CN1318566A - Solvent extraction process of extracting and separating polysaccharide from algae leaching liquor - Google Patents
Solvent extraction process of extracting and separating polysaccharide from algae leaching liquor Download PDFInfo
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Abstract
Algae leaching liquor is extracted with organic phase comprising water insoluble reagent and solvent so that polysaccharide enters to the organic phase for separation from water soluble impurities. Polysaccharide in organic phase is counter extracted with water solution of salt into water phase and thus further separated from water insoluble impurities and enriched with the organic phase being returned to extraction. Polysaccharide in salt solution is recovered through conventional process. The said process has high polysaccharide recovering rate and purity and low production cost.
Description
The present invention relates to the method for extraction separation Sargassum polysaccharides from the aqueous leaching solution of marine alga, particularly relate to the method that adopts solvent extraction extraction separation Sargassum polysaccharides from the aqueous leaching solution of marine alga.
Sargassum polysaccharides has unique physiologically active, increasing result of study has demonstrated Sargassum polysaccharides and has had the wide development application prospect, as the brown alga of one of important marine economy algae, biological activity that algal polysaccharide had and medicines and health protection effect that it is contained are revealed.Especially fucoidin (fucoidan), many studies show that have antitumor, anticoagulation, effect such as antiulcer agent and immunostimulant.Contained polysaccharide mainly comprises algin, fucoidin and laminaran etc. in the brown alga.Can carry out industrial algal polysaccharide so far is algin.Mainly comprise from the process of marine algae plant extract polysaccharide: fragmentation, lixiviate, separation, purifying etc.The extraction separation polysaccharide is the key link of the influence process rate of recovery and economic benefit and quality product from vat liquor and lixiviate reaches.The traditional method that extracts the polysaccharide of biologically active so far from algae leaching liquor mainly is to adopt water-miscible organic solvent (as the ethanol) precipitator method.
As document 1: the cell wall polysaccharides of marine green algae admant water shield. extract and chemical constitution.(B.Ray and M.lahaye, Cell-Wall polysaccharides from the marine green alga Ulva " rigid " (Ulvales, Chlorophyta) .Extraction and chemical composition.Carbohydrate.1995, after introducing sodium oxalate and aqueous extract ultrafiltration 274:251-261) with sea lettuce (Ulva rigida), add 3 times of amount 95% ethanol sedimentation polysaccharide, throw out is through centrifugal, be that 80%, 95% ethanol and acetone thoroughly wash with concentration successively, use P under the vacuum
2O
5Drying gets polysaccharide crude A.
As document 2: the antitumor polysaccharide fractions of mouse tail algae. (H.Ito and M.Sugiura, AntitumorPolysaccharide Fraction from Sargassum thunbergii, Chem Pharm Bull, 1976,24 (5): introduce 1114-1115): from the acid vat liquor of Sargassum thunbergii, obtain polysaccharide through dialysis and 3 times of amount dehydrated alcohol precipitator method.
As document 3:(Zhou Huiping, Zhu Haiyan, Chen Qionghua, the separation of sea grass polysaccharide, purifying and analysis, journal of biological chemistry, 1995,11 (1): 91-93) from the hot water vat liquor of Enteromorpha (Enteromorfha prolifera), after Deproteinization, dialysis, use 95% ethanol sedimentation, obtain sea grass polysaccharide half pure product.
It is virtuous to open that as document 4:(, Yu Lijun, Xiao Xiang etc., the physiologically active and the biochemical research of mouse tail algae alcohol extract, Chinese marine drug, 1994, (3): 1-10; Zhao Jixun, Xu Jianyang, Jiang Shikui etc., the research of mouse tail polysaccharides chemical ingredients and antiulcer action, marine drug, 1987, (1): 19-22) then isolate mouse tail polysaccharides by ethanol precipitation from the hot water vat liquor of mouse tail algae.
As document 5:(Zhou Zhigang, Li Pengfu, Liu Zhili etc., the research of three kinds of spirulinas and protein, polysaccharide and contaminated with lipid selenium, 1997,28 (4): 363-370) isolate outside the born of the same parents and intracellular polyse from the nutrient solution of spirulina and the vat liquor of frond respectively with ethanol precipitation.
