CN1443592A - Multiple solvent extraction method - Google Patents
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Abstract
The multi-solvent extraction method for extracting and separating several components includes the following steps: 1). multi-solvent extraction; adding extraction solvent formed from at least two solvents into raw material and making extraction in homogeneous phase of extraction solvent to obtain extract solution.; 2). separation: adding phase-separating liquor formed from at least one solvent mixture in the extract solution to make phase separation, forming conjugate phase and separating the extract solution into at least two phases of target phase and non-target phase, and taking out every phase; 3). or making the target phase undergo the process of at least once circulation according to the above-mentioned extraction and separation steps; 4). recovering solvent; recovering solvent or removing water content so as to obtain the target material.
Description
Technical field
The present invention relates to the extraction separating method of organic matter, inorganic matter, particularly the method for the multi-solvent extract and separate various active composition of vegetable active composition.
Background technology
At present, conventional macroporous absorbent resin method, solvent extraction, the CO of adopting of the active ingredient in the domestic industry extract and separate natural plants
2Supercritical extraction technique, membrane filtration, other post layer suctions etc.Wherein, mostly contain unconverted monomer, crosslinking agent, pore-foaming agent, dispersant and anticorrisive agent etc. in the macroporous absorbent resin method material therefor macroreticular resin.Owing to these organic matters may be brought product in process of production into and influence health, therefore, national health department closes down the health food of producing with the macroporous absorbent resin method.Supercritical extract, membrane filtration, methods such as other post layer suctions also only are used for breadboard little making, form the industrial production of scale, because the equipment manufacturing cost height; investment is big, and output is little, the production cost of products height; profit is extremely low, and a little less than the market competitiveness, the investee is not good.
The theory of existing solvent extraction is to learn principle according to chemical industry mass transfer and separation engineering, represents the extraction process of object with the triangle phase equilibrium diagram.As shown in drawings, in triangle ABS, A represents object, and B, S represent two kinds of solvents respectively, Ri Ei line (i=0,1,2 ... state when the region representation extractant that n) is enclosed reaches balance is called the conjugation phase; The state that another region representation extractant mixes is called homogeneous phase.In the process that object is extracted, the solvent composition extractant that mixes hardly with water of selecting a kind of intensive polar solvent water and a kind of low pole for use is finished extraction to object in mutually in the conjugation of extractant.The key of this extraction theory is in the extraction process to object, 1) extractant can only be by two kinds of solvent compositions, and wherein have one must be water mutually, and another is a kind of organic solvent that mixes hardly with water of low pole mutually; 2) to the extraction of object, separate all extractant grip mutually altogether in finish; 3) in same operation, can only extract with an object in a kind of raw material; 4) process of solvent extraction is that organic solvent with a kind of low pole places extraction column, and the plant primary extract is pumped in the extraction column repeatedly, allows it by extraction column object be extracted, thus the purpose that reaches extraction, separates the single target thing.
There are the following problems for solvent extraction:
1, in the extraction process, extractant is grips the phase state altogether, and object is the contact of macroscopical geometric surface with contacting of extractant all the time, and therefore, the extraction area is little, causes the rate of extraction of object slow, and the extraction time is long, and it is long to take the equipment time, consumption worker consuming time;
2, can only extract at the some objects in the raw material in same operation, utilization ratio of raw materials is low, the production cost height;
3, must be the factor of water mutually owing to forming one of extractant, limited the range of choice (being the organic solvent that a kind of low pole and water mix hardly) of another phase organic solvent, therefore, the polarity of selected organic solvent can not appropriately cooperate with the polarity of object, has influenced the quality and the quantity of extraction object.
Summary of the invention
In view of above-mentioned, the object of the present invention is to provide a kind of solve extractant in the existing solvent extraction can not reach best fit with extraction object polarity and be applicable to industrial-scale production, the method for various active composition in production cost is low, raw material availability is high, good product quality, recovery rate the are high multi-solvent extract and separate natural plants.
The present invention adopts at least two kinds of solvent to form extractants and by at least a solvent composition phase-splitting liquid, the active component in extraction and the separating natural plant.
Multi-solvent extracting process of the present invention has the following step that carries out successively:
1) multi-solvent extraction: in raw material, add the extractant of forming by at least two kinds of solvent, extraction process carries out in the homogeneous phase of extractant, the weight of extractant is 5～10 times of raw material weight, the weight of each solvent is 1～(100-N) % of extractant gross weight, N is a solvent kind number, N=2～6 can be N=2～3, obtain extraction solution through extraction;
2) separate: in extraction solution, add the phase-splitting liquid that at least a solvent is formed, phase process carries out in extraction solution, form the conjugation phase, the weight of phase-splitting liquid is 0.25～0.5 times of extraction solution, and the weight of each solvent is 1～(100-M) % of phase-splitting liquid gross weight, M is a solvent kind number, M=1～6 can be M=1～3, through leaving standstill, extraction solution is separated into object phase that contains object or the two-phase at least that the non-object phase that does not contain object is arranged, takes out each phase;
3) or to object at least once circulate mutually, above-mentioned steps 1 is carried out in each circulation successively) multi-solvent extraction, 2) separate;
4) reclaim solvent: each phase that will take out, heating is respectively reclaimed solvent or is sloughed moisture, obtains object.
Above-mentioned raw material is can be organic matter, also can be inorganic matter, can be the plant material primary extract of plant material preparation.
Above-mentioned plant material can be the plant that contains at least a active components of plants in chromone and derivative class, organic acid, phenols and tannin, lipid, quinones, saponin class, terpene, alkaloids, sugar and derivative thereof, lactones, coumarin and isocoumarin class, lignanoids, cardiac stimulant glucoside, C12 steroid glucoside, volatile ingredient, the bitter principle.
The plant material that contains above-mentioned vegetable active composition lists as follows:
1, chromone and derivative class: water Chinese honey locust, the root of kudzu vine, legume dyewood (broom top), root of subprostrate sophora, Chinese scholartree fruit, yellow plumage hyacinth dolichos root, flower, Koryo Chinese scholartree heartwood, naple yellow flowers and trees stem, elegant jessamine, rose family Prunus timber, the plumule part of legume chick-pea chitting piece, red clover herb, underground clover seedling is twined yellow wingceltis, single leaf red bean heart wood, Ba Po ladder beans, rosaceous hair Chinese holly fruit, Myristicaceae bole, soya seeds, Chinese scholartree fruit, short Jing Dou etc.;
2, organic acid, phenols and tannin: rhodiola root, tealeaves, honeysuckle, sunflower seeds etc.;
3, lipid: soybean, yeast, the fleece-flower root, almond, rice plumule, rice bran etc.;
4, quinones: hypericum perforatum, Asian puccoon etc.;
5, saponin class: genseng, soybean, pseudo-ginseng, gynostemma pentaphylla etc.;
6, terpene: tomato, algae, watermelon etc.;
7, alkaloids: camptotheca seed, golden cypress bark etc.;
8, sugar and derivative thereof: soybean, Poria cocos, glossy ganoderma, apple etc.;
9, lactones: clover, Russian red clover section plant etc.;
10, lignanoids: schisandra chinensis, fructus schisandrae etc.;
11, cardiac stimulant glucoside: convallaria etc.;
12, C12 steroid glucoside: Semen Carthami etc.;
13, volatile ingredient: fruit, rose etc.;
14, bitter principle: ginkgo leaf;
15, coumarin and isocoumarin class etc.
Above-mentioned multi-solvent extraction step is carried out under normal temperature, condition of normal pressure, and stirs extraction 15～120 minutes, and the elapsed-time standards that leaves standstill of above-mentioned separating step is 10～30 minutes, and the heating-up temperature of above-mentioned recovery solvent step is 50～120 degree Celsius.
The preparation of above-mentioned plant primary extract can be carried out the following step successively:
1) clean: at least a cleaning plant material in water or the organic solvent, remove impurity;
2) extract: add a kind of extraction solvent, the weight of extracting solvent is 5～10 times of plant material weight, extracts under normal temperature or 30 degree～120 degree Celsius, normal pressure or pressurization 0.5MPa, extracts once in per 2 hours, extracts at least three times, obtains plant extraction liquid;
3) reclaim solvent: being heated to temperature is 50～120 degree Celsius, reclaims the extraction solvent in the extract or sloughs moisture, makes the plant primary extract.
Can carry out column extracting before the above-mentioned multi-solvent extraction step.
Above-mentioned extraction solvent can be C
1～C
10Organic solvent, water, aqueous slkali, acid solution.
Above-mentioned extractant can be C
1～C
10Organic solvent, water, aqueous slkali, acid solution.
Above-mentioned phase-splitting liquid can be C
1～C
10Organic solvent, water, aqueous slkali, acid solution.
Above-mentioned C
1～C
10Organic solvent can be ethane; Methylpentane; Dimethylbutane; Heptane; Octane; Trimethylpentane; Nonane; Trimethyl ethane; Benzinum; Gasoline; Pentamethylene; Methyl cyclopentane; Cyclohexane; Hexahydrotoluene; Ethyl cyclohexane; Cyclohexene; Firpene; Limonene; Benzene; Styrene; Toluene; Ortho-xylene; Meta-xylene; Paraxylene; Dimethylbenzene; Ethylbenzene; Diethylbenzene; Butylbenzene; Carrene; Chloroform; Carbon tetrachloride; Dichloroethanes; Trichloroethanes; Dichloroethylene; Trichloro-ethylene; Tetrachloro-ethylene; Chloropropane; Dichloropropane; Chlorobutane; Dichloroetane; Dichloro-dimethyl propane; Bromofom; Bromoethane; Bromofume; N-Propyl Bromide; Dibromopropane; Chlorobenzene; O-dichlorohenzene; M-dichlorobenzene; Paracide; Ortho-chlorotolu'ene; Parachlorotoluene; Bromobenzene; Fluorobenzene; Benzotrifluoride; Methylene bromide; Dibromopropane; Methyl alcohol; Ethanol; Propyl alcohol; Isopropyl alcohol; N-butanol; Isobutanol; Sec-butyl alcohol; The tert-butyl alcohol; Amylalcohol; Isoamyl alcohol; Phenol; Cresols; Ether; Propyl ether; Isopropyl ether; Butyl ether; The second amyl ether; Methyl phenyl ethers anisole; Furans; Methylfuran; Oxolane; Oxinane; Dimethoxym ethane; Acetal; Butyraldehyde; Acetone; Butanone; Pentanone; Hexanone; Methylpentanone; Heptanone; Cyclohexanone; Methyl cyclohexanone; Espeleton; Formic acid; Acetic acid; Propionic acid; Butyric acid; Valeric acid; Acetic anhydride; Propionic andydride; Methyl formate; Ethyl formate; Propyl formate; Butyl formate; Amyl formate; Methyl acetate; Ethyl acetate; Butyl acetate; Pentyl acetate; Methyl propionate; Ethyl propionate.
Above-mentioned aqueous slkali can be sodium hydroxide solution, hydroxide first solution, aqua calcis, sodium bicarbonate solution, ammoniacal liquor.
Above-mentioned acid solution can be hydrochloric acid solution, sulfuric acid solution, carbon acid solution.
The weight of each solvent in the above-mentioned extractant can be 10～(90-N) % of extractant gross weight.
The weight of each solvent in the above-mentioned extractant can be 20～(80-N) % of extractant gross weight.
The weight of each solvent in the above-mentioned extractant can be 30～(70-N) % of extractant gross weight.
The weight of each solvent in the above-mentioned phase-splitting liquid can be 10～(90-M) % of phase-splitting liquid gross weight.
The weight of each solvent in the above-mentioned phase-splitting liquid can be 20～(80-M) % of phase-splitting liquid gross weight.
