CN108586241A - The method of ultrasonic-microwave-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid - Google Patents
The method of ultrasonic-microwave-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid Download PDFInfo
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Abstract
A kind of method of ultrasonic microwave aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid：Inorganic salts are added in the ethanol water of volume fraction 35% 65%, i.e., split-phase becomes aqueous two-phase extractant；Sweet potato leaves powder is added in gained aqueous two-phase extractant, 5 10min of ultrasonic extraction under conditions of ultrasonic power is 180 220W, temperature is 25 35 DEG C, later 60 90s are extracted under the conditions of microwave power is 480 800W, it filters, take filtrate, the extracting solution of upper and lower split-phase is obtained, upper and lower two-phase is separated, supernatant liquid and lower liquid are obtained；By gained supernatant liquid vacuum distillation concentration, it is dried in vacuo to get finished solid chlorogenic acid；The method of the present invention is easy to operate, process integration, rapid efficient, environmental-friendly, is easy to technique amplification and continuous operation.
Description
(1) technical field
The present invention relates to the extraction separation methods of sweet potato leaves chlorogenic acid, and in particular to a kind of ultrasonic-microwave-aqueous two-phase association
With the method for extraction separation sweet potato leaves chlorogenic acid.
(2) background technology
Sweet potato (scientific name：Ipomoea batatas) also known as sweet potato, sweet potato, sweet potato, pachyrhizus etc., it is the annual grass of Convolvulaceae
This plant.According to the statistical result showed of FAO (Food and Agriculture Organization of the United Nation) (FAO), there is more than 100 country plantation sweet potato in the whole world.Mesh
Before, Asia and Africa become the main growing area of sweet potato.Sweet potato is a kind of staple food crop in China, the plantation of the whole nation from the leadership to the masses
Area about 6.16 × 106hm2, total output has 1.7 × 1012Kg, cultivated area and total output are all global the first.It is the world the 7th
One of main cereal crops of generalized grain crop and China.Byproduct one of of the sweet potato leaves as sweet potato, rich in polyphenol, egg
The nutritional ingredients such as white matter, vitamin and mineral, nutritive value are high, have improve immunity, it is anti-oxidant, boost metabolism
Various health care functions.In areas such as Japan, Taiwan, sweet potato leaves have become a kind of novel vegetables.Chlorogenic acid in sweet potato
Have the effects that be depressured kidney tonifying, enhancing immunity of organism, antitumor, anti-oxidant, anti-aging, diuresis, cholagogic and reducing blood lipid.
Chlorogenic acid is the organic acid containing carboxyl and o-phenol hydroxyl, and the chlorogenic acid contained in sweet potato leaves is mostly with glucosides
Form exists, soluble easily in water, alcoholic solution and acetone equal solvent.Chlorogenic acid generally mostly use water, methanol, ethanol solution do extraction it is molten
Agent is extracted.Extracting method is currently used mainly have microwave method, supercritical ultrasonics technology, enzymatic isolation method, extraction, supercritical fluid extraction,
The methods of semi-bionic extraction, aqueous two-phase extraction method, liquid-film method, soxhlet extraction.But select extractant often toxicity compared with
Greatly, extraction time is also longer, time consumption and energy consumption, and recovery rate is low.
Ultrasonic wave extraction is to utilize the strong cavitation effect of Ultrasonic Radiation pressure generation, disturbance effect, high acceleration
It spends, smash and the multistage effect such as stirring action, increase molecular motion of material frequency and speed, increase solvent penetration power, to add
Fast target component enters solvent, promotes the progress of extraction.But ultrasonic wave extraction can not destroy the constraint of cell wall, nothing completely
Method extracts active ingredient and is adequately detached to the maximum extent.
Microwave assisted techniques be using the volume heating of microwave field and the function that selectively heats, accelerate extraction process into
Row.It selects to microwave or translucent and there is the medium of stronger solvability to make solvent target component, in microwave field
In, the material internal molecule opaque to microwave is mutually collided under microwave action, is squeezed, and is conducive to the quick leaching of target component
Go out.Microwave method has highly selective and high efficiency, while substantially reducing the reaction time, and can improve reaction yield.
