CN104096381B - Method for extracting effective components of natural products through mixing of ethyl alcohol and sub-critical fluid - Google Patents
Method for extracting effective components of natural products through mixing of ethyl alcohol and sub-critical fluid Download PDFInfo
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Abstract
The invention discloses a method for extracting effective components of natural products and relates to a method for extracting water-soluble and fat-soluble effective components in the natural products simultaneously, particularly to a method for extracting the effective components of the natural products through mixing of ethyl alcohol and a sub-critical fluid, and belongs to the field of extraction of the effective components of the natural products. According to the method which is a new extraction and separation technology, the ethyl alcohol and the sub-critical fluid are mixed to serve as an extracting solvent, in a closed, oxygen-free and low-pressure extracting tank, all the components are separated and purified respectively through three steps, namely, extraction, desolventizing as well as membrane separation-macroporous adsorbent resin combined separation, and finally, high-purity water-soluble component and fat-soluble component extracts of the natural products are obtained; the method has a broad application prospect in the industry.
Description
Technical field
The invention discloses a kind of extracting method of active ingredient of natural product, and in particular to while in extracting natural products
A kind of method of water-soluble and fat-soluble active ingredient, more particularly to ethanol and subcritical fluids hybrid extraction natural products
The method of active ingredient, belongs to active ingredient of natural product extraction field.
Background technology
Constituent or its metabolite and humans and animals in animal, plant, insect, marine organisms and microbial body
Internal many endogenic chemical compositions are referred to as natural products, wherein mainly including protein, polypeptide, amino acid, nucleic acid, each
Kind of enzyme, monose, oligosaccharides, polysaccharide, glycoprotein, resin, colloid substances, lignin, vitamin, fat, grease, wax, alkaloid, wave
Hair oil, flavones, glycoside, terpene, Phenylpropanoid Glycosides class, organic acid, phenols, quinones, lactone, steroidal compounds, tannins, antibiotic
The naturally occurring chemical composition such as class, water-soluble and fat-soluble two major class can be divided into according to its dissolubility.At present in natural products
In active ingredient extraction field, conventional method mainly has solvent method, milling process, the way of distillation and sublimed method etc..
Solvent extraction method is mainly boiled including decocting, etc. Solvent Extract methods.When using water as solvent, to liposoluble constituent
Extraction effect it is just relatively not good enough；Harm and influence of the hydrophilic organic solvents such as methyl alcohol on human body and environment can not be ignored.
And this several method is although commonly used, but loss of effective components would generally be caused, especially liposoluble constituent；Removed in extract solution
Outside active ingredient, often impurity is more, brings unfavorable to refined；High-temperature operation can cause a large amount of points of thermal sensitivity active ingredient
Solution.As Chinese patent 200910201558.5 announce it is " a kind of to extract simultaneously water-soluble in the natural products red sage root and fat-soluble have
The method for imitating composition ", in its technique using infra-red radiation heat release extract simultaneously in the red sage root it is water-soluble and fat-soluble effective into
Point, Extraction solvent used is the mixed solvent of water and organic solvent (alcohols such as methyl alcohol, ethanol) composition, using water as extraction water
The essence of the solvent of soluble components, Solvent Extract methods liposoluble constituent, but its mixed solvent is still certain density alcoholic solution.