The weight of each solvent in the above-mentioned phase-splitting liquid can be 30～(70-M) % of phase-splitting liquid gross weight.
The inventive method is based on following theory:
One, the inventive method based on extractant, be at the intrinsic polarity of object, select multiple solvent composition extractant for use, determine the ratio of each solvent with the method for experiment, the preparation extractant.As organic solvent, water, aqueous slkali, the acid solution of extractant, each solvent can be that polarity is identical or polarity is different when selecting for use.
Two, the present invention carries out in the homogeneous phase of extractant the extraction process of object, is contacting of microcosmic molecular level between object and extractant, and the extraction area is very big, has shortened the time of extraction object greatly, has improved the recovery rate of object.
Three, the present invention adopts phase-splitting liquid that extraction solution is carried out phase-splitting to the separation of object.Promptly in extraction solution, add phase-splitting liquid, make extraction solution enter and grip the phase state altogether from original homogeneous state, thus the separate targets thing.
" the multi-solvent extracting system " that the inventive method adopts realized cycling extraction, separation, the solvent recovery to object, obtains the active ingredient in the plant.This system connects extractor and the pump and the control valve of one or more common structures according to the step of the inventive method with pipeline, and presses cycle-index formation circulatory system structure.
The present invention has following obvious advantage and remarkable result compared with prior art.
One, the comparison of extraction theory
Extraction is chosen in the homogeneous phase of extractant and carries out to the multi-solvent of object in the present invention, carries out in gripping mutually altogether to being separated in of object; Extractant is that two or more organic solvent, water, aqueous slkali, acid solution formed, and these solvents can be that polarity is close or polarity is different, and the polarity intrinsic according to object is by different ratio row preparation extractants.And existing solvent extraction technology to the extraction of object be chosen in extractant grip mutually altogether in carry out, in gripping mutually altogether, separate; Extractant is that the organic solvent that mixes hardly with water of water and low pole is formed.Therefore, the present invention can be in same operation, and to carrying out extract and separate with a plurality of active ingredients in a kind of raw material, and existing solvent extraction technology can only separate an active ingredient.
Two, realize in " the multi-solvent extracting system " that method of the present invention constitutes with common equipment.And the equipment that existing solvent extraction technology is selected for use is extraction column.Because " multi-solvent extracting system " adopts common device, conventional equipment, even can be that used equipment constitutes, equipment manufacturing cost is low, extraction process, separation process, removal process simple to operate, extraction efficiency height.
Three, the multiple solvent selected for use of the present invention, the close or polarity of its polarity different all can, the selection face width of extractant, existing solvent extraction technology only can adopt water and the organic solvent a kind of and low pole that water mixes hardly.
In sum, the inventive method has and can extract in same operation with the multiple components in a kind of raw material; Can be used for industrial-scale production, production cost is low, raw material availability height, good product quality, purity height, yield advantages of higher.
The present invention is applicable to chromone in extract and separate organic matter, the inorganic matter, particularly natural plants and derivative class, organic acid, phenols and tannin, lipid, quinones, saponin class, terpene, alkaloids, sugar and derivative thereof, lactones, coumarin and isocoumarin class, lignanoids, cardiac stimulant glucoside, C12 steroid glucoside, volatile ingredient, bitter principle isoreactivity composition.
Below, with embodiment the present invention is further described again.
Description of drawings
Accompanying drawing is the triangle phase equilibrium diagram of a kind of multi-solvent extracting process of the present invention.
The specific embodiment
Embodiment 1
A kind of multi-solvent extracting process of the present invention, extraction object lycopene from the dewatered tomato dregs.Extraction process of the present invention carries out at the multi-solvent extracting system, and multi-solvent extracting system of the present invention connects formations such as the pump of the extractor of one or more common structures and configuration thereof and control valve with common pipeline.Present embodiment carries out successively according to table 1 and the following step:
One, prepares the plant primary extract with plant material
1, clean: get the plant material tomato according to table 1, water cleans, and plant primary extract dewatered tomato dregs are made in dehydration;
2, extract: in the dewatered tomato dregs, add 5 times to the extraction solvent methanol of dewatered tomato dregs weight, in temperature is 50 degree Celsius, and pressure is normal pressure, after extracting in 1 hour, with the Impurity removal in the dewatered tomato dregs, filtering the tomato dregs that obtain is the lycopene primary extract;
3, reclaim solvent: it is 65 degree Celsius that extract is heated to temperature, reclaims the methyl alcohol in the extract.
Two, multi-solvent extraction
Choose benzinum, carrene mixing composition extractant, join in the lycopene primary extract, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 1, and in the homogeneous phase of extractant, it is the tomato extraction solution that extraction obtains plant extraction solution.
Three, separate
Choose methyl alcohol, acetone, water combined group and become phase-splitting liquid, join in the tomato extraction solution, the conjugation of extractant mutually in, according to the phase-splitting condition of table 1, leave standstill be separated into after the phase-splitting be dissolved with lycopene object mutually and the non-object that contains dregs mutually.
Four, reclaim solvent
1, is 65 degree Celsius with non-object heat phase to temperature, collects and reclaim organic solvent: methyl alcohol, acetone, deslagging then;
2, be 90 degree Celsius with object heat phase to temperature, collect and reclaim residual organic solvent: benzinum, carrene obtain object: content is 3%～6% lycopene.
Five, be that 3%～6% lycopene repeats two, three stepping single step purifications with the content that obtains, obtain content and be 6%～30% lycopene.
Embodiment 2
A kind of multi-solvent extracting process of the present invention, extraction object isoflavones, soyasaponins, soyabean oligosaccharides, soybean lecithin from dregs of beans.Extraction process of the present invention carries out at the multi-solvent extracting system, and multi-solvent extracting system of the present invention connects formations such as the pump of the extractor of one or more common structures and configuration thereof and control valve with common pipeline.Present embodiment carries out successively according to table 2-1, table 2-2 and the following step:
One, cleans raw material, preparation soybean primary extract
1, take by weighing soybean meal 1000 grams that contain isoflavones 0.3～0.4%, screening places extractor after removing silt, impurity;
2, adding content is extraction solution methyl alcohol 95% or more, and weight is 8 times of soybean meal weight, is Celsius 65 to spend, extract under the condition that pressure is normal pressure in temperature, and every liquid extraction time is 2 hours, extracts three liquid altogether, obtains soybean extract;
3, extract being heated to temperature in inspissator is 65 degree Celsius, behind the collection recovery methyl alcohol wherein, makes the soybean primary extract.
Two, column extracting: column extracting, separation soyabean oligosaccharides from the soybean primary extract
1, make extractant with ethyl acetate, take column extracting mode extracting soybean primary extract, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 2-1, obtains ethyl acetate liquid phase and soyabean oligosaccharides mutually;
2, take out the soyabean oligosaccharides phase, advance baking oven and be heated to the dry moisture of 100, obtain object: soyabean oligosaccharides;
3, take out the ethyl acetate liquid phase, being heated to temperature in inspissator is that 75 degree Celsius reclaim ethyl acetate, has been taken out the soybean primary extract of soyabean oligosaccharides;
Three, multi-solvent extraction:
Adopt the multi-solvent extracting system, select for use methyl alcohol, benzinum to mix and form extractant, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 2-1, adds in the soybean primary extract that has taken out soyabean oligosaccharides to extract, and obtains the soybean extraction solution;
Four, separate
According to table 2-1, water is added in the soybean extraction solution as phase-splitting liquid, mixing, leave standstill, extraction solution is divided into three object phases, separate this three-phase, the benzinum that must contain soyasaponins and soybean lecithin mutually, the crystallization methyl alcohol that contains 40%～60% isoflavones mutually with the methyl alcohol that contains 5%～20% isoflavones mutually.
Five, multi-solvent extraction:
Adopt the multi-solvent extracting system, methyl alcohol, acetone preparation extractant, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 2-2, adds the middle mutually extraction of above-mentioned benzinum, obtains containing the soybean extraction solution of soyasaponins and soybean lecithin.
Six, separate
According to table 2-1, adding contains in the soybean extraction solution of soyasaponins and soybean lecithin as phase-splitting liquid with water, and mixing leaves standstill, and the extraction solution phase-splitting also is separated into acetone, the methyl alcohol phase that contains soyasaponins, contains the benzinum phase of soybean lecithin.
Seven, reclaim solvent
1, with the methyl alcohol phase, being heated to temperature in inspissator is 65 degree Celsius, and behind the recovery methyl alcohol, advance oven drying and obtain object: content is 5%～20% isoflavones.
2, with crystallization methyl alcohol after plate-frame filtering reclaims methyl alcohol, advance oven for drying and obtain object: content is 40%～60% isoflavones.
3, acetone, methyl alcohol being heated to temperature in inspissator is after 65 degree Celsius reclaim acetone, methyl alcohol, to advance oven for drying and obtain object: soyasaponins.
4, benzinum being heated to temperature in inspissator is 90 degree Celsius, behind the recovery benzinum, advances oven drying and obtains object: soybean lecithin.
Present embodiment extracts content from soybean meal be 5%～50% isoflavones, and obtain byproduct soyabean oligosaccharides, soyasaponins, soybean lecithin.With content be 50% isoflavones by extraction, separate and be further purified, can obtain content and be 60% isoflavones.
Embodiment 3
A kind of multi-solvent extracting process of the present invention extracts camptothecine from camptotheca seed.Extraction process of the present invention carries out at the multi-solvent extracting system, and the present invention adopts multi-solvent extracting system similar to Example 1.Present embodiment carries out successively according to table 3 and the following step:
One, cleans raw material, preparation camplotheca acuminata primary extract
1, according to table 3, take by weighing the plant material camptotheca seed, water places extractor after cleaning and removing silt;
2, adding content is the extraction solution methyl alcohol more than 98%, and the dosage of extracting solvent is that the multiple and the extraction conditions of plant material sees Table 3, extracts repeatedly three times, each 2 hours, obtains the camplotheca acuminata extract;
3, extract being put into inspissator, to be heated to temperature be 65 degree Celsius, collect to reclaim methyl alcohol after, make the camplotheca acuminata primary extract.
Two, multi-solvent extraction
Adopt chloroform, benzinum: 1% methanolic sodium hydroxide alkali lye, the preparation extractant adds in the camplotheca acuminata primary extract, and the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 3, and extraction obtains the camplotheca acuminata extraction solution.
Three, separate
According to table 3, with 2% sodium hydrate aqueous solution, methyl alcohol preparation phase-splitting liquid, add in the camplotheca acuminata extraction solution, mixing leaves standstill, and is separated into non-object phase after the extraction solution phase-splitting: methyl alcohol, alkali lye phase, object phase: mixed solution phase.
Four, mixed solution is repeated mutually two, three steps, mixed solution is done 5 circulations mutually, after further removing impurity, being heated to temperature is 90 degree Celsius, reclaim organic solvent chloroform, the benzinum of mixed solution in mutually, collect crystal, and crystal is carried out vacuum drying, remove residual solvent, obtain object: camptothecine.
Five, reclaim solvent
Methyl alcohol, alkali lye are heated to temperature in inspissator be 65 degree Celsius, deslagging behind the collection recovery methyl alcohol.NaOH is with the slag venting.
Present embodiment can extract content from camptotheca seed be 70%～98% camptothecine.
