet the need of different industrial process Green solvents
It wants, how preferably to apply eutectic solvent technology, so that this new technology is made the most of the advantage and be more widely used, be current
The important process of eutectic technical field, but at present eutectic solvent research and it is insufficient, existing green solvent type is also
Relatively fewer, particularly for the eutectic solvent of extracted form natural plant, be suitable for various plants extraction has high extracting efficiency
Eutectic solvent opposite lack.
Natural plants have many important active constituents, are the products currently on the market by extensive concern, but traditional
Extracted form natural plant technology, be to be extracted using the organic solvents such as methanol, ethyl alcohol, this substance has certain toxicity,
It can remain in extract after extraction, the follow-up technique that removes is very complicated, and increases cost, and with duration, efficiency is low.And
Traditional extraction process, and in preparation process some solvents volatilization or be discharged into the Nature pollute environment be not easy to be degraded.
A kind of natural eutectic solvent of reasonable preparation, to extract the active constituent in natural plants, reach higher extraction efficiency,
It is more environmentally protective, and Extraction solvent need not be removed after extracting, allow eutectic solvent as the similar or phase of extract
As material composition, play the function and effect of extract, can preferably simplify technique, it is cost-effective, improve preparation efficiency, protection
Environment;Therefore, a kind of natural eutectic solvent of exploitation is of great practical significance.
In view of this, special propose the present invention.
Invention content
One of the objects of the present invention is to provide a kind of natural eutectic solvents, and the natural eutectic solvent is mainly by glycol
Arbitrary two kinds of combination in class, amino acid, carbohydrate or glycitols and organic salt composition, water content are 10~50%.Alleviate
Conventional solvent not environmentally the shortcomings that, provide a kind of new natural eutectic solvent, which has extraction
It is efficient, environmentally protective, it is renewable, it is suitable for the advantages of various plants are extracted;The method extracted using the solvent is more
Safety, alleviates conventional solvent and needs to be removed solvent, and technique is cumbersome, with duration, and defect not environmentally.
The second object of the present invention is to provide application of the above-mentioned natural eutectic solvent in plant extract.
In order to realize that the above-mentioned purpose of the present invention, spy use following technical scheme:
A kind of natural eutectic solvent, including hydrogen bond donor and hydrogen bond receptor;Hydrogen bond donor include glycols, amino acid,
Arbitrary two kinds of combination in carbohydrate or glycitols;Hydrogen bond receptor includes organic salt;Natural eutectic solvent water content is 10~
50%.
Preferably, on the basis of the present invention program, glycols is butanediol or 1,3-PD;
Preferably, amino acid is glycine or phenylalanine;
Preferably, carbohydrate is one kind in fructose, glucose, sucrose or lactose;
Preferably, glycitols is one kind in glycerine, xylitol, sorbierite, maltitol or mannitol;
Preferably, organic salt is glycine betaine or choline.
Preferably, on the basis of the present invention program, the hydrogen bond donor of natural eutectic solvent is carbohydrate, amino acid or sugar alcohol
Arbitrary two kinds of combination in class.
Preferably, on the basis of the present invention program, the molar ratio of hydrogen bond receptor and hydrogen bond donor in natural eutectic solvent
It is (1:8)~(5:1), preferably (1:5)~(2:1), further preferably (1:2)~(2:1).
Preferably, on the basis of the present invention program, natural eutectic solvent includes mainly by fructose, glycerine and betaine group
It closes, the molar ratio of fructose, glycerine and glycine betaine is (1~4):(1~3):(4~1).Second side according to the present invention
Face, application of the natural eutectic solvent in plant extract;
Preferably, plant is ginseng, pot marigold or Chinese herbaceous peony, further preferably Chinese herbaceous peony.
Preferably, on the basis of the present invention program, include the following steps:
Pretreated plant fragment is placed in prepared natural eutectic solvent and is extracted, separation, impurity removal
Afterwards, it is concentrated, obtains plant extraction liquid;
Preferably, on the basis of the present invention program, separation, impurity removal mode is centrifugation, concentrates and is concentrated for nanofiltration;
Preferably, preservative is added after concentration, obtains plant extraction liquid.
Preferably, on the basis of the present invention program, the ratio of plant fragment and natural eutectic solvent is 0.1~
0.8g/ml (w/v), preferably 0.1~0.3g/ml (w/v).