In subcritical water and subcritical ethanol extraction process, although can by controlling extracting pressure and temperature, make water or
The polarity of ethanol in interior change in a big way, to realize the active ingredient of natural products from the continuous of water-soluble and liposoluble constituent
Extract, and selective extraction.201010500500.3 disclose subcritical water extracts various biologies in Chinese yam as medium simultaneously
The method of active component, although utilize Subcritical water chromotagraphy method by Water-soluable Polysaccharide from Rhizoma Dioscoreae Opposite, allantoin and fat-soluble Dioscin
Extract simultaneously, realize continuous extraction, but its extraction process is completed by three step temperature-rise periods, complex steps, and extract temperature
Degree is higher than 100 DEG C, the structure of par-tial polysaccharide can be destroyed, so as to influence yield.The patent of Subcritical water chromotagraphy, document report, greatly
Mostly it is, using the selective extraction of subcritical water, to realize water soluble ingredient (such as：A kind of Asia of Patent No. 201110002219.1 is faced
The method that boundary's water extracts rice bran polysaccharide) or liposoluble constituent is (such as：201310301124.9 subcritical fennel essential oil water extraction
Preparation method) extraction with separate.In subcritical ethanol extraction method, Patent No. 201010136309.5 is a kind of using subcritical
The method that alcohols extracts grease from the wet algae mud of microalgae, its Extracting temperature is higher than 78.4 DEG C, can destroy thermal sensitivity in natural products
The activity of material.At present, single subcritical fluids (propane, butane, dimethyl ether, HFC-134a) extraction, is particularly suitable for natural
The extraction of liposoluble constituent in product, and the abundant extraction of water soluble ingredient can not be realized.
Above difference extracting process cuts both ways, it is difficult to accomplish that water-soluble and fat-soluble active ingredient takes into account extraction, therefore
A kind of low temperature, efficient, environmental protection are found, while the extracting method for taking into account liposoluble constituent and water soluble ingredient is particularly important.
The content of the invention
The technical problems to be solved by the invention, day is extracted using ethanol and subcritical fluids mixing simultaneously as extractant
Right water in products, fat component, are efficiently modified the weak point of traditional extracting and developing, purifying and concentration process method, in shorter week
Purity product relatively higher, and environmentally friendly, can largely to retain heat-sensitive substance activity, extraction cost phase are obtained in phase
To it is cheap, industrial-scale production can be carried out.It is specifically described below and realizes method of the present invention step and implementation：
1) extract：To be put into closed extractor by the material of pretreatment, vacuumized, to injection certain proportion one in tank
The ethanol solution and appropriate subcritical fluids of volume fraction are determined as mixed solvent, material are totally submerged, in extraction process
In can aid in stirring to improve efficiency.According to the different qualities of material, material, subcritical fluids and ethanol solution addition
Mass volume ratio (w/v/v) is 1:1~50:1~50, the volume fraction of ethanol solution is 50%~95%, and extraction time is 10
~120min, temperature is 0~50 DEG C, and stir speed (S.S.) is 50~1000rpm, is extracted 1~4 time, and pressure is under corresponding extraction temperature
The saturated vapour pressure of corresponding mixed solvent.
2) precipitation：After extraction terminates, slowly liquid flux is put into knockout drum completely, extractor and knockout drum are entered respectively
Row evaporation carrying out precipitation treatment, precipitation completes to obtain the mixed extract comprising liposoluble constituent Yu water soluble ingredient simultaneously；Then
The subcritical solvent gas evaporated from extractor and knockout drum, compress and liquefy by diaphragm type compressor, flow back to solvent storage
Tank, recycles.
3) UF membrane：Mixed solvent extract, it is miscellaneous by the way that (1000~8000rpm) pretreatment removal part solidity is centrifuged
Matter, afterwards by 0.05 μm~0.2 μm microfiltration membranes, insoluble solid particle, thalline and big point on a small quantity in retention removal extract solution
Sub- material；Retained with 5000~20000Da milipore filters again and remove the impurity such as isolating protein, tannin and colloidal substance, by counter-infiltration
Film (CAM, doughnut reverse osmosis membrane) ultrafiltration concentration liquid, to remove a small amount of small-molecule substance, UF membrane operation is whole
Individual process, completes in model HC-DGM25-2X multifunctional membranes experimental system (Chengdu and sincere filtering technique Co., Ltd).
4) resin is separated：Membrane separating and purifying liquid by optimal type macroporous absorbent resin (such as D-101, DA-201, AB-
8th, D-301 etc.) absorption, the ethanol solution (25%~95%) of desired volume fraction is selected, from natural product extraction liquid, finally
The liposoluble substance and water-soluble substances of isolated high-purity.
The material can be the natural plants, microorganism or animal of fresh (or through dried process), and conventional method
Extract and separate halfway or impurity content extract high etc..