Embodiment 4
A kind of multi-solvent extracting process of the present invention extracts hypericin from the plant hypericum perforatum.Extraction process of the present invention carries out at the multi-solvent extracting system, and the present invention adopts multi-solvent extracting system similar to Example 1.Embodiment carries out successively according to table 4 and the following step:
One, cleans raw material, preparation hypericum perforatum primary extract
1, according to table 4, take by weighing the plant material hypericum perforatum, water places extractor after cleaning and removing silt;
2, according to table 4, adding content is the extraction solvent methanol more than 95%, and the dosage of extracting solvent is that the multiple of hypericum perforatum sees Table 4, extracts by extraction conditions, three times repeatedly, each 2 hours, obtains the hypericum perforatum extract;
3, the hypericum perforatum extract being put into inspissator, to be heated to temperature be that 65 degree Celsius reclaim methyl alcohol, makes the hypericum perforatum primary extract;
Two, multi-solvent extraction
Select chloroform, benzinum, pyridine, acetone, methyl alcohol for use: benzene preparation extractant, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 4, joins in the hypericum perforatum primary extract, extraction obtains the hypericum perforatum extraction solution;
Three, separate
According to table 4, water adds phase-splitting liquid as phase-splitting liquid in the hypericum perforatum extraction solution, and mixing leaves standstill, and separates after the extraction solution phase-splitting, obtains non-object phase: chloroform, benzinum, benzene phase, object phase: the mixing phase that contains hypericin.
Four, reclaim solvent
1, be after 90 degree Celsius reclaim organic solvent chloroform, benzinum, benzene with chloroform, benzinum, benzene heat phase to temperature, deslagging.
2, will take out mix heat phase to temperature be Celsius 65 reclaim organic solvent-acetones, methyl alcohol after, temperature is advanced oven drying and is obtained hypericin.
Present embodiment extracts content from the plant hypericum perforatum be 0.15%～5% hypericin.
Embodiment 5
A kind of multi-solvent extracting process of the present invention extracts TSPG from the plant genseng.Extraction process of the present invention carries out at the multi-solvent extracting system, and the present invention adopts multi-solvent extracting system similar to Example 1.Present embodiment carries out successively according to table 5 and the following step:
One, cleans raw material, preparation genseng primary extract
1, according to table 5, take by weighing the raw material genseng, water places extractor after cleaning and removing silt;
2, adding content is the extraction solvent methanol more than 95%, and the dosage of extracting solvent is that the multiple of genseng sees Table 5, extracts by extraction conditions, three times repeatedly, each 2 hours, obtains Ginseng extract;
3, extract being put into inspissator, to be heated to temperature be that 65 degree Celsius reclaim methyl alcohol, makes the genseng primary extract;
Two, column extracting
1, use ethyl acetate as the column extracting solvent, add the genseng primary extract and carry out column extracting, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 5, and extraction obtains the ethyl acetate phase and contains the water of polysaccharose substance;
2, take out water, obtain the polysaccharose substance in the genseng primary extract;
3, take out the ethyl acetate phase, being heated to temperature in inspissator is that 75 degree Celsius reclaim ethyl acetate, has been removed the genseng primary extract of polysaccharose substance;
Three, multi-solvent extraction
With chloroform, benzinum, acetone preparation extractant, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 5, adds the extraction of genseng primary extract and obtains the genseng extraction solution;
Four, separate
According to table 5, water, methyl alcohol preparation phase-splitting liquid add in the genseng extraction solution, and mixing leaves standstill, and is separated into the target phase after the extraction solution phase-splitting: chloroform, benzinum phase, methyl alcohol, acetone, water;
Five, reclaim solvent
1, with methyl alcohol, acetone, water, being heated to temperature in inspissator is that 65 degree Celsius reclaim methyl alcohol, advances oven drying and obtains TSPG;
2, with chloroform, benzinum phase, being heated to temperature in inspissator is that 90 degree Celsius reclaim chloroform, benzinum, obtains fats, carotene class, Sitosterolum class material.
Present embodiment extracts content 10～60% TSPGs from the plant genseng, and obtains accessory substance fats, carotene class, Sitosterolum class material.
Embodiment 6
A kind of multi-solvent extracting process of the present invention extracts chlorogenic acid from the plant honeysuckle.Extraction process of the present invention carries out at the multi-solvent extracting system, and the present invention adopts multi-solvent extracting system similar to Example 1.Present embodiment carries out successively according to table 6 and the following step:
One, cleans raw material, preparation honeysuckle primary extract
1, according to table 6, take by weighing plant material honeysuckle 1000 grams, water places extractor after cleaning and removing silt;
2, adding content is the extraction solvent methanol more than 95%, and the dosage of extracting solvent is multiple and the extraction conditions 6 of honeysuckle, extracts repeatedly three times, each 2 hours, obtains Flos Lonicerae extractive solution;
3, Flos Lonicerae extractive solution being put into inspissator, to be heated to temperature be that 65 degree Celsius reclaim methyl alcohol, makes the honeysuckle primary extract.
Two, column extracting
1, use acetone as the column extracting solvent, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 6, and the honeysuckle primary extract is carried out column extracting, obtains acetone phase and water (glucide);
2, take out water, remove the glucide in the honeysuckle primary extract;
3, take out the acetone phase, in inspissator, be heated to temperature 56 degree Celsius and reclaim acetone, obtain the honeysuckle primary extract of desaccharification class material.
Three, multi-solvent extraction
With chloroform, benzinum preparation extractant, add in the honeysuckle primary extract and stir, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 6, obtains the honeysuckle extraction solution.
Four, separate
According to table 6, water, methyl alcohol preparation phase-splitting liquid add in the honeysuckle extraction solution, and mixing leaves standstill, and is separated into chloroform, benzinum phase and methyl alcohol, water after the extraction solution phase-splitting;
Five, reclaim solvent
1,, in inspissator, is heated to temperature 90 degree Celsius and reclaims deslagging behind chloroforms, the benzinum with chloroform, benzinum phase;
2, with methyl alcohol, water, in inspissator, be heated to temperature 65 degree Celsius and reclaim methyl alcohol, advance oven drying and obtain chlorogenic acid.
Present embodiment extracts content from the plant honeysuckle be 10～30% chlorogenic acid.
Embodiment 7
A kind of multi-solvent extracting process of the present invention extracts the content rhodioloside from plant rhodiola root piece root.Extraction process of the present invention carries out at the multi-solvent extracting system, and the present invention adopts multi-solvent extracting system similar to Example 1.Present embodiment carries out successively according to table 7 and the following step:
One, cleans raw material, preparation rhodiola root primary extract
1, according to table 7, take by weighing raw material rhodiola root 1000 grams, clean and go silt to place extractor;
2, adding content is the extraction solvent methanol more than 95%, and the dosage of extracting solvent is that the multiple and the extraction conditions of rhodiola root sees Table 7, extracts repeatedly three times, each 2 hours, obtains rhodiola extract;
3, rhodiola extract being put into inspissator, to be heated to temperature be that 65 degree Celsius reclaim methyl alcohol, makes the rhodiola root primary extract.
Two, column extracting
1, use ethyl acetate as extractant, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 7, and the rhodiola root primary extract is carried out column extracting, obtains ethyl acetate phase and water (polysaccharose substance);
2, take out water, remove the glucide in the rhodiola root primary extract;
3, take out the ethyl acetate phase, in inspissator, be heated to temperature 75 degree Celsius and reclaim ethyl acetate, obtain the rhodiola root primary extract of desaccharification class material.
Three, multi-solvent extraction
With chloroform, benzinum preparation extractant, add the rhodiola root primary extract behind column extracting, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 7, stirs extraction, obtains extraction solution.
Four, separate
Water, methyl alcohol preparation phase-splitting liquid add in the extraction solution, and according to table 7 condition, mixing leaves standstill, and is separated into chloroform, benzinum phase and methyl alcohol, water after the extraction solution phase-splitting;
Five, reclaim solvent
1,, in inspissator, is heated to temperature 90 degree Celsius and reclaims deslagging behind chloroforms, the benzinum with chloroform, benzinum phase;
2, with methyl alcohol, water, in inspissator, be heated to temperature 65 degree Celsius and reclaim methyl alcohol, advance oven drying and obtain rhodioloside.
Present embodiment extracts content from the plant rhodiola root be 3%～30% rhodioloside.
Embodiment 8
A kind of multi-solvent extracting process of the present invention extracts Osthole from the plant frutus cnidii.Extraction process of the present invention carries out at the multi-solvent extracting system, and the present invention adopts multi-solvent extracting system similar to Example 1.Embodiment carries out successively according to table 8 and the following step:
One, cleans raw material, preparation frutus cnidii primary extract
1, according to table 8, take by weighing the plant material frutus cnidii, water places extractor after cleaning and removing silt;
2, according to table 8, adding content is the extraction etoh solvent more than 95%, and the dosage of extracting solvent is that the multiple of frutus cnidii sees Table 8, extracts by extraction conditions, three times repeatedly, each 2 hours, obtains the frutus cnidii extract;
3, the frutus cnidii extract being put into inspissator, to be heated to temperature be that 75 degree Celsius reclaim ethanol, makes the frutus cnidii primary extract;
Two, multi-solvent extraction
Select chloroform, benzinum, methyl alcohol preparation extractant for use, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 8, joins in the frutus cnidii primary extract, and extraction obtains the frutus cnidii extraction solution;
Three, separate
According to table 8, the aqueous hydrochloric acid solution with 1% adds phase-splitting liquid as phase-splitting liquid in the frutus cnidii extraction solution, and mixing leaves standstill, and separates after the extraction solution phase-splitting, obtains the object phase: chloroform, benzinum phase.Non-object phase: methyl alcohol, sour water phase.
Four, reclaim solvent
1, be after 90 degree Celsius reclaim organic solvent chloroform, benzinum, to advance oven drying and obtain Osthole chloroform, benzinum heat phase to temperature.
2, methyl alcohol, sour water adjusted the pH value mutually be 6.5 after, be heated to temperature and be Celsius 65 and reclaim organic solvent methyl alcohol, deslagging.
Embodiment 9
A kind of multi-solvent extracting process of the present invention extracts schizandrin from the plant fruit of Chinese magnoliavine.Extraction process of the present invention carries out at the multi-solvent extracting system, and the present invention adopts multi-solvent extracting system similar to Example 1.Embodiment carries out successively according to table 9 and the following step:
One, cleans raw material, preparation fruit of Chinese magnoliavine primary extract
1, according to table 9, take by weighing the plant material fruit of Chinese magnoliavine, water places extractor after cleaning and removing silt;
2, according to table 9, adding content is the extraction etoh solvent more than 95%, and the dosage of extracting solvent is that the multiple of the fruit of Chinese magnoliavine sees Table 9, extracts by extraction conditions, three times repeatedly, each 2 hours, obtains Fructus Schisandrae Chinensis extractive solution;
3, Fructus Schisandrae Chinensis extractive solution being put into inspissator, to be heated to temperature be that 75 degree Celsius reclaim ethanol, makes fruit of Chinese magnoliavine primary extract;
Two, multi-solvent extraction
Select chloroform, benzene, methyl alcohol preparation extractant for use, the dosage of extractant is that the multiple and the extraction conditions of primary extract sees Table 9, joins in the fruit of Chinese magnoliavine primary extract, and extraction obtains fruit of Chinese magnoliavine extraction solution;
Three, separate
According to table 9, as phase-splitting liquid, in the frutus cnidii extraction solution, add phase-splitting liquid with methyl alcohol, the aqueous solution, according to the condition of table 9, mixing leaves standstill, and separates after the extraction solution phase-splitting, obtains the object phase: chloroform, benzene phase.Non-object phase: methyl alcohol, water.
Four, reclaim solvent
1, be after 80 degree Celsius reclaim organic solvent chloroform, benzene, to advance oven drying and obtain schizandrin chloroform, benzene heat phase to temperature.