As the document 6:(bright marquis that records, high flood peak, Cao Wenda, uses model dawn
13The C-NMR spectrography is studied the constitutional features of several red algae sulfur-bearing Polygalactans, Oceanologia et Limnologia Sinica, 1996,27 (3): 330-335) go out the sulfur-bearing Polygalactan with 3 times of ethanol sedimentations from the water extract of red algae.
As document 7: the anti-tumor activity of edible seaweed: from the leukemic effect of anti-L-1210 (the I.Yamamoto et al of the thick fucoidin fraction of edible brown alga preparation, Antitumor activity of edible marine algae:Effect of crude fucoidanfractions preparedfrom edible brown seaweeds againstL-1210leukemia, Hydrobiologia, 1984,116/117:145-148) introduce: the thick fucoidin that then adopts the ethanol step-by-step precipitation method and come grading purification from Eisenia bicyclis, to obtain in conjunction with the CPC precipitator method.Its process is: 3 gram Crude polysaccharides are dissolved in 120 ml distilled waters, and adding 100 ml concns are 5% cetylpyridinium chloride in the solution again, stir the mixture once in a while, at room temperature place 2 hours, and are centrifugal then.Throw out with 30 ml concns be 5% cetylpyridinium chloride solution washing, centrifugal after, be dissolved in 200 milliliters of 3mol/L CaCl
2Solution stirred 30 minutes.Mixture is centrifugal, and throw out is dissolved in 100 milliliters of 3mol/L CaCl
2Solution, centrifugal then, filtration, filtrate and last time centrifugal supernatant merging.Merge and to add ethanol in the mixed solution to make final alcohol concn be 85% (volume/volume).This solution was placed 2 hours in room temperature, and is centrifugal.Throw out is dissolved in 100 milliliters of 3mol/LCaCl again
2Solution stirred 30 minutes, and is centrifugal then.Adding ethanol in the gained supernatant, to make final alcohol concn be 85% (volume/volume), and the solution kept at room temperature overnight is centrifugal then.Throw out does not have chlorine and disappears in the absorption maximum value of wavelength 260nm until wash water several times with 85% (volume/volume) washing with alcohol, handles with ethanol and ether then, 45 ℃ of dried overnight.Final product is filbert, output 0.44 gram, Fucose content 30.2%.
Thereby the ethanol sedimentation ratio juris mainly is to make the polysaccharide dehydration produce precipitation by the specific inductivity that reduces the aqueous solution to come separating polyose, this method almost is applicable to all water-soluble polysaccharides, though homopolysaccharide can fractional precipitation under the condition of different concentration ethanol, but specificity is not high, cause the separation selectivity of required polysaccharide relatively poor, the purity that improves polysaccharide needs through the repeated multiple times reprecipitation, thereby causes polysaccharide loss big, has reduced the rate of recovery of polysaccharide.
Polysaccharide chemically can be divided into acidity, neutrality and alkaline polysaccharide, therefore if can be according to the chemical property of polysaccharide, corresponding employing Aqueous Solutions with Non-water Soluble Reagents of different nature and solvent, make polysaccharide of different nature obtain separation and Extraction by combining between organic reagent (extraction agent) and polysaccharide, just can overcome the deficiency of existing ethanol step-by-step precipitation method.
The objective of the invention is to: low in order to overcome present employing water-miscible organic solvent (mainly being ethanol) existing product yield of the precipitator method of extraction separation Sargassum polysaccharides from algae leaching liquor, the shortcoming that purity is not high, the extraction system (organic phase) that the present invention adopts water-insoluble reagent and organic solvent to form, effect by the polysaccharide in extraction agent and the algae leaching liquor, the polysaccharide extraction that originally is insoluble to organic solvent is entered organic phase, thereby separate with most of water-soluble impurity, the organic phase that contains polysaccharide is contacted with the aqueous solution that contains inorganic salt commonly used, polysaccharide promptly reenters salt brine solution and polysaccharide is further separated with non-water soluble impurity, make polysaccharide obtain separating and enrichment like this, organic phase after the back extraction is returned extraction again, recycle, reduce solvent consumption greatly, save cost; Thereby provide a kind of from algae leaching liquor the method for extraction separation polysaccharide.