The subcritical solvent is effumability organic solvent, it is easy to which solid-liquid is completely separated, including propane, butane, diformazan
The mixing of one or more in ether, HFC-134a.
The mass volume ratio (w/v/v) of the material, subcritical fluids and ethanol solution addition is 1:1~50:1~
50。
The volume fraction of the ethanol solution is 50%~95%.
The mixing extraction conditions：Temperature is 0~50 DEG C, and pressure is corresponding saturated vapour pressure, time under relevant temperature
It is 10~120min, stir speed (S.S.) is 50~1000rpm.
Subcritical solvent reusable edible after the precipitation.
The isolated liposoluble substance can respectively carry out follow-up working process with water-soluble substances.
The extract solution pretreatment centrifugal rotational speed is 1000~8000rpm.
20~40 DEG C of described UF membrane temperature.
The film is micro-filtration (MF0.05~10 μm), ultrafiltration (UF1~100nm), nanofiltration (NF1~10nm) and counter-infiltration
In (RO≤1nm) one or more.
The macroreticular resin can be D-101 types, DA201 types, SIP series, X-5 types, AB-8 types, GDX-104 types, LD-605
Type, LD-601 types, CAD-40 types, DM-130 types, R-A types, CHA-111 types, WLD types (mixed type), H-107 types, NKA-9 types etc.
In one or more.
The volume fraction range of the macroporous absorbent resin eluting solvent ethanol solution is 25%~95% (for different materials
Wash-out concentration used by the heterogeneity of material is different, and listed is total ethanol volume range, concrete condition concrete analysis).
The present invention is mixed as extractant by the use of ethanol and subcritical fluids, in closed, anaerobic, the extractor of low pressure
It is interior, according to the similar principle for mixing of organic matter, by material and molecule diffusion process of the extractant in immersion process, make thing
Liposoluble constituent and water soluble ingredient in material are transferred in extractant, finally by the process of reduction vaporization by mixed extract
In subcritical fluids removing, each component is isolated and purified respectively with reference to UF membrane-macroporous absorbent resin GC-MS, most
The high-purity water soluble components of natural products and a kind of novel extraction of fat soluble component extract and isolation technics are obtained eventually.
It is of the invention to be advantageous in that：
1) extraction process：Process is simple, equipment investment are low, are adapted to large-scale production；Extraction temperature is relatively low (under normal circumstances
It is room temperature), the natural activity of heat-sensitive substance will not be destroyed；Product extraction degree is high, cycle is short, efficiency high；Mixed solvent
Use, increased liposoluble constituent and the selectivity and efficiency of water soluble ingredient extraction in natural products；Solvent reusable edible,
Environment will not be polluted, isolated liposoluble constituent is below with water soluble ingredient Subcritical dissolvent residual
1ppm。
2) separate, purify and concentration process：UF membrane-macroporous absorbent resin is combined the selection of mechanism, it is to avoid impurity is to tree
The pollution of fat post, increased the service life of resin column, and isolate product purity be higher than only with a kind of method separate concentration
Purity.
Active ingredient in natural products is obtained with ethanol and subcritical fluids hybrid extraction technology, with reference to UF membrane-big
Hole resin adsorption is isolated and purified to the sample for being extracted, overcome traditional extraction method (such as decocting boil, solvent extraction) and
The cycle is long, efficiency is low, impurity-eliminating effect is undesirable for partition method (such as solvent extraction and separation, precipitate and separate), loss of effective components etc.
Shortcoming, can be to obtain the natural products water soluble ingredient of high-purity and a kind of novel extraction of fat soluble component extract and divide
From technology.