Preferably, on the basis of the present invention program, extraction time is 30~60min, and Extracting temperature is 30~55 DEG C;
Preferably, extraction time is 50~60min, and Extracting temperature is 40~50 DEG C.
Compared with the prior art, the present invention has the advantages that:
(1) natural eutectic solvent provided by the invention includes arbitrary two in glycols, amino acid, carbohydrate or glycitols
Kind;And organic salt, optimize the water content of eutectic solvent, it is dangerous to alleviate conventional solvent, not environmentally the shortcomings that, provide
A kind of new environmentally protective natural eutectic solvent, the natural eutectic solvent have extraction efficiency it is high, it is repeatable utilize,
Easily biological-degradable is suitable for the advantages of various plants are extracted.The method extracted using the solvent is safer, and alleviating makes
With needing to be removed solvent after traditional solvent extraction, technique is cumbersome, with duration, and defect not environmentally.
(2) it due to the advantage that the natural eutectic solvent of the present invention has safety and environmental protection, extraction efficiency high, can be used as a variety of
The Extraction solvent of plant uses, and alleviates cumbersome step dangerous using conventional solvent, and needing to carry out solvent removal after extracting
Suddenly, extracting method technique of the present invention is simpler, and the used time is short, and cost is lower, environmentally safe.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
According to the first aspect of the invention, provide a kind of natural eutectic solvent, including hydrogen bond donor and hydrogen bond by
Body;Hydrogen bond donor includes arbitrary two kinds of the combination in glycols, amino acid, carbohydrate or glycitols;Hydrogen bond receptor includes organic
Salt;Natural eutectic solvent water content is 10~50%.
Eutectic solvent is the eutectic mixture formed by specific mol ratio combination by different molecular, by special
Proportioning obtain a kind of liquid of stabilization so that the fusing point of mixture is less than each component fusing point of itself, eutectic mixture
By it is a kind of based on the supramolecular structure of the very strong hydrogen bond action of intramolecular characterized by, it can be considered as a kind of single pure point
Son.
The eutectic solvent of the present invention is a kind of eutectic solvent being made of natural component.
Eutectic solvent is composed of the hydrogen bond receptor and hydrogen bond donor of certain stoichiometric ratio.
The hydrogen bond donor of the present invention includes arbitrary two kinds of combination in glycols, amino acid, carbohydrate or glycitols;Hydrogen bond by
Body includes organic salt.
Glycols, i.e. dihydric alcohol, typical but non-limiting glycols are, for example,:Butanediol, 1,3- propylene glycol etc..
It is, for example, containing amino and carboxyl Liang Zhong functional groups, typical but non-limiting amino acid in amino acid molecular:It is sweet
Propylhomoserin, phenylalanine etc..
Carbohydrate, typical but non-limiting carbohydrate are, for example,:Fructose, glucose, sucrose or lactose etc..
Glycitols, typical but non-limiting glycitols are, for example,:Glycerine, xylitol, sorbierite, maltitol or sweet dew
Alcohol.
Organic salt, typical but non-limiting organic salt are glycine betaine or choline, can use choline chloride.
The water content of natural eutectic solvent is 10~50%, and typical but non-limiting water content is, for example,:10%,
15%, 20%, 25%, 30%, 35%, 40%, 45% or 50% etc..
V/v refers to the volume ratio of water and natural eutectic solvent.
The present invention has prepared one kind according to the constituent optimization of widely applied plant extracts can effectively extract a variety of plants
The new natural eutectic solvent of object extract, mainly with arbitrary two kinds of combination in glycols, amino acid, carbohydrate or glycitols
As hydrogen bond donor, using organic salt as hydrogen bond receptor, mentioned component is selected from natural component, and it is molten that preparation obtains natural eutectic
Agent optimizes water content, and it is more preferable to have obtained mobility, the higher eutectic solvent of extraction efficiency.Solvent is repeatable to be utilized,
Easily biological-degradable can be used as the Extraction solvent of various plants.The method extracted using the solvent is safer, and
It can be used directly after extraction without removing solvent, need to be removed solvent after alleviating traditional solvent extraction, technique is numerous
It is trivial, with duration, and defect not environmentally.
In a preferred embodiment, the hydrogen bond donor of natural eutectic solvent is carbohydrate, amino acid or glycitols
In arbitrary two kinds of combination.
Solvent composition can be made closer to natural plants using two kinds of natural components combination in carbohydrate, amino acid or glycitols
Ingredient reaches better extraction effect.