The object of the present invention is achieved like this: the present invention uses water-insoluble reagent and solvent composition organic phase that Sargassum polysaccharides in the algae leaching liquor is extracted, make polysaccharide enter organic phase and separate with water-soluble impurity, collection is gone into the polysaccharide salt brine solution back extraction backwater phase of organic phase, thereby further separate and obtain enrichment with non-water soluble impurity, organic phase is returned extraction, and the polysaccharide in the salt brine solution can reclaim with well-established law.Thereby realize the extraction separation of Sargassum polysaccharides.The method of employing solvent extraction of the present invention extraction separation Sargassum polysaccharides from the aqueous leaching solution of marine alga comprises the steps:
(A) provide a kind of and comprise that water-insoluble reagent is quaternary ammonium salt (as extraction agent), its concentration is that 0.2%～30% (weight/volume) and surplus are the extraction system (organic phase) that organic solvent (as thinner) is formed;
(B) organic phase that step (A) is prepared and the aqueous leaching solution of marine alga, by being in a ratio of 1: 1-1: 50 batchings, the aqueous leaching solution of organic phase and marine alga is put into common extraction plant, carry out single extraction at least by common extraction process, extraction process is at room temperature operated, starting time 10-30 minute; Centrifugal phase-splitting;
(C) being extracted into the Sargassum polysaccharides of organic phase can be with the aqueous solution back extraction backwater that contains inorganic salt commonly used mutually and further obtain enrichment, be in a ratio of 1 by back extraction: 1-4: 1 batching, get organic phase and stripping workshop after the phase-splitting, its concentration is the aqueous solution that 0.5-4.0mol/L contains inorganic salt commonly used, in common extraction plant, carry out at least back extraction by common anti-extraction process, the back extraction process can at room temperature be operated, starting time 10-30 minute, carry out centrifugal phase-splitting.
Wherein water-insoluble reagent is arquad, can comprise the additive of 0～30% (volume/volume), and additive is weakly alkaline amine, comprises long-chain primary amine, secondary amine and tertiary amine, and their molecular weight is between 250-600.The adding of additive or help improving and be separated or help extraction and back extraction.
Wherein water-insoluble reagent quaternary ammonium salt is an extraction agent, and the quarternary ammonium salt compound structural formula is:
R
1R
2R
3CH
3N
+Z
-And R
1R
2(CH
3)
2N
+Z
-Wherein: R
1, R
2, R
3Be alkyl, its carbonatoms both can be identical also can be different, total carbon number is 16-36; Z
-For organizing salifiable negatively charged ion, can be Cl
-Or Br
-As home-made N263 (quaternary ammonium mixture that mainly contains chlorination trialkyl (C7-C9) ammonium methyl) and 7401 (quaternary ammonium mixtures that mainly contain chlorination trialkyl (C8-C10) ammonium methyl) and external Aliquat336 and Adogen464 etc.The extraction ability of these quaternary ammonium salts is very similar.
Wherein remainder is an organic solvent: as alcohol, ketone, ester, alkane and aromatic hydrocarbons organic solvent.
Wherein said organic solvent is the mixture that pentyl acetate, 2-Ethylhexyl Alcohol, methyl iso-butyl ketone (MIBK), kerosene, toluene, tetracol phenixin or above-mentioned solvent combine mutually, for example: kerosene and 2-Ethylhexyl Alcohol, pentyl acetate and 2-Ethylhexyl Alcohol, kerosene and toluene, kerosene and methyl iso-butyl ketone (MIBK), kerosene and pentyl acetate etc.