Brief description of the drawings
Fig. 1 extracts flow chart
Specific embodiment
Embodiment 1
200g locust trees (water content ﹤ 13%) are taken, is crushed and after 80 mesh sieve excessively, is placed in closed extractor, add volume
Fraction is 70% ethanol 1800mL, after closing feeding-passage, is evacuated to vacuum, to diformazan ether solvents are injected in extractor, by material
It is totally submerged, the mass volume ratio (w/v/v) of material, subcritical dimethyl ether and ethanol solution addition is 1:6:9.It is in temperature
25 DEG C (pressure be relevant temperature under corresponding saturated vapour pressure), under conditions of stir speed (S.S.) is 700rpm, extracts 50min；Extraction
After taking end, slowly mixed solvent is put into knockout drum completely, carrying out precipitation treatment is evaporated respectively to extractor and knockout drum, most
The extract containing liposoluble constituent Yu water soluble ingredient simultaneously is obtained eventually.What is removed from extractor and knockout drum is subcritical molten
Agent, compresses and liquefies by diaphragm type compressor, and the solvent of liquid flows back to solvent holding vessel, recycles.Locust tree extract and ethanol
Mixed system, is centrifuged by multifunctional membrane experimental system 7000rmp, the visible solidity impurity of removal naked eyes, by 0.1 μm of microfiltration membranes
Clarification filtration, then by the milipore filter removal of impurities is filtered of 10000Da, eventually passes the NF membrane concentration removing extract of 150Da
In ethanol.After removing ethanol, locust tree extract is isolated and purified, the locust tree concentrate for obtaining is inhaled through D-101 types macropore
After attached resin adsorption, the locust tree flavones on adsorption resin column is desorbed using 70% ethanol；Then NK-11 type macroporous absorption trees are used again
After fat absorption, the locust tree polyphenol on adsorption resin column is desorbed with 80% ethanol.Through Folin-Phenol colorimetric method, high performance liquid chromatography
Detection, the recovery rate of water soluble ingredient locust tree polyphenol is 0.19%, and the recovery rate of liposoluble constituent locust tree flavones is 1.29%, high
In the 1.06% recovery rate (research of total flavone extracting process in Yang Zhaoyan, Sun Yuanlin, Chen Jing leaf of locust of soxhlet extraction
[J], experimental study, 2009 (8):61-64), extract Subcritical dissolvent residual is below 1ppm.
Embodiment 2
The dry mulberry leaf of 200g (water content ﹤ 13%) are taken, is crushed and after 80 mesh sieve excessively, is placed in closed extractor, plus
Enter volume fraction for 70% ethanol 400mL, after closing feeding-passage, be evacuated to vacuum, to diformazan ether solvents are injected in extractor, will
Material is totally submerged, and the mass volume ratio (w/v/v) of material, subcritical dimethyl ether and ethanol solution addition is 1:13:2.
45 DEG C of temperature (pressure is the corresponding saturated vapor pressure of the temperature), stir speed (S.S.) is to extract 30min under conditions of 600rpm；Extraction
After end, mixed solvent is put into knockout drum, carrying out precipitation treatment is evaporated respectively to extractor and knockout drum, again to extraction
Injected slurry volume fraction is 70% ethanol 400mL in tank, is vacuumized, and injection diformazan ether solvents are extracted.In triplicate, it is final to obtain
Extract containing liposoluble constituent Yu water soluble ingredient simultaneously, remaining step is ibid.