In a preferred embodiment, the molar ratio of hydrogen bond receptor and hydrogen bond donor is in natural eutectic solvent
(1:8)~(5:1), preferably (1:5)~(2:1), further preferably (1:2)~(2:1).
Hydrogen bond receptor is, for example, with the typical but non-limiting molar ratio of hydrogen bond donor:1:1、1:2、1:3、1:4、1:5、1:
6、1:7、2:1、2:3、2:5、3:1 or 7:8 etc..
Optimize hydrogen bond donor and hydrogen bond donor molar ratio range, can obtain more suitably solvent viscosity and formed
Hydrogen bond is stablized, and higher extraction efficiency is obtained.
In a preferred embodiment, natural eutectic solvent includes mainly being combined by fructose, glycerine and glycine betaine
It forms, the molar ratio of fructose, glycerine and glycine betaine is (1~4):(1~3):(4~1).
The molar ratio of typical but non-limiting fructose, glycerine and glycine betaine is, for example,:1:1:2、2:2:3、1:3:2、3:
3:2 or 2:3:3 etc..
Using the natural eutectic solvent of above-mentioned composition closer to the natural component of plant, better extraction can be reached
Effect, also there are many ingredient containing carbohydrate and glycitols in natural plants, using carbohydrate, glycitols, organic salt not only without
Poison, and chemical property is similar to many natural components in plant, not only more environmentally friendly safety, but also can reach and preferably carry
Take effect.
Above-mentioned natural eutectic solvent is referred to conventional eutectic solvent preparation method and is prepared, typical but non-limit
The preparation method of property processed is, for example,:Boulton process or heating etc..
According to the second aspect of the invention, a kind of application of natural eutectic solvent in plant extract is provided;
Preferably, plant is ginseng, pot marigold or Chinese herbaceous peony, further preferably Chinese herbaceous peony.
In a preferred embodiment, include the following steps:
Pretreated plant fragment is placed in prepared natural eutectic solvent and is extracted, after separation, impurity removal
It is concentrated;Obtain plant extraction liquid.
Plant fragment is, for example, the powder being ground into after plant is broken.
In a preferred embodiment, separation, impurity removal mode is centrifugation;
Preferably, the concentration is that nanofiltration concentrates.
Preferably, preservative is added after concentration, obtains plant extraction liquid.
Pretreated plant material is come into full contact with, chemical property is similar with natural eutectic solvent gradual at branch
It enters in natural eutectic solvent system, reaches extraction effect.The mode of separation centrifuges and nanofiltration, can reach and preferably divide
From effect, the plant extraction liquid of acquisition is more clarified, and solid impurity content is lower, and preservative, which is added, can make the extracting solution longer time
Ground keeps initial quality and activity.
In a preferred embodiment, the ratio of plant fragment and natural eutectic solvent is 0.1~0.8g/ml
(w/v), preferably 0.1~0.3g/ml (w/v).
The ratio of typical but non-limiting plant and natural eutectic solvent is, for example,:0.1g/ml(w/v)、0.2g/ml
(w/v), 0.3g/ml (w/v), 0.4g/ml (w/v), 0.5g/ml (w/v), 0.6g/ml (w/v), 0.7g/ml (w/v) or 0.8g/
ml(w/v)。
The ratio for optimizing plant and natural eutectic solvent can reach better extraction efficiency, and extraction is more thorough, saves
The cost of plant as raw material.
In a preferred embodiment, extraction time is 30~60min, and Extracting temperature is 30~55 DEG C;
Typical but non-limiting extraction time is, for example,:30min, 35min, 40min, 45min, 50min, 55min or
60min;Typical but non-limiting Extracting temperature is, for example,:30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C or 55 DEG C;
Preferably, extraction time is 50~60min, and Extracting temperature is 40~50 DEG C.
Extraction time and Extracting temperature are optimized, the ingredient in plant can be allowed to be sufficiently disengaged from plant, and to enter eutectic molten
In agent, reach better extraction effect and separating effect.