Effect of the present invention:
The present invention is subjected to the influence of salt concn in extractant concentration, the vat liquor etc. to the efficient that adopts solvent extraction extraction separation Sargassum polysaccharides from algae leaching liquor, and its advantage is as follows:
(1) percentage extraction of polysaccharide is subjected to the influence of vat liquor pH hardly, all can effectively extract in the scope that initial pH is 1-12, and this is just very favourable to the vat liquor extraction polysaccharide from different pH;
(2) influence compared hardly of the extraction efficiency of polysaccharide is 1 comparing (O/A): 1-1: all can implement effective extraction in 50 the scope, this just can make polysaccharide reach highly enriched by changing the extraction phase ratio;
(3) in the presence of the capacity extraction agent, the extraction of fucoidin is not subjected to Temperature Influence substantially, thereby to the adaptability broad of liquid temperature.
(4) method of the present invention and the precipitator method compare the separation degree height, and the percentage extraction height of polysaccharide from table 1-3 as can be seen, reaches as high as 99.8%; Resulting Sargassum polysaccharides product purity is also high.
(5) method of the present invention is with bigger than ion-exchange and absorption method treatment capacity, lack than distillation method power consumption, and what use in the method to extraction separation Sargassum polysaccharides from algae leaching liquor all is home-made extraction agents, has saved foreign exchange widely, reduce cost, improved economic benefit.
(6) but method of the present invention is easy to continuous operation and automatic production.
Now at length the present invention will be described in conjunction with the accompanying drawings and embodiments:
The relation of fucoidin percentage extraction and extractant concentration when accompanying drawing 4 is a different solvents (or solvent mixture) for thinner.Among the figure curve represent respectively different solvents or solvent mixture (-pentyl acetate, ●-CCl
4, o-2-ethylhexanol, -toluene, ◇-methyl iso-butyl ketone (MIBK), Δ-kerosene+2-Ethylhexyl Alcohol) and be thinner.Experiment condition is: initial water fucoidin concentration 1g/L, and temperature is 20 ℃, compare=1/5.
Embodiment 1: the extracting and enriching of fucoidin
Table 1 for different compare, extraction embodiment when different extractant concentration and different feed liquid fucoidin concentration.
Employing N263 is an extraction agent, pentyl acetate is the solvent composition organic phase, by comparing shown in the table 1, the aqueous solution of getting the organic phase of certain volume and containing polysaccharide is in Centrifuge Cup, at room temperature induction stirring is 10 minutes, and after the centrifugal phase-splitting, fucoidin concentration is measured in the Hengshui of making even mutually, calculate percentage extraction with this, extraction results is listed in table 1.As known from Table 1, compare down in difference, the fucoidin of different concns can reach the purpose that extracts fucoidin by changing the organic extractant phase agent concentration, and fucoidin obtains highly enriched in organic phase.
The extraction of table 1 fucoidin (extraction agent: N263, solvent: pentyl acetate)
| Feed liquid sugar concentration extractant concentration extraction phase is than the sugared concentration percentage extraction of organic phase, % | 0.1 0.2 1/5 0.487 97.6 | 0.097 0.2 1/5 0.484 99.3 | 1.01 2.0 1/5 4.92 97.8 | 1.02 2.0 1/5 5.13 ～100 | 1.04 2.0 1/5 5.17 99.8 | 1.11 4.0 1/10 10.70 96.4 | 1.03 4.0 1/10 10.27 ～100 | 1.08 4.0 1/10 10.55 97.8 | 1.01 4.0 1/10 10.07 99.5 | 0.98??9.8 10.0??30.0 1/25??1/3 23.85?29.25 97.1??99.5 |
Annotate: sugared concentration is g/L; Extractant concentration is (volume) %; Be in a ratio of volume ratio.
Embodiment 2: the example of the salt back extraction of fucoidin
Table 2 is gone into the embodiment of the fucoidin of organic phase with the salt brine solution back extraction for collection.