D-101 types macroporous absorbent resin adsorbs flavones in mulberry leaves and mulberry leaf polysaccharide, NKA-9 types macroporous absorbent resin absorption mulberry leaf
Alkaloid.Detected through phenol-sulphuric acid colorimetry, Reinecke's salt colorimetric method and high performance liquid chromatography, water soluble ingredient mulberry leaf polysaccharide
Recovery rate be respectively 2.98%, and traditional water extraction method is only approximately equal to 2.51% (Zhao Jun, the hypoglycemic drop of haze mulberry leaf polysaccharides high
Fat effect [J] Tianjin traditional Chinese medicine, 2004,21 (6):505–506.)；The recovery rate of water soluble ingredient Folium Mori alkaloid is
0.95%, and traditional water extraction method is only approximately equal to 0.50% (Deng Weijie, Sun Zhiping, Luo Xingen, Wu Xin honor Orthogonal Experiment and Designs
Optimization mulberry leaf total alkaloid extraction process [J] China traditional Chinese medicine academic periodical, 2012,30 (3):608-609), alcohol extracting is followed the example of and is approximately equal to
0.40% (it is excellent that Liu Fan, Huang Yong, Liao Sentai, Xiao Gengsheng, Zou Yuxiao, Shi Ying, Mu Lixia, Liu Jun, Shen Wei control application response phase methods
Change mulberry leaf polysaccharide, flavones and alkaloid combined extraction technology condition [J] silkworm industry science, 2013,39 (3):0568–0575)；Fat
Soluble components flavones in mulberry leaves recovery rate is 1.69%, and traditional water extraction method be only about 1.14% (Zhang Liangliang, Wang Yongmei, Xu Man,
Precious traditional Chinese medical science traditional Chinese medicines, 2013,24 when Wu Dongmei, Chen Jia letter different cultivars mulberry leaf polyphenol and flavones content Changing Pattern research [J]
(5):1064-1066) about 0.72% (Yang Hu, Ma Xie, Chen Hong, poplar Guo, Cai Wenqiu, Huang in yellow middle forest mulberry leaf is followed the example of in, alcohol extracting
Study on extraction [J] application chemical industry of ketone compounds, 2008,37 (5):520-522), extract Subcritical solvent is residual
Stay and be below 1ppm.
Embodiment 3
Dry Bark of Eucommia Ulmoides (water content ﹤ 13%) 1000kg is taken, 100 mesh sieve is crossed after crushing, be placed in closed extractor,
The ethanol solution for adding volume fraction to be 70%, vacuumizes, and is totally submerged material to butane solvent is injected in tank, material, Asia
The mass volume ratio (w/v/v) of critical butane and ethanol solution addition is 1:5:5, extraction conditions is：Time 30min, temperature
30 DEG C (pressure at this temperature corresponding saturated vapor pressure), stir speed (S.S.) is 500rpm.After extraction terminates, mixed solvent is put
In entering knockout drum, be evaporated carrying out precipitation treatment respectively to extractor and knockout drum, precipitation complete to obtain final product simultaneously containing it is fat-soluble into
Divide the Cortex Eucommiae extract with water soluble ingredient, remaining step is ibid.Wherein, the inorganic ceramic membrane (pellumina) of 200nm, has
Effect retention liposoluble constituent (betulic acid, cupreol, ursolic acid etc.)；The type such as D-101, S-8, AB-8 and LD-605 macropore is inhaled
Aqueous soluble active constituent (alkaloid, chlorogenic acid, glycoside, phenol etc.) in attached resin adsorption Bark of Eucommia Ulmoides.Through high performance liquid chromatography, purple
The detection of the method such as outer visible spectrophotometry and aluminum nitrate-natrium nitrosum colorimetric method, gained water soluble ingredient with it is fat-soluble into
Divide recovery rate respectively up to 95% and 98%, and subcritical dissolvent residual is below 1ppm.
Listed above is only to realize several specific embodiments of the invention.It is clear that the invention is not restricted to above example,
There can also be many deformations.The institute that one of ordinary skill in the art can directly derive from present disclosure or associate
There is deformation, be considered as protection scope of the present invention.