In order to further appreciate that the present invention, the method for the present invention and effect are done further in detail with reference to specific embodiment
Explanation.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same or
Production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
According to molar ratio 1:1:2 weigh fructose, glycerine, glycine betaine, prepare natural eutectic solvent (water content 10%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Peony Root is accurately weighed according to the ratio 0.1g/ml (w/v) of Peony Root fragment and natural eutectic solvent
It minces and is put into mixing in extraction element with natural eutectic solvent, extract, extraction time 50min, Extracting temperature 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Embodiment 2
According to molar ratio 3:1 weighs choline chloride and phenylalanine, prepares natural eutectic solvent (water content 10%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Peony Root is accurately weighed according to the ratio 0.1g/ml (w/v) of Peony Root fragment and natural eutectic solvent
It minces and natural eutectic solvent, is put into mixing in extraction element, extracts, extraction time 50min;Extracting temperature is 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Embodiment 3
According to molar ratio 1:1:6 weigh butanediol, maltitol and glycine betaine, prepare natural eutectic solvent (water content
For 11%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Chinese herbaceous peony is accurately weighed according to the ratio 0.1g/ml (w/v) of Peony Root fragment and natural eutectic solvent
Object and natural eutectic solvent, are put into mixing in extraction element, extract, extraction time 50min;Extracting temperature is 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Embodiment 4
According to molar ratio 1:1:6 weigh sorbierite, maltitol and glycine betaine, prepare natural eutectic solvent (water content
For 15%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Chinese herbaceous peony is accurately weighed according to the ratio 0.3g/ml (w/v) of Peony Root fragment and natural eutectic solvent
Object and natural eutectic solvent, are put into mixing in extraction element, extract, extraction time 50min;Extracting temperature is 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Embodiment 5
According to molar ratio 2:1:1 weighs choline chloride, fructose and glycine, and preparing natural eutectic solvent, (water content is
18%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Peony Root is accurately weighed according to the ratio 0.1g/ml (w/v) of Peony Root fragment and natural eutectic solvent
It minces and natural eutectic solvent, is put into mixing in extraction element, extracts, extraction time 40min;Extracting temperature is 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Embodiment 6
With differing only in for embodiment 5, extraction time becomes 50min.
Embodiment 7
According to molar ratio 1:1 weighs choline chloride, sorbierite, prepares natural eutectic solvent (water content 20%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Peony Root is accurately weighed according to the ratio 0.1g/ml (w/v) of Peony Root fragment and natural eutectic solvent
It minces and natural eutectic solvent, is put into mixing in extraction element, extracts, extraction time 50min;Extracting temperature is 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Embodiment 8
According to molar ratio 5:5:4 weigh choline chloride, fructose, 1, and 3 propylene glycol prepare natural eutectic solvent (water content
For 16%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Peony Root is accurately weighed according to the ratio 0.1g/ml (w/v) of Peony Root fragment and natural eutectic solvent
It minces and natural eutectic solvent, is put into mixing in extraction element, extracts, extraction time 50min;Extracting temperature is 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Embodiment 9
According to molar ratio 3:3:4 weigh glycine betaine, lactose, 1, and 3 propylene glycol prepare natural eutectic solvent (water content
25%).
Chinese herbaceous peony is extracted using obtained natural eutectic solvent, Paeoniflorin, extracting method packet are extracted from Chinese herbaceous peony
Include following steps:
(a) it is broken that Peony Root is accurately weighed according to the ratio 0.1g/ml (w/v) of Peony Root fragment and natural eutectic solvent
It minces and natural eutectic solvent, is put into mixing in extraction element, extracts, extraction time 50min;Extracting temperature is 45
DEG C, extracting solution is obtained after extraction;
(b) after centrifuging extracting solution, supernatant liquid is obtained, then concentrated with NF membrane, preservative is added, obtain Chinese herbaceous peony extraction
Liquid.
Comparative example 1
Peony Root fragment 20g is weighed, respectively using 12 times of amount distilled water, 80% ethyl alcohol, 50% methanol as solvent, 100 DEG C
It is heated to reflux, extracts 2 times, each 1.5h, filtrate merges concentration, and constant volume is in 100mL measuring bottles.With 12 times of amount solvent volumes, often
Secondary 1.5h carries out the extraction 2 times of total glucosides of paeony.When extraction, takes 240mL solvents to be added in flask, be heated at reflux and extract Chinese herbaceous peony
Medicine glycosides extracts 1.5h, is filtered after letting cool for the first time, and filter residue is recycled addition 240mL solvents carries out refluxing extraction 1.5h again, carries
It is filtered after taking, filter residue is cleaned with a small amount of solvent, the solution of filtrate twice and cleaning filter residue is transferred to 100mL capacity together
Bottle constant volume.4 DEG C of refrigerations, spare, parallel extraction is three times.