Employing N263 is an extraction agent, pentyl acetate is the solvent composition organic phase, the aqueous solution of getting the organic phase of certain volume and containing polysaccharide is in Centrifuge Cup, at room temperature induction stirring is 10 minutes, after the centrifugal phase-splitting, measure the fucoidin concentration of balance aqueous phase, calculate fucoidin concentration in the organic phase with this, get this load organic phase in centrifuge tube, compare with back extraction shown in the table 2, in test tube, add the aqueous solution that certain volume contains inorganic salt commonly used, hand mixing is about 1 minute under the room temperature, and centrifugal phase-splitting is got salt brine solution and analyzed wherein fucoidin concentration, calculate back extraction ratio with this, the results are shown in table 2.From table 2 listed data as can be known, the fucoidin that is extracted into organic phase can be with salt-containing solution back extraction backwater mutually and further obtain enrichment, but stripping efficiency increases with the concentration of fucoidin in the organic phase and reduces.
The back extraction of table 2 fucoidin
| Extraction agent organic phase concentration, % sugar concentration | The salt title | Salt concn mol/L | O/A is compared in back extraction | Strip liquor sugar concentration | Back extraction ratio % |
| ????2????4.87 ????2????4.84 ????2????4.92 ????2????4.87 ????2????5.13 | NaCl CaCl 2NaCl CaCl 2NaCl | ?1.5 ?0.75 ?2.0 ?1.0 ?2.0 | ?2/1 ?2/1 ?2/1 ?2/1 ?1/1 | ?9.42 ?8.69 ?9.48 ?9.03 ?5.03 | ????96.6 ????89.7 ????96.4 ????92.6 ????98.0 |
| ????4????10.70 ????4????10.27 ????4????10.55 ????4????10.07 ????4????10.55 | NaCl CaCl 2NaCl CaCl 2NaCl | ?1.5 ?0.75 ?2.0 ?1.0 ?4.0 | ?2/1 ?2/1 ?2/1 ?2/1 ?4/1 | ?13.89 ?15.12 ?16.68 ?14.63 ?33.48 | ????64.9 ????73.6 ????79.1 ????71.6 ????79.4 |
| ????10????23.85 | NaCl | ?4.0 | ?2/1 | ?33.61 ?6.40 | ????70.5 ????13.4 |
Wherein sugared concentration is g/L in the table.
Embodiment 3: extraction in the actual algae leaching liquor and back extraction
Table 3 is the extraction and the back extraction embodiment of fucoidin in the actual algae leaching liquor.
Adopting 7401 (or TOA) is extraction agent, join (or being unworthy of) with additive TOA, pentyl acetate is the solvent composition organic phase, with extraction phase shown in the table 3 than and proportioning, get the hot acid water extract of the organic phase of certain volume and mouse tail algae or sea-tangle or ultrasonic vat liquor in Centrifuge Cup, at room temperature induction stirring is 10 minutes, after the centrifugal phase-splitting, measure the Fucose concentration of balance aqueous phase, calculate percentage extraction with this, the Fucose concentration in the organic phase is calculated with minusing.Back extraction: get this load organic phase in centrifuge tube, compare with back extraction shown in the table 3, add the certain volume salt-containing solution in test tube, hand mixing is about 1 minute under the room temperature, and salt brine solution (1) is taken out in centrifugal phase-splitting; Repeat above step, get salt brine solution (2), analyze the Fucose concentration in salt brine solution (1), (2), calculate back extraction ratio with this.
The result of table 3 shows that weakly alkaline amine trioctylamine (TOA) is lower as the extracting power of extraction agent, but as additive, then helps extraction and back extraction, and other weakly alkaline amines are also similar with the effect of TOA.The result shows that also the extraction from ultrasonic vat liquor is better than the extraction from the hot acid water extract.