Claims (9)
1. a kind of method of ethanol and subcritical fluids hybrid extraction active ingredient of natural product, its feature comprises the following steps：
1）Extraction：To be put into closed extractor by the material of pretreatment, vacuumized, to the injection certain body of certain proportion in tank
The ethanol solution of fraction and appropriate subcritical fluids, to material is totally submerged, were being extracted as hybrid extraction solvent
Aid in stirring to improve efficiency in journey, according to the different qualities of material, repeatedly extracted under certain extraction conditions；
2）Precipitation：After extraction terminates, slowly liquid flux is put into knockout drum completely, extractor and knockout drum are steamed respectively
Hair carrying out precipitation treatment, precipitation completes to obtain the mixed extract comprising liposoluble constituent Yu water soluble ingredient simultaneously；From extractor
Subcritical solvent gas with being evaporated in knockout drum, compress and liquefy by diaphragm type compressor, solvent holding vessel are flowed back to, after precipitation
Subcritical solvent reusable edible；
3）UF membrane：Mixed solvent extract, is centrifuged by 1000 ~ 8000 rpm, pretreatment removal part solidity impurity, afterwards
Retained by microfiltration membranes and remove insoluble solid particle, thalline and a small amount of macromolecular substances in extract solution；Retained with milipore filter again
5000 ~ 20000 Da protein of removal, tannin and colloidal substance impurity, finally cross reverse osmosis membrane ultrafiltration concentration liquid, few to remove
Amount small-molecule substance, the temperature of UF membrane operation whole process maintains 20 ~ 40 DEG C；
4）Resin is separated：Membrane separating and purifying liquid is by after the absorption of different types of macroporous absorbent resin, selecting desired volume fraction
Ethanol solution eluted, final separation obtains the liposoluble substance and water-soluble substances of high-purity.
2. method according to claim 1, it is characterised in that the step 1) in material can be fresh or through drying
The natural plants for the treatment of, microorganism or animal, and traditional method for extracting separate halfway or impurity content extract high.
3. method according to claim 1, it is characterised in that the step 1）The volume fraction of middle ethanol solution be 50% ~
95%。
4. method according to claim 1, it is characterised in that the step 1）Subcritical solvent is volatile, is easy to solid
The mixing of one or more in the organic solvent that liquid is completely separated, including propane, butane, dimethyl ether, HFC-134a.
5. method according to claim 1, it is characterised in that the step 1）Middle extraction conditions is：Extraction time be 10 ~
120 min, temperature is 0 ~ 50 DEG C, and stir speed (S.S.) is 50 ~ 1000 rpm, and pressure mixes molten for corresponding under corresponding extraction temperature
The saturated vapour pressure of agent, extracts 1 ~ 4 time.
6. method according to claim 1, it is characterised in that the step 3）In film used be the μ of micro-filtration MF 0.05 ~ 10
In m, the nm of ultrafiltration UF 1 ~ 100, the nm of nanofiltration NF 1 ~ 10 and reverse osmosis (RO)≤1 nm one or more.
7. method according to claim 1, it is characterised in that the reverse osmosis membrane can be CAM or hollow
Fibre reverse osmosis film.
8. method according to claim 1, it is characterised in that the step 4）Middle macroreticular resin can be D-101 types, DA201
Type, SIP series, X-5 types, AB-8 types, GDX-104 types, LD-605 types, LD-601 types, CAD-40 types, DM-130 types, R-A types,
One or more in CHA-111 types, WLD types, H-107 types, NKA-9 types.
9. method according to claim 1, it is characterised in that the step 4）Middle macroporous absorbent resin eluting solvent ethanol
The volume fraction range of solution is 25% ~ 95%.
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| CN105349253B (en) * | 2015-11-16 | 2019-12-10 | 山东万路达园林科技有限公司 | Method for extracting Cornus walteri seed oil by combining ultrahigh pressure with subcritical double solvent |
| CN106916172A (en) * | 2017-02-10 | 2017-07-04 | 梅跃进 | A kind of method of subcritical abstraction nimbin |
| CN106974250B (en) * | 2017-03-23 | 2021-06-01 | 华南协同创新研究院 | Pricklyash peel flavor substance and extraction method thereof |
| CN107299002A (en) * | 2017-08-09 | 2017-10-27 | 中国热带农业科学院农产品加工研究所 | The extracting method of agilawood essential oil |
| CN108147964A (en) * | 2017-12-23 | 2018-06-12 | 安徽名创新材料科技有限公司 | A kind of method with Integrated Membrane Technology separating chlorogenic acid |
| CN110813205A (en) * | 2019-08-01 | 2020-02-21 | 铜仁学院 | Mode for removing pesticide residues in natural product extract |
| CN114618303A (en) * | 2022-03-30 | 2022-06-14 | 别敏口腔护理用品(扬州)股份有限公司 | Method for separating and purifying effective components in natural product |
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