Comparative example 2
Chinese herbaceous peony powder 20g is weighed, respectively using 12 times of amount distilled water as solvent, 100 DEG C are heated to reflux, extraction 2 times, every time
1.5h, filtrate merge concentration, and constant volume is in 100mL measuring bottles.With 12 times of amount solvent volumes, each 1.5h carries out total glucosides of paeony
Extraction 2 times.It when extraction, takes 240mL solvents to be added in flask, is heated at reflux and extracts Paeoniflorin, extract 1.5h for the first time, put
It is filtered after cold, filter residue is recycled and 240mL solvents are added carry out refluxing extraction 1.5h again, is filtered after extraction, with a small amount of
Solvent cleans filter residue, and the solution of filtrate twice and cleaning filter residue is transferred to 100mL volumetric flask constant volumes together.4 DEG C of refrigerations, it is spare,
Parallel extraction is three times.
Test example
High performance liquid chromatography carries out ingredient and content detection to the Chinese herbaceous peony extracting solution that embodiment and comparative example obtains.
Experiment reagent:Paeoniflorin standard items, acetonitrile (HPLC grades), methanol (traditional Chinese medicines), ultra-pure water.
Instrument:Agilent1260-DVD, (number:JY-lab-167);
Chromatographic column:ZobaxSB-C18 (4.6mm*250mm, 5 μm)
Electronic balance (AL204, plum Teller-support benefit, number:JY-lab-029)
Standard items information
Solvent:50% methanol.
(1) Paeoniflorin (100 μ g/mL, 500 μ g/mL, 600 μ g/mL, 700 μ g/mL, 800 μ g/mL, 900 μ g/mL, 1000 μ
g/mL)
The preparation of test sample
Test sample 0.5mL is taken, 50mL is settled to 50% methanol dilution, is crossed spare after 0.45 μm of film;
Radix paeoniae alba extraction (solid), takes 11.1mg, is placed in 100mL volumetric flasks, is dissolved with 50% methanol, ultrasonic 15min,
It cools down, constant volume, it is spare after 0.45 μm of film excessively.
Chromatographic condition
Chromatographic column:ZobaxElipseplus-C18 (4.6mm × 250mm, 5 μm), column temperature:30℃;
Mobile phase:Acetonitrile:0.05% phosphate aqueous solution gradient elution (45min), is shown in Table 1, flow velocity:1.0mL/min;
Sample size:10μL;
Detection wavelength:230nm.
Table 1
Eluent gradient table
Time | Acetonitrile (%) | 0.05% phosphate aqueous solution (%) |
0 | 5 | 95 |
20 | 15 | 85 |
30 | 20 | 80 |
40 | 25 | 75 |
45 | 55 | 55 |
The high performance liquid chromatography detection result testing result such as table 2 for the plant extracts that embodiment is obtained with comparative example.
Table 2
The high performance liquid chromatography detection result for the plant extracts that embodiment is obtained with comparative example
Embodiment | The total recovery rate of Paeoniflorin (ug/ml) |
Embodiment 1 | 968 |
Embodiment 2 | 786 |
Embodiment 3 | 850 |
Embodiment 4 | 821 |
Embodiment 5 | 875 |
Embodiment 6 | 910 |
Embodiment 7 | 743 |
Embodiment 8 | 786 |
Embodiment 9 | 758 |
Comparative example 1 | 721 |
Comparative example 2 | 705 |
By 1~9 embodiment measurement result in table 2 as it can be seen that adjusting process parameter and extraction conditions within the scope of the present invention,
Higher recovery rate can be reached, can effectively extract plant extracts.
By the measurement result of embodiment 1 in table 2 as it can be seen that when select optimization component, molar ratio, water content, liquid ratio with
And extraction conditions extract, and obtain highest extraction efficiency.I.e. fructose, glycerine, glycine betaine are with 1:1:It is prepared by 2 molar ratio
Natural eutectic solvent, extraction effect is best.
By the measurement result of embodiment 3 and embodiment 4 comparison in table 2 as it can be seen that being matched with glycols, glycitols and organic salt
Preferable extraction effect can be obtained, by optimizing the proportioning of plant material and eutectic solvent, extraction efficiency can be improved
By the measurement result of embodiment 4 in table 2 as it can be seen that the molar ratio of hydrogen bond donor and hydrogen bond receptor in the larger context
It adjusts, also disclosure satisfy that plant extract, realize higher extraction efficiency;Meanwhile the ratio of medicine material and solvent is in larger model
Interior adjusting is enclosed, still disclosure satisfy that higher extraction efficiency.