Aqueous two phase extraction technique (Aqueous Two-Phase Extraction ATPS) is by two kinds of chemical constitution differences
Hydrophilic polymer or polymer and inorganic salts form immiscible two-phase in water, according to substance in two alternate selections
Property distribution achieve the purpose that detach target substance, be the new of the great development prospect studied and grown up in recent decades
Type extraction and separation technology, also known as aqueous solution two-phase partitioning technology, aqueous two phase extraction technique is due to its mild condition, mass transport
Soon, at low cost, it is easy to operate, it is adjusted, amplification is easy, the features such as can operating continuously, with traditional organic solvent extraction system phase
Compare, there is original superior place in the separation of biological substance.Traditional high polymer/high polymer or high polymer/inorganic salt is double
Aqueous phase system has been used successfully to detach and extract various protein (polypeptide and enzyme), has detached and extract various antibiotic, amino
The fields such as the effective ingredient of acid, metal and Chinese medicine.
The double-aqueous phase system that high polymer is formed, although extraction efficiency is high, polyethylene glycol (abbreviation PEG) used and Portugal are poly-
Sugared (abbreviation Dextran) cost is too high, and system large viscosity, and recycling is difficult, thus of high cost, is unsuitable for industrial-scale life
Production.And lower alcohol (such as ethyl alcohol) is low with the double-aqueous phase system toxicity that the aqueous solution of salt is formed, the reclaimer operation letter to organic solvent
Just, it can recycle, it is at low cost.Its principle is the hydration using salt ion, competes hydrone jointly with ethyl alcohol to shape
At the aqueous solution two-phase of ethanol water and salt.When the active ingredient in biological substance or natural products enters double-aqueous phase system
When, due to surface nature, the presence of charge effect and various power (hydrophobic key, hydrogen bond and ionic bond) and environmental factor (concentration, temperature
Degree, the type of pH value and ion and intensity etc.) influence, the active ingredient in biological substance or natural products is easily alternate two
Form the distribution of selectivity.
Currently, research report of the double-aqueous phase system (ATPS) for chlorogenic acid to isolate and purify is relatively more, but it is directly used in and carries
Take the few of chlorogenic acid.A kind of preparation side of honeysuckle chlorogenic acid of the Introduction To Cn Patent of Publication No. CN102001947A
Method：Use honeysuckle and its branches and leaves for raw material, water carry after with water-miscible organic solvent and salting liquid and water-soluble compound by than
Example composition double-aqueous phase system, is then dissolved in total extract medicinal extract in double-aqueous phase system and is allocated, make up to medicinal extract and exist
Mean concentration in two-phase is 30~50% partition equilibrium, then is extracted with the extractant immiscible with two water phases, separates
Extract liquor, the impurity for first polarity being less than chlorogenic acid remove, and remaining aqueous two-phase is extracted with the three-phase that another extractant is extracted again
Take method, selectively direct enrichment and separation purifies to obtain chlorogenic acid head product, after by decoloration, crystallize and be dried to obtain matter
Amount score is 95% chlorogenic acid product.This method first extracts plant component with extractant, obtains extracting solution after filtering, then to extraction
Double-aqueous phase system and extractant are added in liquid, extraction, liquid separation obtain main component, and step is more, and the time is long.Publication No.
The Introduction To Cn Patent of CN103420838A (application number CN201310339674.X) is a kind of to utilize temperature-induced aqueous two-phase body
It is the method for isolating and purifying chlorogenic acid, includes the following steps：(1) it is put into extractor after crushing folium cortex eucommiae, 5 is added thereto
The water of~7 times of weight, is heated to reflux 1.5~2h, is concentrated into medicinal extract, as chlorogenic acid crude product；(2) by volume by EOPO and water
1~3: 1~4 mixing, are then added salt thereto, are uniformly mixed, and chlorogenic acid crude product is added into solution, after mixing, from
The heart detaches water phase and the organic phase rich in EOPO, and chlorogenic acid is enriched in organic phase, and impurity is enriched in water phase；(3) step (2) are obtained
For the organic phase arrived in 50~70 DEG C of 10~30min of water-bath, solution is automatically separated into two-phase, centrifuges organic phase and water phase, green original
Acid is enriched in water phase, and EOPO is enriched with and is recycled in organic phase；(4) obtained water phase is cooled to room temperature, is stood overnight, analysed
Go out crystallization, chlorogenic acid pure product is obtained by filtration.This method equally exists the problem that step is more, and the time is grown.