2, methyl alcohol, water are heated to temperature be Celsius 65 reclaim the organic solvent methyl alcohol after, deslagging.
Table 1 is from the embodiment list of dewatered tomato dregs extraction lycopene
| The embodiment sequence number | One, system plant extracts | Two, multi-solvent extraction | Three, separate | Lycopene | |||||||||||
| Dewatered tomato dregs gram | Extract solvent | Extractant and weight % ratio | The extractant total amount doubly | Extraction conditions | Phase-splitting liquid and weight % ratio | Phase-splitting liquid total amount doubly | The phase-splitting condition | Content % | The output gram | Yield % | |||||
| Temperature ℃ | Pressure MP a | The time branch | Temperature ℃ | Pressure MP a | The time branch | ||||||||||
| ?1-1 | ??1000 | Methyl alcohol | Benzinum: carrene 5: 95 | ????9 | Normal temperature | Normal pressure | 15 | Methyl alcohol: acetone: water 5: 60: 35 | ?0.25 | Normal temperature | Normal pressure | 10 | ?4.4 | ?40.9 | ?4.09 |
| ?1-2 | ??1000 | Methyl alcohol | Benzinum: carrene 95: 5 | ????9 | Normal temperature | Normal pressure | 25 | Methyl alcohol: acetone: water 60: 5: 35 | ?0.35 | Normal temperature | Normal pressure | 15 | ?3.98 | ?45.2 | ?4.52 |
| ?1-3 | ??1000 | Methyl alcohol | Benzinum: carrene 30: 70 | ????9 | Normal temperature | Normal pressure | 40 | Methyl alcohol: acetone: water 40: 30: 30 | ?0.4 | Normal temperature | Normal pressure | 18 | ?6.50 | ?27.7 | ?2.77 |
| ?1-4 | ??1000 | Methyl alcohol | Benzinum: carrene 40: 60 | ????10 | Normal temperature | Normal pressure | 70 | Methyl alcohol: acetone: water 30: 30: 40 | ?0.45 | Normal temperature | Normal pressure | 25 | ?6.51 | ?25.7 | ?2.57 |
| ?1-5 | ??1000 | Methyl alcohol | Benzinum: carrene 50: 50 | ????10 | Normal temperature | Normal pressure | 100 | Methyl alcohol: acetone: water 50: 10: 40 | ?0.5 | Normal temperature | Normal pressure | 30 | ?6.79 | ?25.8 | ?2.58 |
The embodiment guide look of table 2-1 extracting soybean isoflavone, soyasaponins, soyabean oligosaccharides, soybean lecithin from soybean meal
| The embodiment sequence number | One system plant extracts | Two, column extracting | Three, multi-solvent extraction | Four, separate | Isoflavones | |||||||||||||||
| The soybean meal gram | Extract solvent | Extractant | Extraction conditions | The extractant dosage doubly | Extractant | Extractant | The extractant total amount doubly | Phase-splitting liquid | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | The output gram | Yield % | |||||||
| Pressure MP a | Temperature ℃ | The time branch | Benzinum: methyl alcohol and weight % ratio | Pressure MP a | Temperature ℃ | The time branch | Pressure MP a | Temperature ℃ | The time branch | |||||||||||
| ??2-1 | ??1000 | Methyl alcohol | Ethyl acetate | Normal pressure | Normal temperature | ??180 | ??20 | ?40∶60 | Normal pressure | Normal temperature | ??30 | ??5 | Water | Normal pressure | Normal temperature | ??10 | ??0.25 | ??28.97 | ??7.5 | ??0.75 |
| ??2-2 | ??1000 | Methyl alcohol | Ethyl acetate | Normal pressure | Normal temperature | ??180 | ??20 | ?50∶50 | Normal pressure | Normal temperature | ??40 | ??6 | Water | Normal pressure | Normal temperature | ??10 | ??0.25 | ??35.1 | ??6.1 | ??0.61 |
| ??2-3 | ??1000 | Methyl alcohol | Ethyl acetate | Normal pressure | Normal temperature | ??180 | ??20 | ?60∶40 | Normal pressure | Normal temperature | ??30 | ??7 | Water | Normal pressure | Normal temperature | ??10 | ??0.3 | ??42.1 | ??5.3 | ??0.53 |
| ??2-4 | ??1000 | Methyl alcohol | Ethyl acetate | Normal pressure | Normal temperature | ??240 | ??15 | ?70∶30 | Normal pressure | Normal temperature | ??40 | ??8 | Water | Normal pressure | Normal temperature | ??10 | ??0.3 | ??48.6 | ??4.4 | ??0.44 |
| ??2-5 | ??1000 | Methyl alcohol | Ethyl acetate | Normal pressure | Normal temperature | ??240 | ??15 | ?80∶20 | Normal pressure | Normal temperature | ??50 | ??9 | Water | Normal pressure | Normal temperature | ??15 | ??0.3 | ??49.9 | ??4.1 | ??0.41 |
| ??2-6 | ??1000 | Methyl alcohol | Ethyl acetate | Normal pressure | Normal temperature | ??240 | ??15 | ?95∶5 | Normal pressure | Normal temperature | ??60 | ??10 | Water | Normal pressure | Normal temperature | ??15 | ??0.4 | ??47.89 | ??4.3 | ??0.43 |
| ??2-7 | ??1000 | Methyl alcohol | N-butanol | Normal pressure | Normal temperature | ??300 | ??13 | ?5∶95 | Normal pressure | Normal temperature | ??70 | ??8.5 | Water | Normal pressure | Normal temperature | ??15 | ??0.4 | ??11.2 | ??12.7 | ??1.27 |
| ??2-8 | ??1000 | Methyl alcohol | N-butanol | Normal pressure | Normal temperature | ??300 | ??13 | ?20∶80 | Normal pressure | Normal temperature | ??80 | ??6.5 | Water | Normal pressure | Normal temperature | ??20 | ??0.5 | ??15 | ??9.9 | ??0.99 |
| ??2-9 | ??1000 | Methyl alcohol | N-butanol | Normal pressure | Normal temperature | ??300 | ??13 | ?30∶70 | Normal pressure | Normal temperature | ??90 | ??7.5 | Water | Normal pressure | Normal temperature | ??20 | ??0.5 | ??21.9 | ??8 | ??0.8 |
| ??2-10 | ??1000 | Methyl alcohol | N-butanol | Normal pressure | Normal temperature | ??360 | ??10 | ?40∶60 | Normal pressure | Normal temperature | ??100 | ??8.5 | Water | Normal pressure | Normal temperature | ??25 | ??0.45 | ??26.3 | ??7 | ??0.7 |
| ??2-11 | ??1000 | Methyl alcohol | N-butanol | Normal pressure | Normal temperature | ??360 | ??10 | ?50∶50 | Normal pressure | Normal temperature | ??110 | ??8 | Water | Normal pressure | Normal temperature | ??30 | ??0.35 | ??33.2 | ??6.1 | ??0.61 |
| ??2-12 | ??1000 | Methyl alcohol | N-butanol | Normal pressure | Normal temperature | ??360 | ??10 | ?60∶40 | Normal pressure | Normal temperature | ??120 | ??9 | Water | Normal pressure | Normal temperature | ??30 | ??0.35 | ??41.1 | ??5.5 | ??0.55 |
The embodiment list of table 2-2 extracting soybean isoflavone, soyasaponins, soyabean oligosaccharides, soybean lecithin from soybean meal
| The embodiment sequence number | Extraction phase | Five, multi-solvent extraction | Six, separate | Soybean lecithin | Soyasaponins | ||||||||||||
| Extractant | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | The output gram | Yield % | Content % | The output gram | Yield % | ||||||
| Benzinum: acetone and weight % ratio | Pressure MPa | Temperature ℃ | The time branch | Pressure MPa | Temperature ℃ | The time branch | |||||||||||
| ??2-1 | The benzinum phase | ??40∶60 | Normal pressure | Normal temperature | ????30 | ????5 | Water | Normal pressure | Normal temperature | ????15 | ????0.3 | ?39.7 | ?50.4 | ?5.04 | ?39.5 | ?38 | ?3.8 |
| ??2-2 | The benzinum phase | ??50∶50 | Normal pressure | Normal temperature | ????30 | ????5 | Water | Normal pressure | Normal temperature | ????15 | ????0.3 | ?33.6 | ?59.5 | ?5.95 | ?35.4 | ?42.4 | ?4.24 |
| ??2-3 | The benzinum phase | ??60∶40 | Normal pressure | Normal temperature | ????30 | ????7 | Water | Normal pressure | Normal temperature | ????15 | ????0.3 | ?29 | ?69 | ?6.9 | ?30.9 | ?48.5 | ?4.85 |
| ??2-4 | The benzinum phase | ??70∶30 | Normal pressure | Normal temperature | ????50 | ????7 | Water | Normal pressure | Normal temperature | ????15 | ????0.3 | ?24.9 | ?80.3 | ?8.03 | ?27.6 | ?54.3 | ?5.43 |
| ??2-5 | The benzinum phase | ??80∶20 | Normal pressure | Normal temperature | ????50 | ????6 | Water | Normal pressure | Normal temperature | ????15 | ????0.3 | ?21.7 | ?92.2 | ?9.22 | ?25.4 | ?59.1 | ?5.91 |
| ??2-6 | The benzinum phase | ??90∶10 | Normal pressure | Normal temperature | ????50 | ????6 | Water | Normal pressure | Normal temperature | ????20 | ????0.4 | ?18.7 | ?107 | ?10.7 | ?22.3 | ?67.3 | ?6.73 |
| ??2-7 | The benzinum phase | ??10∶90 | Normal pressure | Normal temperature | ????80 | ????8 | Water | Normal pressure | Normal temperature | ????20 | ????0.4 | ?47.9 | ?41.8 | ?4.18 | ??42 | ?35.7 | ?3.57 |
| ??2-8 | The benzinum phase | ??20∶80 | Normal pressure | Normal temperature | ????80 | ????8 | Water | Normal pressure | Normal temperature | ????20 | ????0.4 | ?46.7 | ?42.8 | ?4.28 | ??41 | ?36.6 | ?3.66 |
| ??2-9 | The benzinum phase | ??30∶70 | Normal pressure | Normal temperature | ????80 | ????8 | Water | Normal pressure | Normal temperature | ????20 | ????0.4 | ?38.9 | ?51.4 | ?5.14 | ?36.9 | ?40.7 | ?4.07 |
| ??2-10 | The benzinum phase | ??40∶60 | Normal pressure | Normal temperature | ????90 | ????9 | Water | Normal pressure | Normal temperature | ????20 | ????0.4 | ?35.5 | ?56.3 | ?5.63 | ?33.1 | ?45.3 | ?4.53 |
| ??2-11 | The benzinum phase | ??50∶50 | Normal pressure | Normal temperature | ????90 | ????9 | Water | Normal pressure | Normal temperature | ????20 | ????0.4 | ?32.6 | ?61.3 | ?6.13 | ?30.2 | ?49.7 | ?4.97 |
| ??2-12 | The benzinum phase | ??60∶40 | Normal pressure | Normal temperature | ????90 | ????10 | Water | Normal pressure | Normal temperature | ????20 | ????0.4 | ?29 | ?69 | ??6.9 | ?26.4 | ?56.8 | ?5.68 |
Table 3 extracts the embodiment list of camptothecine from camptotheca seed
| The embodiment sequence number | One, system plant extracts | Two, multi-solvent extraction | Three, separate | The camptothecine product | |||||||||||||||
| The camptotheca seed gram | Extract solvent | Extract the solvent dosage doubly | Extraction conditions | Extractant and weight % are than chloroform: benzinum: 1% methyl alcohol alkali lye | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid and weight % are than methyl alcohol: 2% sodium hydroxide solution | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | Yield % | The output gram | |||||||
| Time hour | Pressure MPa | Temperature ℃ | Pressure M Pa | Temperature ℃ | The time branch | Pressure MPa | Temperature ℃ | The time branch | |||||||||||
| ?3-1 | ?1000 | Methyl alcohol | ????7 | ??6 | ??0.04 | ??68 | ??5∶90∶5 | Normal pressure | Normal temperature | ??30 | ????5 | ???3∶97 | Normal pressure | Normal temperature | 15 | ?0.3 | ?65.25 | ?0.0459 | ?0.459 |
| ?3-2 | ?1000 | Methyl alcohol | ????7 | ??6 | ??0.04 | ??68 | ??20∶70∶10 | Normal pressure | Normal temperature | ??30 | ????6 | ???20∶80 | Normal pressure | Normal temperature | 15 | ?0.3 | ?82.93 | ?0.0362 | ?0.362 |