Use carbohydrate, amino acid and organic salt according to optimization as it can be seen that working as by embodiment 1 in table 2 and 5 measurement result of embodiment
Molar ratio, water content, liquid ratio and reaction condition when extracting, extraction efficiency is higher, but is used under similarity condition
Carbohydrate, glycitols and organic salt extract, and extraction efficiency is some higher.
By the measurement result of embodiment 2 in table 2 as it can be seen that only with a kind of hydrogen bond donor in the present invention and a kind of hydrogen bond receptor Lai
Prepare eutectic solvent, be equally reached preferable extraction effect, also indicate that simultaneously, water content, molar ratio, hydrogen bond donor and
Hydrogen bond receptor can also meet higher extraction efficiency in wide range adjusting.
By embodiment 5 in table 2 or 6 measurement result comparison as it can be seen that according to optimization molar ratio, water content, plant material
When being extracted with liquor ratio and reaction condition with organic solvent, higher extraction efficiency can be obtained.
By the measurement result of embodiment 5 and embodiment 6 in table 2 as it can be seen that extraction time is appropriately extended, can obtain preferably
Extraction effect.
By the measurement result of embodiment 7 in table 2 as it can be seen that being prepared with two kinds of substances of glycitols and organic media natural low total
Molten solvent, can also extract peony extract, reach preferable extraction effect.
By embodiment 8 in table 2 and 9 measurement result of embodiment as it can be seen that with organic salt, carbohydrate, glycols formulated in combination it is low
Congruent melting solvent equally can obtain higher extraction efficiency.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from the present invention's
Many other change and modification can be made in the case of spirit and scope.It is, therefore, intended that wrapping in the following claims
Include all such changes and modifications belonged in the scope of the invention.
Claims (10)
1. a kind of natural eutectic solvent, which is characterized in that including hydrogen bond donor and hydrogen bond receptor;
The hydrogen bond donor includes arbitrary two kinds of the combination in glycols, amino acid, carbohydrate or glycitols;
The hydrogen bond receptor includes organic salt;
Natural eutectic solvent water content is 10~50%.
2. according to natural eutectic solvent described in claim 1, which is characterized in that the glycols is butanediol or 1,3- the third two
Alcohol;
Preferably, the amino acid is glycine or phenylalanine;
Preferably, the carbohydrate is one kind in fructose, glucose, sucrose or lactose;
Preferably, the glycitols is one kind in glycerine, xylitol, sorbierite, maltitol or mannitol;
Preferably, the organic salt is glycine betaine or choline.
3. natural eutectic solvent described in accordance with the claim 1, which is characterized in that the hydrogen bond of the natural eutectic solvent supplies
Body is arbitrary two kinds of the combination in carbohydrate, amino acid or glycitols.
4. according to the natural eutectic solvent of claim 1-3 any one of them, which is characterized in that the natural eutectic solvent
The molar ratio of middle hydrogen bond receptor and hydrogen bond donor is (1:8)~(5:1), preferably (1:5)~(2:1), further preferably (1:
2)~(2:1).
5. natural eutectic solvent according to claim 4, which is characterized in that the natural eutectic solvent includes fruit
The molar ratio of sugar, glycerine and glycine betaine, fructose, glycerine and glycine betaine is (1~4):(1~3):(4~1).
6. a kind of application of natural eutectic solvent of claim 1-5 any one of them in plant extract;
Preferably, the plant is ginseng, pot marigold or Chinese herbaceous peony, further preferably Chinese herbaceous peony.
7. applying according to claim 6, which is characterized in that include the following steps:
Pretreated plant fragment is placed in prepared natural eutectic solvent and is extracted, is carried out after separation, impurity removal
Concentration, obtains plant extraction liquid.
8. applying according to claim 7, which is characterized in that the separation, impurity removal mode is centrifugation;Preferably, described dense
It is condensed to nanofiltration concentration;
Preferably, preservative is added after concentration, obtains plant extraction liquid.
9. according to claim 7-8 any one of them applications, which is characterized in that plant fragment and natural eutectic solvent
Ratio is 0.1~0.8g/ml (w/v), preferably 0.1~0.3g/ml (w/v).
10. according to the application of claim 7-8 any one of them, which is characterized in that extraction time is 30~60min, extraction
Temperature is 30~55 DEG C;
Preferably, extraction time is 50~60min, and Extracting temperature is 40~50 DEG C.
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