(3) invention content
For the deficiencies in the prior art, the present invention proposes a kind of side of new extraction separation sweet potato leaves chlorogenic acid
Method, the method is directly made into double-aqueous phase system solution with aqueous solutions of organic solvent and a certain amount of inorganic salts, as extractant
Ultrasonic wave, microwave cooperating chlorogenic acid extracting are carried out, is extracted in extraction, step is few, the time is short, efficient.
The present invention cooperates with extractive technique using ultrasonic-microwave-aqueous two-phase, and the ethyl alcohol organic solvent used is to environment and people
The product purity of member's safety, acquisition is high, no solvent residue, and extraction process is simple, is easy to continuous operation, mild condition, while ring
Border is friendly, of low cost.
Technical scheme is as follows：
A kind of method of ultrasonic-microwave-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid, the method is by following step
It is rapid to carry out：
(1) aqueous two-phase extractant is prepared
Inorganic salts are added in the ethanol water of volume fraction 35%-65%, i.e., split-phase becomes aqueous two-phase extractant；
Mass fraction of the inorganic salts in gained aqueous two-phase extractant is 10%-30%；
The inorganic salts are three water dipotassium hydrogen phosphates, potassium dihydrogen phosphate, potassium carbonate or ammonium sulfate；It is preferred that three water phosphoric acid hydrogen two
Potassium；
(2) ultrasonic-microwave-aqueous two-phase collaboration extraction
Sweet potato leaves powder is added in aqueous two-phase extractant obtained by step (1), ultrasonic power is 180-220W, temperature is
Ultrasonic extraction 5-10min under conditions of 25-35 DEG C extracts 60-90s under the conditions of microwave power is 480-800W later, filters,
Filtrate is taken, the extracting solution of upper and lower split-phase is obtained, upper and lower two-phase is separated, supernatant liquid and lower liquid are obtained；It will be on gained
Layer liquid pressure-reducing distillation and concentration (vacuum degree 0.1MPa, 30-45 DEG C of temperature), vacuum drying are to get finished solid chlorogenic acid；Gained
Lower liquid is cooled to 0~10 DEG C, and inorganic salt crystal is precipitated, and is recovered by filtration；
The solid-liquid ratio of the sweet potato leaves powder and aqueous two-phase extractant is 1：50-120 (w/v, g/mL), preferably 1：80~100；
The sweet potato leaves powder is made by raw material sweet potato leaf through drying, crushing.
The present invention makees solvent in extraction process using double-aqueous phase system, and at the operational, also split-phase is apparent for two-phase,
Sweet potato leaves powder is suspended between two-phase just, be soluble in ethyl alcohol phase chlorogenic acid extract after enter upper phase, be soluble in water phase
Polysaccharide is dissolved in lower phase.In this way, extraction and separation process are carried out at the same time.Sweet potato leaves chlorogenic acid significant enrichment is several in upper phase, lower phase
Do not have, the mass fraction by changing the salt being added changes the volume of upper and lower phase, the upper phase volume of reductions, reaches to be enriched with and concentrates
Purpose, sweet potato leaves chlorogenic acid is soluble in weakly alkaline solution, double water that dipotassium hydrogen phosphate is formed with ethyl alcohol due to its design feature
Phase extractant is alkalescent, is conducive to the dissolution of sweet potato leaves chlorogenic acid.It is experimentally confirmed that from yield and sweet potato leaves chlorogenic acid upper and lower
From the point of view of the distribution condition of phase, the effect of dipotassium hydrogen phosphate is all undoubtedly best.