| ?3-3 | ?1000 | Methyl alcohol | ????7 | ??6 | ??0.04 | ??68 | ??10∶80∶10 | Normal pressure | Normal temperature | ??50 | ????7 | ???40∶60 | Normal pressure | Normal temperature | 15 | ?0.3 | ?84.17 | ?0.0356 | ?0.356 |
| ?3-4 | ?1000 | Methyl alcohol | ????7 | ??6 | ??0.05 | ??68 | ??25∶60∶15 | Normal pressure | Normal temperature | ??50 | ????9 | ???5∶95 | Normal pressure | Normal temperature | 25 | ?0.3 | ?90.58 | ?0.0331 | ?0.331 |
| ?3-5 | ?1000 | Methyl alcohol | ????10 | ??6 | ??0.05 | ??68 | ??40∶40∶20 | Normal pressure | Normal temperature | ??50 | ????10 | ???20∶80 | Normal pressure | Normal temperature | 25 | ?0.3 | ?95.79 | ?0.0313 | ?0.313 |
| ?3-6 | ?1000 | Methyl alcohol | ????10 | ??6 | ??0.03 | ??68 | ??60∶30∶10 | Normal pressure | Normal temperature | ??80 | ????10 | ???40∶60 | Normal pressure | Normal temperature | 20 | ?0.3 | ?96.1 | ?0.0312 | ?0.312 |
| ?3-7 | ?1000 | Methyl alcohol | ????10 | ??6 | ??0.03 | ??68 | ??70∶15∶15 | Normal pressure | Normal temperature | ??80 | ????10 | ???95∶5 | Normal pressure | Normal temperature | 20 | ?0.4 | ?97.1 | ?0.0309 | ?0.309 |
| ?3-8 | ?1000 | Methyl alcohol | ????10 | ??6 | ??0.03 | ??68 | ??70∶20∶10 | Normal pressure | Normal temperature | ??10 ???0 | ????10 | ???20∶80 | Normal pressure | Normal temperature | 25 | ?0.4 | ?98.3 | ?0.0305 | ?0.305 |
| ?3-9 | ?1000 | Methyl alcohol | ????10 | ??6 | ??0.03 | ??65 | ??90∶5∶5 | Normal pressure | Normal temperature | ??10 ??0 | ????10 | ???97∶3 | Normal pressure | Normal temperature | 25 | ?0.4 | ?88.2 | ?0.0434 | ?0.434 |
Table 4 extracts the embodiment list of hypericin from the plant hypericum perforatum
| The embodiment sequence number | One, just carries plant extracts | Two, multi-solvent extraction | Three, separate | Hypericin | |||||||||||||||
| The hypericum perforatum gram | Extract solvent | Extract the solvent total amount doubly | Extraction conditions | Extractant and weight % ratio | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | The output gram | Yield % | |||||||
| Time hour | Pressure MPa | Temperature ℃ | |||||||||||||||||
| Chloroform: benzinum: pyridine: acetone: methyl alcohol: benzene | The time branch | Pressure M Pa | Temperature ℃ | The time branch | Pressure MPa | Temperature ℃ | |||||||||||||
| ?4-1 | ?1000 | Methyl alcohol | 5 | ?6 | ?0.03 | ?68 | 20∶10∶1∶49∶17∶ 3 | ??20 | Normal pressure | Normal temperature | ????5 | Water | 30 | Normal pressure | Normal temperature | 0.5 | ?4.68 | ?6.4 | ?0.6 |
| ?4-2 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.03 | ?68 | 25∶10∶1∶39∶20∶ 5 | ??20 | Normal pressure | Normal temperature | ????5 | Water | 30 | Normal pressure | Normal temperature | 0.5 | ?4.56 | ?6.6 | ?0.66 |
| ?4-3 | ?1000 | Methyl alcohol | 7 | ?6 | ?0.02 | ?68 | 20∶20∶1∶34∶20∶ 5 | ??30 | Normal pressure | Normal temperature | ????7 | Water | 30 | Normal pressure | Normal temperature | 0.45 | ?3.98 | ?7.5 | ?0.75 |
| ?4-4 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.02 | ?68 | 40∶15∶1∶29∶30∶ 5 | ??30 | Normal pressure | Normal temperature | ????7 | Water | 30 | Normal pressure | Normal temperature | 0.45 | ?2.75 | ?10.9 | ?1.09 |
| ?4-5 | ?1000 | Methyl alcohol | 9 | ?6 | ?0.02 | ?68 | 30∶30∶1∶4∶30∶5 | ??30 | Normal pressure | Normal temperature | ????9 | Water | 30 | Normal pressure | Normal temperature | 0.42 | ?1.66 | ?18.1 | ?1.81 |
| ?4-6 | ?1000 | Methyl alcohol | 10 | ?6 | ?0.05 | ?68 | 20∶35∶1∶9∶30∶5 | ??20 | Normal pressure | Normal temperature | ????9 | Water | 20 | Normal pressure | Normal temperature | 0.26 | ?0.86 | ?34.9 | ?3.49 |
| ?4-7 | ?1000 | Methyl alcohol | 8. 5 | ?6 | ?0.04 | ?68 | 35∶20∶1∶9∶30∶5 | ??20 | Normal pressure | Normal temperature | ????10 | Water | 20 | Normal pressure | Normal temperature | 0.37 | ?0.34 | ?88.2 | ?8.82 |
Table 5 extracts the embodiment list of panaxoside from genseng
| The embodiment sequence number | One, system plant extracts | Two, column extracting | Three, multi-solvent extraction | Four, separate | Panaxoside | |||||||||||||||||||
| The genseng gram | Extract solvent | Extract quantity of solvent doubly | Extraction conditions | Extractant | The extractant total amount doubly | Extraction conditions | Extractant and weight % ratio | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid and weight % ratio | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | Yield % | The output gram | |||||||||
| Time hour | Pressure MPa | Temperature ℃ | ||||||||||||||||||||||
| The time branch | Pressure MPa | Temperature ℃ | Chloroform: benzinum: acetone | The time branch | Pressure MPa | Temperature ℃ | Methyl alcohol: water | The time branch | Pressure MPa | Temperature ℃ | ||||||||||||||
| ????5-1 | ????1000 | Methyl alcohol | ????5 | ??6 | ??0.05 | ??68 | Ethyl acetate | ????12 | ????120 | Normal pressure | Normal temperature | ??10∶ ??50∶40 | ??70 | Normal pressure | Normal temperature | 10 | ?10∶90 | ?20 | Normal pressure | Normal temperature | 0.4 | ?45.7 | ??10.97 | ?109.7 |
| ????5-2 | ????1000 | Methyl alcohol | ????6 | ??6 | ??0.03 | ??68 | Ethyl acetate | ????12 | ????120 | Normal pressure | Normal temperature | ??20∶ ??40∶40 | ??70 | Normal pressure | Normal temperature | 10 | ?20∶80 | ?20 | Normal pressure | Normal temperature | 0.4 | ?50.75 | ??9.85 | ?98.5 |
| ????5-3 | ????1000 | Methyl alcohol | ????7 | ??6 | ??0.02 | ??68 | Ethyl acetate | ????12 | ????120 | Normal pressure | Normal temperature | ??10∶ ??20∶70 | ??90 | Normal pressure | Normal temperature | 9 | ?40∶60 | ?20 | Normal pressure | Normal temperature | 0.4 | ?55.41 | ??9.02 | ?90.2 |
| ????5-4 | ????1000 | Methyl alcohol | ????8 | ??6 | ??0.02 | ??68 | Ethyl acetate | ????15 | ????120 | Normal pressure | Normal temperature | ??10∶ ??30∶60 | ??90 | Normal pressure | Normal temperature | 9 | ?60∶40 | ?20 | Normal pressure | Normal temperature | 0.4 | ?60.02 | ??8.33 | ?83.3 |
| ????5-5 | ????1000 | Methyl alcohol | ????9 | ??6 | ??0.02 | ??68 | Ethyl acetate | ????15 | ????120 | Normal pressure | Normal temperature | ??20∶ ??20∶60 | ??110 | Normal pressure | Normal temperature | 7 | ?20∶80 | ?20 | Normal pressure | Normal temperature | 0.4 | ?58.02 | ??8.62 | ?86.2 |
| ????5-6 | ????1000 | Methyl alcohol | ????10 | ??6 | ??0.05 | ??68 | Ethyl acetate | ????15 | ????120 | Normal pressure | Normal temperature | ??20∶ ??10∶70 | ??110 | Normal pressure | Normal temperature | 7 | ?40∶60 | ?30 | Normal pressure | Normal temperature | 0.4 | ?57.21 | ??8.74 | ?87.4 |
| ????5-7 | ????1000 | Methyl alcohol | ????8.5 | ??6 | ??0.04 | ??68 | Ethyl acetate | ????18 | ????100 | Normal pressure | Normal temperature | ??15∶ ??25∶60 | ??110 | Normal pressure | Normal temperature | 7 | ?60∶40 | ?30 | Normal pressure | Normal temperature | 0.4 | ?55.76 | ??8.97 | ?89.7 |
| ????5-8 | ????1000 | Methyl alcohol | ????7.5 | ??6 | ??0.04 | ??68 | Ethyl acetate | ????18 | ????100 | Normal pressure | Normal temperature | ??25∶ ??25∶50 | ??60 | Normal pressure | Normal temperature | 10 | ?20∶80 | ?30 | Normal pressure | Normal temperature | 0.4 | ?53.62 | ??9.32 | ?93.2 |
| ????5-9 | ????1000 | Methyl alcohol | ????9.5 | ??6 | ??0.03 | ??68 | Ethyl acetate | ????18 | ????100 | Normal pressure | Normal temperature | ??30∶ ??15∶55 | ??60 | Normal pressure | Normal temperature | 10 | ?40∶60 | ?30 | Normal pressure | Normal temperature | 0.4 | ?53.01 | ??9.43 | ?94.3 |
Table 6 extracts the embodiment list of chlorogenic acid from honeysuckle
| The embodiment sequence number | One, system plant extracts | Two, column extracting | Three, multi-solvent extraction | Four, separate | Chlorogenic acid | |||||||||||||||||||
| Honeysuckle | Extract solvent | Extract quantity of solvent doubly | Extraction conditions | Extractant | The extractant total amount doubly | Extraction conditions | Extractant and weight % ratio | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid and weight % ratio | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | Yield % | The output gram | |||||||||
| Time hour | Pressure MPa | Temperature ℃ | The time branch | Pressure MP a | Temperature ℃ | Chloroform: benzinum | The time branch | Pressure MP a | Temperature ℃ | Methyl alcohol: water | The time branch | Pressure MP a | Temperature ℃ | |||||||||||
| ??6-1 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.05 | ?65 | Acetone | 9 | ?200 | Normal pressure | Normal temperature | ??3∶97 | ?60 | Normal pressure | Normal temperature | 8 | ?30∶70 | ?13 | Normal pressure | Normal temperature | 0.4 | ??26.02 | ??5.76 | ?57.6 |
| ??6-2 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.05 | ?65 | Acetone | 5 | ?200 | Normal pressure | Normal temperature | ??20∶80 | ?60 | Normal pressure | Normal temperature | 8 | ?20∶80 | ?10 | Normal pressure | Normal temperature | 0.4 | ??27.6 | ??5.43 | ?54.3 |
| ??6-3 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.05 | ?65 | Acetone | 7 | ?240 | Normal pressure | Normal temperature | ??30∶70 | ?60 | Normal pressure | Normal temperature | 8 | ?40∶60 | ?10 | Normal pressure | Normal temperature | 0.4 | ??30.28 | ??4.95 | ?49.5 |
| ??6-4 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.05 | ?65 | Acetone | 9 | ?240 | Normal pressure | Normal temperature | ??40∶60 | ?60 | Normal pressure | Normal temperature | 8 | ?60∶40 | ?10 | Normal pressure | Normal temperature | 0.4 | ??28.13 | ??5.33 | ?53.3 |
| ??6-5 | ?1000 | Methyl alcohol | 9 | ?6 | ?0.04 | ?65 | Acetone | 7 | ?280 | Normal pressure | Normal temperature | ??50∶50 | ?60 | Normal pressure | Normal temperature | 8 | ?20∶80 | ?15 | Normal pressure | Normal temperature | 0.3 | ??26.3 | ??5.7 | ?57 |
| ??6-6 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.04 | ?65 | Acetone | 7 | ?280 | Normal pressure | Normal temperature | ??60∶40 | ?80 | Normal pressure | Normal temperature | 5 | ?40∶60 | ?15 | Normal pressure | Normal temperature | 0.3 | ??23.99 | ??6.25 | ?62.5 |
| ??6-7 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.04 | ?65 | Acetone | 9 | ?280 | Normal pressure | Normal temperature | ??70∶30 | ?80 | Normal pressure | Normal temperature | 5 | ?60∶40 | ?15 | Normal pressure | Normal temperature | 0.5 | ??22.29 | ??6.73 | ?97 |
| ??6-8 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.04 | ?65 | Acetone | 9 | ?300 | Normal pressure | Normal temperature | ??80∶20 | ?80 | Normal pressure | Normal temperature | 5 | ?20∶80 | ?15 | Normal pressure | Normal temperature | 0.5 | ??21.01 | ??7.14 | ?71.4 |
| ??6-9 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.03 | ?65 | Acetone | 9 | ?300 | Normal pressure | Normal temperature | ??7∶93 | ?80 | Normal pressure | Normal temperature | 5 | ?10∶90 | ?30 | Normal pressure | Normal temperature | 0.5 | ??19.22 | ??7.81 | ?78.1 |
Table 7 is from the embodiment list of rhodiola root extraction rhodioloside
| The embodiment sequence number | One, system plant extracts | Two, column extracting | Three, multi-solvent extraction | Four, separate | Rhodioloside | |||||||||||||||||||
| Rhodiola root | Extract solvent | Extraction quantity of solvent gram | Extraction conditions | Extractant | The extractant total amount doubly | Extraction conditions | Extractant and weight % ratio | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid and weight % ratio | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | Yield % | The output gram | |||||||||
| Time hour | Pressure MPa | Temperature ℃ | The time branch | Pressure MP a | Temperature ℃ | Chloroform: benzinum | The time branch | Pressure MP a | Temperature ℃ | Methyl alcohol: water | The time branch | Pressure MP a | Temperature ℃ | |||||||||||
| ?7-1 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.03 | ?68 | Ethyl acetate | 10 | ?160 | Normal pressure | Normal temperature | 10∶90 | ?20 | Normal pressure | Normal temperature | 5 | ?5∶95 | ?15 | Normal pressure | Normal temperature | 0.3 | ?7.53 | ?6.64 | ?66.4 |
| ?7-2 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.03 | ?68 | Ethyl acetate | 10 | ?360 | Normal pressure | Normal temperature | 20∶80 | ?20 | Normal pressure | Normal temperature | 5 | ?20∶80 | ?15 | Normal pressure | Normal temperature | 0.3 | ?8.62 | ?5.8 | ?58 |
| ?7-3 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.03 | ?68 | Ethyl acetate | 10 | ?360 | Normal pressure | Normal temperature | 30∶70 | ?20 | Normal pressure | Normal temperature | 5 | ?40∶60 | ?15 | Normal pressure | Normal temperature | 0.3 | ?10.3 | ?4.84 | ?48.4 |
| ?7-4 | ?1000 | Methyl alcohol | 6 | ?6 | ?0.03 | ?68 | Ethyl acetate | 9 | ?360 | Normal pressure | Normal temperature | 40∶60 | ?25 | Normal pressure | Normal temperature | 4 | ?60∶40 | ?15 | Normal pressure | Normal temperature | 0.3 | ?10 | ?5 | ?50 |
| ?7-5 | ?1000 | Methyl alcohol | 9 | ?6 | ?0.03 | ?68 | Ethyl acetate | 9 | ?480 | Normal pressure | Normal temperature | 50∶50 | ?25 | Normal pressure | Normal temperature | 4 | ?20∶80 | ?15 | Normal pressure | Normal temperature | 0.3 | ?9.65 | ?5.18 | ?51.8 |
| ?7-6 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.03 | ?68 | Ethyl acetate | 9 | ?300 | Normal pressure | Normal temperature | 60∶40 | ?25 | Normal pressure | Normal temperature | 4 | ?40∶60 | ?25 | Normal pressure | Normal temperature | 0.3 | ?8.83 | ?5.66 | ?56.6 |
| ?7-7 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.03 | ?68 | Ethyl acetate | 9 | ?300 | Normal pressure | Normal temperature | 70∶30 | ?30 | Normal pressure | Normal temperature | 4 | ?60∶40 | ?25 | Normal pressure | Normal temperature | 0.4 | ?8.11 | ?6.17 | ?61.7 |
| ?7-8 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.03 | ?68 | Ethyl acetate | 9 | ?300 | Normal pressure | Normal temperature | 80∶20 | ?30 | Normal pressure | Normal temperature | 4 | ?20∶80 | ?25 | Normal pressure | Normal temperature | 0.4 | ?7.51 | ?6.66 | ?66.6 |
| ?7-9 | ?1000 | Methyl alcohol | 8 | ?6 | ?0.03 | ?68 | Ethyl acetate | 9 | ?300 | Normal pressure | Normal temperature | 90∶10 | ?40 | Normal pressure | Normal temperature | 8 | ?40∶60 | ?25 | Normal pressure | Normal temperature | 0.4 | ?6.88 | ?7.27 | ?72.7 |
From frutus cnidii, the come together embodiment list of Osthole of table 8
| The embodiment sequence number | One, just carries plant extracts | Two, multi-solvent extraction | Three, separate | Osthole | |||||||||||||||
| The frutus cnidii gram | Extract solvent | Extract the solvent total amount doubly | Extraction conditions | Extractant and weight % ratio | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid | Phase-splitting bar ox | Phase-splitting liquid total amount doubly | Content % | The output gram | Yield % | |||||||
| Time hour | Pressure MPa | Temperature ℃ | The time branch | Pressure MP a | Temperature ℃ | ||||||||||||||
| Chloroform: benzinum: methyl alcohol | The time branch | Pressure MP a | Temperature ℃ | ||||||||||||||||
| ?8-1 | ??1000 | Ethanol | 5 | ?6 | ?0.03 | ?75 | ??90∶5∶5 | ??20 | Normal pressure | Normal temperature | ??5 | 1% salt sour water | 30 | Normal pressure | Normal temperature | 0.5 | ?5.68 | ??10.4 | ?1.04 |
| ?8-2 | ??1000 | Ethanol | 6 | ?6 | ?0.03 | ?75 | ??80∶10∶10 | ??20 | Normal pressure | Normal temperature | ??5 | 1% salt sour water | 30 | Normal pressure | Normal temperature | 0.5 | ?6.56 | ??11.6 | ?1.16 |
| ?8-3 | ??1000 | Ethanol | 7 | ?6 | ?0.02 | ?75 | ??70∶20∶10 | ??30 | Normal pressure | Normal temperature | ??7 | 1% salt sour water | 30 | Normal pressure | Normal temperature | 0.45 | ?5.98 | ??11.5 | ?1.15 |
| ?8-4 | ??1000 | Ethanol | 8 | ?6 | ?0.02 | ?75 | ??60∶30∶10 | ??30 | Normal pressure | Normal temperature | ??7 | 1% salt sour water | 30 | Normal pressure | Normal temperature | 0.45 | ?5.31 | ??10.9 | ?1.09 |
| ?8-5 | ??1000 | Ethanol | 9 | ?6 | ?0.02 | ?75 | ??40∶40∶20 | ??30 | Normal pressure | Normal temperature | ??9 | 1% salt sour water | 30 | Normal pressure | Normal temperature | 0.42 | ?5.10 | ??11.1 | ?1.11 |
| ?8-6 | ??1000 | Ethanol | 10 | ?6 | ?0.05 | ?75 | ??30∶50∶20 | ??20 | Normal pressure | Normal temperature | ??9 | 1% salt sour water | 20 | Normal pressure | Normal temperature | 0.26 | ?3.9 | ??11.7 | ?1.17 |
| ?8-7 | ??1000 | Ethanol | 8. 5 | ?6 | ?0.04 | ?75 | ??10∶80∶10 | ??20 | Normal pressure | Normal temperature | ??10 | 1% salt sour water | 20 | Normal pressure | Normal temperature | 0.37 | ?3.34 | ??10.8 | ?1.08 |
| The embodiment sequence number | One, just carries plant extracts | Two, multi-solvent extraction | Three, separate | Schizandrin | |||||||||||||||
| Fruit of Chinese magnoliavine gram | Extract solvent | Extract the solvent total amount doubly | Extraction conditions | Extractant and weight % ratio | Extraction conditions | The extractant total amount doubly | Phase-splitting liquid and weight % ratio | The phase-splitting condition | Phase-splitting liquid total amount doubly | Content % | The output gram | Yield % | |||||||
| The time branch | Pressure MP a | Temperature ℃ | The time branch | Pressure MP a | Temperature ℃ | ||||||||||||||
| The time branch | Pressure MPa | Temperature ℃ | Chloroform: benzene: methyl alcohol | Methyl alcohol: water | |||||||||||||||
| ??9-1 | ??1000 | Ethanol | ???5 | ??6 | ??0.03 | ??75 | ???90∶5∶5 | ??20 | Normal pressure | Normal temperature | ??5 | ??50∶50 | ??30 | Normal pressure | Normal temperature | ??0.5 | ??10.68 | ?12.1 | ??1.21 |
| ??9-2 | ??1000 | Ethanol | ???6 | ??6 | ??0.03 | ??75 | ???60∶30∶10 | ??20 | Normal pressure | Normal temperature | ??5 | ??40∶60 | ??30 | Normal pressure | Normal temperature | ??0.5 | ??11.56 | ?12.5 | ??1.25 |
| ??9-3 | ??1000 | Ethanol | ???7 | ??6 | ??0.02 | ??75 | ???40∶50∶10 | ??30 | Normal pressure | Normal temperature | ??7 | ??30∶70 | ??30 | Normal pressure | Normal temperature | ??0.45 | ??11.98 | ?13.5 | ??1.3 |
| ??9-4 | ??1000 | Ethanol | ???8 | ??6 | ??0.02 | ??75 | ???20∶60∶20 | ??30 | Normal pressure | Normal temperature | ??7 | ??5∶95 | ??30 | Normal pressure | Normal temperature | ??0.45 | ??12.5 | ?13.9 | ??1.39 |
| ??9-5 | ??1000 | Ethanol | ???9 | ??6 | ??0.02 | ??75 | ???10∶70∶20 | ??30 | Normal pressure | Normal temperature | ??9 | ??20∶80 | ??30 | Normal pressure | Normal temperature | ??0.42 | ??12.66 | ?13.1 | ??1.31 |
| ??9-6 | ??1000 | Ethanol | ???10 | ??6 | ??0.05 | ??75 | ???5∶80∶15 | ??20 | Normal pressure | Normal temperature | ??9 | ??50∶50 | ??20 | Normal pressure | Normal temperature | ??0.26 | ??12.86 | ?13.9 | ??1.39 |
| ??9-7 | ??1000 | Ethanol | ???8.5 | ??6 | ??0.04 | ??75 | ???5∶90∶5 | ??20 | Normal pressure | Normal temperature | ??10 | ??50∶50 | ??20 | Normal pressure | Normal temperature | ??0.37 | ??11.34 | ?12.8 | ??1.28 |
From the fruit of Chinese magnoliavine, the come together embodiment list of schizandrin of table 9
Claims (35)
1, a kind of multi-solvent extracting process is characterized in that having the following step that carries out successively:
1) multi-solvent extraction: in raw material, add the extractant of forming by at least two kinds of solvent, extraction process carries out in the homogeneous phase of extractant, the weight of extractant is 5～10 times of raw material weight, the weight of each solvent is 1～(100-N) % of extractant gross weight, N is a solvent kind number, N=2～6 obtain extraction solution through extraction;
2) separate: in extraction solution, add the phase-splitting liquid that at least a solvent is formed, phase process carries out in extraction solution, form the conjugation phase, the weight of phase-splitting liquid is 0.25～0.5 times of extraction solution, and the weight of each solvent is 1～(100-M) % of phase-splitting liquid gross weight, and M is a solvent kind number, M=1～6, through leaving standstill, extraction solution is separated into object phase that contains object or the two-phase at least that the non-object phase that does not contain object is arranged, take out each phase;
3) or to object at least once circulate mutually, above-mentioned steps 1 is carried out in each circulation successively) multi-solvent extraction, 2) separate;
4) reclaim solvent: each phase that will take out, heating is respectively reclaimed solvent or is sloughed moisture, obtains object.