Compared with the prior art, the advantage of the invention is that：
1, easy to operate, without waiting for split-phase
It observes in an experiment, after salt, ethanol water are mixed, sweet potato leaves powder, which is added, can enter extraction step, no
With waiting for split-phase apparent, yield is constant.
2, process integration
Extraction, extraction and separation and enriching step are integrated into onestep extraction mistake by ultrasonic-microwave-aqueous two-phase collaboration extraction method
Journey, it is simple to operate, complete extracting and enriching in extraction process, by sweet potato leaves chlorogenic acid and sweet potato leaf polyose and other easily
The component being soluble in the aqueous phase separates, and sweet potato leaves chlorogenic acid is enriched in phase, and cycles of concentration is up to 4 times or more.
3, extraction process is rapid, efficiently
The strong cavitation effect that is generated by Ultrasonic Radiation pressure, high acceleration, smashes and stirring action disturbance effect
Deng multistage effect and microwave irradiation effect, the extraction process for needing several hours originally was foreshortened within 15 minutes, sweet potato leaves
The high income of chlorogenic acid.
4, Extraction solvent low toxicity
Extractant is made using ethyl alcohol/inorganic salts aqueous two-phase, avoids the use of toxic solvent such as acetone, raw material environmental protection.
5, interfacial tension is small, contributes to the mass transfer between two-phase
The double-aqueous phase system, upper phase are organic solution ethyl alcohol, and lower phase is the solution of salt, up and down the interfacial surface tension of phase
Small, free energy is small, contributes to the transmission of substance between two-phase.
6, a large amount of impurity can remove together with solid matter, be conducive to purification of samples
After extraction, solid residue is suspended between two-phase or lower phase, and a large amount of impurity can enter lower phase with residue, and red
Potato leaf chlorogenic acid separates.
7, the extracting method is easy to technique amplification and continuous operation, can be connected directly with subsequent purification process, without carrying out
Specially treated.
(4) specific implementation mode
Below by way of specific embodiment, the invention will be further described, but protection scope of the present invention is not limited in
This.
Ultrasonic extraction uses KQ5200DE type numerical control ultrasonic cleaners, Microwave Extraction to use Glanz in following embodiment
Micro-wave oven D80D20EP-A3 types.
Embodiment 1：
(1) double-aqueous phase system is prepared
Take 5g K2HPO4·3H2O is added 50% ethyl alcohol of 50mL, is formulated as aqueous two-phase extractant.
(2) ultrasonic-microwave-aqueous two-phase collaboration extraction
Gained double-aqueous phase system 25mL in step (1) is taken, the sweet potato leaves powder 0.5g of accurately weighed 60 mesh of mistake sieve, material is added
Liquor ratio 1:50 (g/mL), set ultrasound condition as 200W, 30 DEG C of processing time 8min, then microwave treatment conditions be 480W,
1.5min carries out the collaboration extraction of ultrasonic-microwave-aqueous two-phase, after extraction, filter apparent split-phase sweet potato leaves chlorogenic acid
Extracting solution, recovery rate 4.26%.Upper and lower two-phase is separated, supernatant liquid is taken, through reduced pressure (vacuum degree 0.1MPa, temperature 40
DEG C), vacuum drying (60 DEG C, 3.5h), obtain solid chlorogenic acid 0.0326g, yield 6.5%, purity 65.3%.
The sweet potato leaves chlorogenic acid extracting solution of apparent split-phase can utilize determined by ultraviolet spectrophotometry wherein sweet potato in step (2)
The concentration of leaf chlorogenic acid, and press formula (3) calculated yield：
R=VOn/VUnder (1)
K=COn/CUnder (2)
Y=COn×VOn/ M × 100% (3)
In formula：R be compared to；VOnAnd VUnderThe volume (ml) of phase up and down；COn, CUnderIt is target isolate in upper and lower phase respectively
Mass concentration (mg/ml)；K is distribution coefficient；Μ is the quality for the sweet potato leaves powder being added.