2, a kind of multi-solvent extracting process according to claim 1 is characterized in that having the following step that carries out successively:
1) multi-solvent extraction: in raw material, add the extractant of forming by at least two kinds of solvent, extraction process carries out in the homogeneous phase of extractant, the weight of extractant is 5～10 times of raw material weight, the weight of each solvent is 1～(100-N) % of extractant gross weight, N is a solvent kind number, N=2～3 obtain extraction solution through extraction;
2) separate: in extraction solution, add the phase-splitting liquid that at least a solvent is formed, phase process carries out in extraction solution, form the conjugation phase, the weight of phase-splitting liquid is 0.25～0.5 times of extraction solution, and the weight of each solvent is 1～(100-M) % of phase-splitting liquid gross weight, and M is a solvent kind number, M=1～3, through leaving standstill, extraction solution is separated into object phase that contains object or the two-phase at least that the non-object phase that does not contain object is arranged, take out each phase;
3) or to object at least once circulate mutually, above-mentioned steps 1 is carried out in each circulation successively) multi-solvent extraction, 2) separate;
4) reclaim solvent: each phase that will take out, heating is respectively reclaimed solvent or is sloughed moisture, obtains object.
3, multi-solvent extracting process according to claim 1, it is characterized in that said raw material is the plant material primary extract of plant material preparation, said multi-solvent extraction step is carried out under normal temperature, condition of normal pressure, and stirring extracted 15～120 minutes, the elapsed-time standards that leaves standstill of said separating step is 10～30 minutes, and the heating-up temperature of said recovery solvent step is 50～120 degree Celsius.
4, multi-solvent extracting process according to claim 2, it is characterized in that said raw material is the plant material primary extract of plant material preparation, said multi-solvent extraction step is carried out under normal temperature, condition of normal pressure, and stirring extracted 15～120 minutes, the elapsed-time standards that leaves standstill of said separating step is 10～30 minutes, and the heating-up temperature of said recovery solvent step is 50～120 degree Celsius.
5, multi-solvent extracting process according to claim 3 is characterized in that the following step is carried out in the preparation of said plant primary extract successively:
1) clean: at least a cleaning plant material in water or the organic solvent, remove impurity;
2) extract: add a kind of extraction solvent, the weight of extracting solvent is 5～10 times of plant material weight, extracts under normal temperature or 30 degree～120 degree Celsius, normal pressure or pressurization 0.5MPa, extracts once in per 2 hours, extracts at least three times, obtains plant extraction liquid;
3) reclaim solvent: being heated to temperature is 50～120 degree Celsius, reclaims the extraction solvent in the extract or sloughs moisture, makes the plant primary extract.
6, multi-solvent extracting process according to claim 4 is characterized in that the following step is carried out in the preparation of said plant primary extract successively:
1) clean: at least a cleaning plant material in water or the organic solvent, remove impurity;
2) extract: add a kind of extraction solvent, the weight of extracting solvent is 5～10 times of plant material weight, extracts under normal temperature or 30 degree～120 degree Celsius, normal pressure or pressurization 0.5MPa, extracts once in per 2 hours, extracts at least three times, obtains plant extraction liquid;
3) reclaim solvent: being heated to temperature is 50～120 degree Celsius, reclaims the extraction solvent in the extract or sloughs moisture, makes the plant primary extract.
7, multi-solvent extracting process according to claim 1 is characterized in that before the said multi-solvent extraction step or carries out column extracting.
8, multi-solvent extracting process according to claim 2 is characterized in that before the said multi-solvent extraction step or carries out column extracting.
9, multi-solvent extracting process according to claim 3 is characterized in that before the said multi-solvent extraction step or carries out column extracting.
10, multi-solvent extracting process according to claim 4 is characterized in that before the said multi-solvent extraction step or carries out column extracting.
11, multi-solvent extracting process according to claim 5 is characterized in that before the said multi-solvent extraction step or carries out column extracting.
12, multi-solvent extracting process according to claim 6 is characterized in that before the said multi-solvent extraction step or carries out column extracting.
13,, it is characterized in that said plant material is the plant that contains at least a active components of plants in chromone and derivative class, organic acid, phenols and tannin, lipid, quinones, saponin class, terpene, alkaloids, sugar and derivative thereof, lactones, coumarin and isocoumarin class, lignanoids, cardiac stimulant glucoside, C12 steroid glucoside, volatile ingredient, the bitter principle according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process.
14, multi-solvent extracting process according to claim 5 is characterized in that said extraction solvent is C
1～C
10Organic solvent, water, aqueous slkali, acid solution.
15, multi-solvent extracting process according to claim 6 is characterized in that said extraction solvent is C
1～C
10Organic solvent, water, aqueous slkali, acid solution.
16, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, it is characterized in that said extractant is C
1～C
10Organic solvent, water, aqueous slkali, acid solution.
17, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, it is characterized in that said phase-splitting liquid is C
1～C
10Organic solvent, water, aqueous slkali, acid solution.
18, multi-solvent extracting process according to claim 14 is characterized in that said C
1～C
10Organic solvent be ethane; Methylpentane; Dimethylbutane; Heptane; Octane; Trimethylpentane; Nonane; Trimethyl ethane; Benzinum; Gasoline; Pentamethylene; Methyl cyclopentane; Cyclohexane; Hexahydrotoluene; Ethyl cyclohexane; Cyclohexene; Firpene; Limonene; Benzene; Styrene; Toluene; Ortho-xylene; Meta-xylene; Paraxylene; Dimethylbenzene; Ethylbenzene; Diethylbenzene; Butylbenzene; Carrene; Chloroform; Carbon tetrachloride; Dichloroethanes; Trichloroethanes; Dichloroethylene; Trichloro-ethylene; Tetrachloro-ethylene; Chloropropane; Dichloropropane; Chlorobutane; Dichloroetane; Dichloro-dimethyl propane; Bromofom; Bromoethane; Bromofume; N-Propyl Bromide; Dibromopropane; Chlorobenzene; O-dichlorohenzene; M-dichlorobenzene; Paracide; Ortho-chlorotolu'ene; Parachlorotoluene; Bromobenzene; Fluorobenzene; Benzotrifluoride; Methylene bromide; Dibromopropane; Methyl alcohol; Ethanol; Propyl alcohol; Isopropyl alcohol; N-butanol; Isobutanol; Sec-butyl alcohol; The tert-butyl alcohol; Amylalcohol; Isoamyl alcohol; Phenol; Cresols; Ether; Propyl ether; Isopropyl ether; Butyl ether; The second amyl ether; Methyl phenyl ethers anisole; Furans; Methylfuran; Oxolane; Oxinane; Dimethoxym ethane; Acetal; Butyraldehyde; Acetone; Butanone; Pentanone; Hexanone; Methylpentanone; Heptanone; Cyclohexanone; Methyl cyclohexanone; Espeleton; Formic acid; Acetic acid; Propionic acid; Butyric acid; Valeric acid; Acetic anhydride; Propionic andydride; Methyl formate; Ethyl formate; Propyl formate; Butyl formate; Amyl formate; Methyl acetate; Ethyl acetate; Butyl acetate; Pentyl acetate; Methyl propionate; Ethyl propionate.
19, multi-solvent extracting process according to claim 15 is characterized in that said C
1～C
10Organic solvent be ethane; Methylpentane; Dimethylbutane; Heptane; Octane; Trimethylpentane; Nonane; Trimethyl ethane; Benzinum; Gasoline; Pentamethylene; Methyl cyclopentane; Cyclohexane; Hexahydrotoluene; Ethyl cyclohexane; Cyclohexene; Firpene; Limonene; Benzene; Styrene; Toluene; Ortho-xylene; Meta-xylene; Paraxylene; Dimethylbenzene; Ethylbenzene; Diethylbenzene; Butylbenzene; Carrene; Chloroform; Carbon tetrachloride; Dichloroethanes; Trichloroethanes; Dichloroethylene; Trichloro-ethylene; Tetrachloro-ethylene; Chloropropane; Dichloropropane; Chlorobutane; Dichloroetane; Dichloro-dimethyl propane; Bromofom; Bromoethane; Bromofume; N-Propyl Bromide; Dibromopropane; Chlorobenzene; O-dichlorohenzene; M-dichlorobenzene; Paracide; Ortho-chlorotolu'ene; Parachlorotoluene; Bromobenzene; Fluorobenzene; Benzotrifluoride; Methylene bromide; Dibromopropane; Methyl alcohol; Ethanol; Propyl alcohol; Isopropyl alcohol; N-butanol; Isobutanol; Sec-butyl alcohol; The tert-butyl alcohol; Amylalcohol; Isoamyl alcohol; Phenol; Cresols; Ether; Propyl ether; Isopropyl ether; Butyl ether; The second amyl ether; Methyl phenyl ethers anisole; Furans; Methylfuran; Oxolane; Oxinane; Dimethoxym ethane; Acetal; Butyraldehyde; Acetone; Butanone; Pentanone; Hexanone; Methylpentanone; Heptanone; Cyclohexanone; Methyl cyclohexanone; Espeleton; Formic acid; Acetic acid; Propionic acid; Butyric acid; Valeric acid; Acetic anhydride; Propionic andydride; Methyl formate; Ethyl formate; Propyl formate; Butyl formate; Amyl formate; Methyl acetate; Ethyl acetate; Butyl acetate; Pentyl acetate; Methyl propionate; Ethyl propionate.
20, multi-solvent extracting process according to claim 16 is characterized in that said C
1～C
10Organic solvent be ethane; Methylpentane; Dimethylbutane; Heptane; Octane; Trimethylpentane; Nonane; Trimethyl ethane; Benzinum; Gasoline; Pentamethylene; Methyl cyclopentane; Cyclohexane; Hexahydrotoluene; Ethyl cyclohexane; Cyclohexene; Firpene; Limonene; Benzene; Styrene; Toluene; Ortho-xylene; Meta-xylene; Paraxylene; Dimethylbenzene; Ethylbenzene; Diethylbenzene; Butylbenzene; Carrene; Chloroform; Carbon tetrachloride; Dichloroethanes; Trichloroethanes; Dichloroethylene; Trichloro-ethylene; Tetrachloro-ethylene; Chloropropane; Dichloropropane; Chlorobutane; Dichloroetane; Dichloro-dimethyl propane; Bromofom; Bromoethane; Bromofume; N-Propyl Bromide; Dibromopropane; Chlorobenzene; O-dichlorohenzene; M-dichlorobenzene; Paracide; Ortho-chlorotolu'ene; Parachlorotoluene; Bromobenzene; Fluorobenzene; Benzotrifluoride; Methylene bromide; Dibromopropane; Methyl alcohol; Ethanol; Propyl alcohol; Isopropyl alcohol; N-butanol; Isobutanol; Sec-butyl alcohol; The tert-butyl alcohol; Amylalcohol; Isoamyl alcohol; Phenol; Cresols; Ether; Propyl ether; Isopropyl ether; Butyl ether; The second amyl ether; Methyl phenyl ethers anisole; Furans; Methylfuran; Oxolane; Oxinane; Dimethoxym ethane; Acetal; Butyraldehyde; Acetone; Butanone; Pentanone; Hexanone; Methylpentanone; Heptanone; Cyclohexanone; Methyl cyclohexanone; Espeleton; Formic acid; Acetic acid; Propionic acid; Butyric acid; Valeric acid; Acetic anhydride; Propionic andydride; Methyl formate; Ethyl formate; Propyl formate; Butyl formate; Amyl formate; Methyl acetate; Ethyl acetate; Butyl acetate; Pentyl acetate; Methyl propionate; Ethyl propionate.
21, multi-solvent extracting process according to claim 17 is characterized in that said C
1～C
10Organic solvent be ethane; Methylpentane; Dimethylbutane; Heptane; Octane; Trimethylpentane; Nonane; Trimethyl ethane; Benzinum; Gasoline; Pentamethylene; Methyl cyclopentane; Cyclohexane; Hexahydrotoluene; Ethyl cyclohexane; Cyclohexene; Firpene; Limonene; Benzene; Styrene; Toluene; Ortho-xylene; Meta-xylene; Paraxylene; Dimethylbenzene; Ethylbenzene; Diethylbenzene; Butylbenzene; Carrene; Chloroform; Carbon tetrachloride; Dichloroethanes; Trichloroethanes; Dichloroethylene; Trichloro-ethylene; Tetrachloro-ethylene; Chloropropane; Dichloropropane; Chlorobutane; Dichloroetane; Dichloro-dimethyl propane; Bromofom; Bromoethane; Bromofume; N-Propyl Bromide; Dibromopropane; Chlorobenzene; O-dichlorohenzene; M-dichlorobenzene; Paracide; Ortho-chlorotolu'ene; Parachlorotoluene; Bromobenzene; Fluorobenzene; Benzotrifluoride; Methylene bromide; Dibromopropane; Methyl alcohol; Ethanol; Propyl alcohol; Isopropyl alcohol; N-butanol; Isobutanol; Sec-butyl alcohol; The tert-butyl alcohol; Amylalcohol; Isoamyl alcohol; Phenol; Cresols; Ether; Propyl ether; Isopropyl ether; Butyl ether; The second amyl ether; Methyl phenyl ethers anisole; Furans; Methylfuran; Oxolane; Oxinane; Dimethoxym ethane; Acetal; Butyraldehyde; Acetone; Butanone; Pentanone; Hexanone; Methylpentanone; Heptanone; Cyclohexanone; Methyl cyclohexanone; Espeleton; Formic acid; Acetic acid; Propionic acid; Butyric acid; Valeric acid; Acetic anhydride; Propionic andydride; Methyl formate; Ethyl formate; Propyl formate; Butyl formate; Amyl formate; Methyl acetate; Ethyl acetate; Butyl acetate; Pentyl acetate; Methyl propionate; Ethyl propionate.
22, multi-solvent extracting process according to claim 14 is characterized in that said aqueous slkali is sodium hydroxide solution, potassium hydroxide solution, aqua calcis, sodium bicarbonate solution, ammoniacal liquor.
23, multi-solvent extracting process according to claim 15 is characterized in that said aqueous slkali is sodium hydroxide solution, potassium hydroxide solution, aqua calcis, sodium bicarbonate solution, ammoniacal liquor.
24, multi-solvent extracting process according to claim 16 is characterized in that said aqueous slkali is sodium hydroxide solution, potassium hydroxide solution, aqua calcis, sodium bicarbonate solution, ammoniacal liquor.
25, multi-solvent extracting process according to claim 17 is characterized in that said aqueous slkali is sodium hydroxide solution, potassium hydroxide solution, aqua calcis, sodium bicarbonate solution, ammoniacal liquor.
26, multi-solvent extracting process according to claim 14 is characterized in that said acid solution is hydrochloric acid solution, sulfuric acid solution, carbon acid solution.
27, multi-solvent extracting process according to claim 15 is characterized in that said acid solution is hydrochloric acid solution, sulfuric acid solution, carbon acid solution.
28, multi-solvent extracting process according to claim 16 is characterized in that said acid solution is hydrochloric acid solution, sulfuric acid solution, carbon acid solution.
29, multi-solvent extracting process according to claim 17 is characterized in that said acid solution is hydrochloric acid solution, sulfuric acid solution, carbon acid solution.
30, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, the weight that it is characterized in that each solvent in the said extractant is 10～(90-N) % of extractant gross weight.
31, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, the weight that it is characterized in that each solvent in the said extractant is 20～(80-N) % of extractant gross weight.
32, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, the weight that it is characterized in that each solvent in the said extractant is 30～(70-N) % of extractant gross weight.
33, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, the weight that it is characterized in that each solvent in the said phase-splitting liquid is 10～(90-M) % of phase-splitting liquid gross weight.
34, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, the weight that it is characterized in that each solvent in the said phase-splitting liquid is 20～(80-M) % of phase-splitting liquid gross weight.
35, according to claim 3,4,5,6,7,8,9,10,11 or 12 described multi-solvent extracting process, the weight that it is characterized in that each solvent in the said phase-splitting liquid is 30～(70-M) % of phase-splitting liquid gross weight.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03117695XA CN1180866C (en) | 2003-04-15 | 2003-04-15 | Multiple solvent extraction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03117695XA CN1180866C (en) | 2003-04-15 | 2003-04-15 | Multiple solvent extraction method |
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| Publication Number | Publication Date |
|---|---|
| CN1443592A true CN1443592A (en) | 2003-09-24 |
| CN1180866C CN1180866C (en) | 2004-12-22 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101580525B (en) * | 2009-06-06 | 2011-06-29 | 中国科学院西北高原生物研究所 | Method for extracting salidroside, polysaccharose and tannin-type substances from rhodiola root crude drugs |
| US8876925B2 (en) | 2008-12-23 | 2014-11-04 | Kior, Inc. | Bio-oil having reduced mineral content, and process for making |
| CN104271212A (en) * | 2012-02-02 | 2015-01-07 | 绿色能源有限公司 | Methods for recovering and/or removing reagents from porous media |
| CN107670333A (en) * | 2017-08-25 | 2018-02-09 | 中国石油天然气股份有限公司 | Method for separating alkylphenol in crude oil |
| CN110590863A (en) * | 2019-08-15 | 2019-12-20 | 安徽金禾实业股份有限公司 | Extraction method of sucralose-6-ethyl ester |
| CN111544923A (en) * | 2020-05-08 | 2020-08-18 | 河北瑞龙生物科技有限公司 | Preparation method of snow pear extract for cigarettes |
| CN112970860A (en) * | 2021-04-15 | 2021-06-18 | 王跃生 | Selenium-rich lipid-lowering edible oil and preparation method thereof |
| CN114053752A (en) * | 2021-11-18 | 2022-02-18 | 西安天一生物技术股份有限公司 | Method for removing benzopyrene in hypericum perforatum extract by using solvent |
| CN116041908A (en) * | 2023-02-02 | 2023-05-02 | 南雄市星隆化工有限公司 | Modified epoxy resin with antifouling effect and preparation method thereof |
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2003
- 2003-04-15 CN CNB03117695XA patent/CN1180866C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8876925B2 (en) | 2008-12-23 | 2014-11-04 | Kior, Inc. | Bio-oil having reduced mineral content, and process for making |
| CN101580525B (en) * | 2009-06-06 | 2011-06-29 | 中国科学院西北高原生物研究所 | Method for extracting salidroside, polysaccharose and tannin-type substances from rhodiola root crude drugs |
| CN104271212A (en) * | 2012-02-02 | 2015-01-07 | 绿色能源有限公司 | Methods for recovering and/or removing reagents from porous media |
| US9181490B2 (en) | 2012-02-02 | 2015-11-10 | Green Source Holdings Llc | Methods for recovering and/or removing reagents from porous media |
| CN104271212B (en) * | 2012-02-02 | 2017-03-29 | 绿色能源有限公司 | For the method for reclaiming from permeability medium and/or remove reagent |
| CN107670333B (en) * | 2017-08-25 | 2019-12-10 | 中国石油天然气股份有限公司 | Method for separating alkylphenol in crude oil |
| CN107670333A (en) * | 2017-08-25 | 2018-02-09 | 中国石油天然气股份有限公司 | Method for separating alkylphenol in crude oil |
| CN110590863A (en) * | 2019-08-15 | 2019-12-20 | 安徽金禾实业股份有限公司 | Extraction method of sucralose-6-ethyl ester |
| CN111544923A (en) * | 2020-05-08 | 2020-08-18 | 河北瑞龙生物科技有限公司 | Preparation method of snow pear extract for cigarettes |
| CN111544923B (en) * | 2020-05-08 | 2021-12-10 | 河北瑞龙生物科技有限公司 | Preparation method of snow pear extract for cigarettes |
| CN112970860A (en) * | 2021-04-15 | 2021-06-18 | 王跃生 | Selenium-rich lipid-lowering edible oil and preparation method thereof |
| CN112970860B (en) * | 2021-04-15 | 2022-08-02 | 安徽硒都云峰食品有限公司 | Selenium-rich lipid-lowering edible oil and preparation method thereof |
| CN114053752A (en) * | 2021-11-18 | 2022-02-18 | 西安天一生物技术股份有限公司 | Method for removing benzopyrene in hypericum perforatum extract by using solvent |
| CN116041908A (en) * | 2023-02-02 | 2023-05-02 | 南雄市星隆化工有限公司 | Modified epoxy resin with antifouling effect and preparation method thereof |
| CN116041908B (en) * | 2023-02-02 | 2023-09-05 | 南雄市星隆化工有限公司 | Modified epoxy resin with antifouling effect and preparation method thereof |
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