The assay of chlorogenic acid uses spectrophotometry.It is as follows：Weigh a certain amount of sweet potato leaves chlorogenic acid
Extracting solution does reference with blank solution, and absorbance is measured at 328nm, substitutes into standard curve and calculates containing for sweet potato leaves chlorogenic acid
Amount.
Embodiment 2：
(1) double-aqueous phase system is prepared
Take 5g K2HPO4·3H2O is added 50mL50% ethyl alcohol, is formulated as aqueous two-phase extractant；
(2) ultrasonic-microwave-aqueous two-phase collaboration extraction
Gained double-aqueous phase system 40mL in step (1) is taken, the sweet potato leaves powder 0.5g of accurately weighed 60 mesh of mistake sieve, material is added
Liquor ratio 1:80 (g/mL), set ultrasound condition as 220W, 35 DEG C of processing time 5min, then microwave treatment conditions be 800W,
1min carries out the collaboration extraction of ultrasonic-microwave-aqueous two-phase, after extraction, filter the sweet potato leaves chlorogenic acid of apparent split-phase carries
Take liquid, recovery rate 4.32%.Upper and lower two-phase is separated, supernatant liquid is taken, through reduced pressure (vacuum degree 0.1MPa, temperature 45
DEG C), vacuum drying (60 DEG C, 3.5h), obtain solid chlorogenic acid 0.0333g, yield 6.66%, purity 64.9%.
Embodiment 3：
(1) double-aqueous phase system is prepared
Take 5g K2HPO4·3H2O is added 50mL50% ethyl alcohol, is formulated as aqueous two-phase extractant；
(2) ultrasonic-microwave-aqueous two-phase collaboration extraction
Gained double-aqueous phase system 50mL in step (1) is taken, the sweet potato leaves powder 0.5g of accurately weighed 60 mesh of mistake sieve, material is added
Liquor ratio 1:100 (g/mL), set ultrasound condition as 180W, 25 DEG C of processing time 10min, then microwave treatment conditions be 560W,
1.5min carries out the collaboration extraction of ultrasonic-microwave-aqueous two-phase, after extraction, filter apparent split-phase sweet potato leaves chlorogenic acid
Extracting solution, recovery rate 4.42%.Upper and lower two-phase is separated, supernatant liquid is taken, through reduced pressure (vacuum degree 0.1MPa, temperature 40
DEG C), vacuum drying (60 DEG C, 3.5h), obtain solid chlorogenic acid 0.0324g, yield 6.49%, purity 63.5%.
Embodiment 4：
(1) double-aqueous phase system is prepared
Take 10g K2HPO4·3H2O is added 50% ethyl alcohol of 100mL, is formulated as aqueous two-phase extractant；
(2) ultrasonic-microwave-aqueous two-phase collaboration extraction
Gained double-aqueous phase system 60mL in step (1) is taken, the sweet potato leaves powder 0.5g of accurately weighed 60 mesh of mistake sieve, material is added
Liquor ratio 1:120 (g/mL), set ultrasound condition as 200W, 30 DEG C of processing time 8min, then microwave treatment conditions be 560W,
1min carries out the collaboration extraction of ultrasonic-microwave-aqueous two-phase, after extraction, filter the sweet potato leaves chlorogenic acid of apparent split-phase carries
Take liquid, recovery rate 4.48%.Upper and lower two-phase is separated, supernatant liquid is taken, through reduced pressure (vacuum degree 0.1MPa, temperature 30
DEG C), vacuum drying (62 DEG C, 3.5h), obtain solid chlorogenic acid 0.0348g, yield 6.97%, purity 64.3%.
Embodiment 5：
(1) double-aqueous phase system is prepared
Take 5g K2HPO4·3H2O is added 50mL50% ethyl alcohol, is formulated as aqueous two-phase extractant；
(2) ultrasonic-microwave-aqueous two-phase collaboration extraction
Gained double-aqueous phase system 25mL in step (1) is taken, the sweet potato leaves powder 0.5g of accurately weighed 60 mesh of mistake sieve, material is added
Liquor ratio 1:50 (g/mL), set ultrasound condition as 220W, 30 DEG C of processing time 5min, then microwave treatment conditions be 480W,
1min carries out the collaboration extraction of ultrasonic-microwave-aqueous two-phase, after extraction, filter the sweet potato leaves chlorogenic acid of apparent split-phase carries
Take liquid, recovery rate 4.23%.Upper and lower two-phase is separated, supernatant liquid is taken, through reduced pressure (vacuum degree 0.1MPa, temperature 45
DEG C), vacuum drying (60 DEG C, 4h), obtain solid chlorogenic acid 0.0325g, yield 6.50%, purity 65.1%.
Comparative example
Xie Renyou etc.：" technical study of ultrasonic wave assisted extraction Sweet Potato Leaf Content of Chlorogenic Acid " the result shows that：In optimum extraction
Condition is：Concentration of alcohol 60%, solid-liquid ratio 1：30, ultrasonic time 50min, the extraction of Sweet Potato Leaf chlorogenic acid at 50 DEG C of ultrasonic temperature
Rate is up to 3.42%.
Zhang Chunyan etc.：" optimization of the response phase method to sweet potato leaves and stems chlorogenic acid ultrasonic extraction process " the result shows that：Optimizing
Combination condition is volumes of aqueous ethanol score 70%, solid-liquid ratio 1：20, under ultrasonic time 24min, chlorogenic acid yield is
3.0972%.
It can be seen that compared with ultrasonic wave assisted extraction, extraction time of the invention can be obviously shortened, and recovery rate also has aobvious
It writes and improves.
Claims (6)
1. a kind of method of ultrasonic-microwave-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid, which is characterized in that the side
Method carries out as follows：
(1) aqueous two-phase extractant is prepared
Inorganic salts are added in the ethanol water of volume fraction 35%-65%, i.e., split-phase becomes aqueous two-phase extractant；
Mass fraction of the inorganic salts in gained aqueous two-phase extractant is 10%-30%；
The inorganic salts are three water dipotassium hydrogen phosphates, potassium dihydrogen phosphate, potassium carbonate or ammonium sulfate；
(2) ultrasonic-microwave-aqueous two-phase collaboration extraction
Sweet potato leaves powder is added in aqueous two-phase extractant obtained by step (1), ultrasonic power be 180-220W, temperature 25-
Ultrasonic extraction 5-10min under conditions of 35 DEG C extracts 60-90s under the conditions of microwave power is 480-800W later, filters, takes
Filtrate obtains the extracting solution of upper and lower split-phase, and upper and lower two-phase is separated, supernatant liquid and lower liquid are obtained；By gained upper layer
Liquid pressure-reducing distillation and concentration, vacuum drying are to get finished solid chlorogenic acid；
The solid-liquid ratio of the sweet potato leaves powder and aqueous two-phase extractant is 1：50-120.
2. the method for ultrasonic-microwave as described in claim 1-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid, special
Sign is, in step (1), the inorganic salts are three water dipotassium hydrogen phosphates.
3. the method for ultrasonic-microwave as described in claim 1-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid, special
Sign is, in step (2), the sweet potato leaves powder is made by raw material sweet potato leaf through drying, crushing.
4. the method for ultrasonic-microwave as described in claim 1-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid, special
Sign is, in step (2), the solid-liquid ratio of the sweet potato leaves powder and aqueous two-phase extractant is 1：80~100.
5. the method for ultrasonic-microwave as described in claim 1-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid, special
Sign is, in step (2), the lower liquid is cooled to 0~10 DEG C, and inorganic salt crystal is precipitated, and is recovered by filtration.
6. the method for ultrasonic-microwave as described in claim 1-aqueous two-phase collaboration extraction separation sweet potato leaves chlorogenic acid, special
Sign is, in step (2), the vacuum degree 0.1MPa of the supernatant liquid vacuum distillation concentration, and 30-45 DEG C of temperature.
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