The extraction of fucoidin and back extraction embodiment in the actual algae leaching liquor of table 3.
| The feed liquid sequence number | Feed liquid sugar concentration g/l | Extraction agent (concentration, %) | Extraction phase compares O/A | Percentage extraction % | Organic phase sugar concentration g/l | NaCl concentration mol/L | O/A (number of times) is compared in back extraction | Strip liquor sugar concentration g/l | Back extraction ratio % |
| ????1 | ?0.514 | TOA(10) | 1/2.5 | ?40.9 | ?1.187 | ????2 | ????4/1(1) ????(2) | 1.046 0.117 | ?86.4 ?9.63 |
| ????2 | ?0.537 | 7401(1) | 1/5 | ?68.4 | ?1.837 | ????2 | ????2/1(1) ????(2) | 2.642 0.259 | ?71.9 ?7.05 |
| ????3 | ?0.486 | 7401(1)+TOA(4.5) | 1/5 | ?69.4 | ?1.684 | ????2 | ????2/1(1) ????(2) | 2.327 0.231 | ?72.6 ?6.85 |
| 7401(1)+TOA(9) | 1/5 | ?77.3 | ?1.878 | ???1.6 ????2 | ?1.6/1(1) ????2/1(2) | 2.260 0.303 | ?75.2 ?8.06 | ||
| ????4 | ?0.560 | 7401(2)+TOA(8) | 1/5 | ?79.4 | ?2.223 | ???1.7 ????2 | ?1.7/1(1) ????2/1(2) | 2.204 0.575 | ?59.5 ?12.9 |
| ????5 | ?0.693 | 7401(3)+TOA(7) | 1/5 | ?96.3 | ?3.336 | ????2 | ????2/1(1) ????(2) | 5.318 0.523 | ?79.7 ?7.84 |
| ????6 | ?0.570 | 7401(3) 7401(3)+TOA(7) | 1/5 | ?97.0 ?97.2 | ?2.763 ?2.768 | ????2 ????2 | ????2/1(1) ????(2) ????2/1(1) ????(2) | 3.914 0.467 4.483 0.366 | ?70.8 ?8.45 ?81.0 ?6.62 |
| ????7 | ?0.585 | 7401(6)+TOA(4) | 1/10 | ?95.7 | ?5.595 | ????2 | ????1/1(1) ????(2) | 4.240 0.217 | ?75.8 ?3.88 |
| ????8 | ?0.657 | 7401(3)+TOA(7) | 1/5 | ?97.4 | ?3.200 | ????2 | ????2/1(1) ????(2) | 3.981 0.872 | ?62.2 ?14.3 |
| ?9 | ?0.567 | 7401(1.5)+ TOA(8.5) | 1/2.5 | ?98.5 | ?1.401 | ????2 | ????1/4(1) ????(2) | 4.015 0.907 | ?71.7 ?16.2 |
| ?10 | ?0.603 | 7401(3)+TOA(7) | 1/5 | ?97.5 | ?2.945 | ????2 | ????1/1(1) ????(2) | 2.409 0.0902 | ?81.8 ?3.06 |
Wherein example 1～3 is a mouse tail algae hot acid water extract; Example 4 is a sea-tangle hot acid water extract; Example 5～10 is the ultrasonic vat liquor of sea-tangle.
Embodiment 4: the comparison of ethanol precipitation and extraction process purity of polysaccharide from mouse tail algae vat liquor
Get mouse tail algae vat liquor 200ml, heating is concentrated into 50ml, add dehydrated alcohol to 30% (volume/volume) under stirring, discard precipitation after centrifugal, continue to add dehydrated alcohol to 60% (volume) in the supernatant liquor, mixture is put refrigerator overnight, gets precipitation after centrifugal, through washing, the dry Crude polysaccharides that gets, containing Fucose by analysis is 19.3%.
Other gets mouse tail algae vat liquor 200ml, and containing 7401 with 40ml is the pentyl acetate solution extraction of 5% (weight/volume), organic phase 2mol/L CaCl
2The solution back extraction adds dehydrated alcohol to 60% (volume/volume) in the strip liquor, mixture is put refrigerator overnight, and centrifuging and taking precipitation (1) continues to add ethanol to 80% in the supernatant liquor, places after 3 hours centrifuging and taking precipitation (2).Precipitation (1) and (2) obtains the solid polysaccharide through washing, drying, and by analysis, containing Fucose respectively is 20.4% and 43.1%.As seen, extraction process gained purity of polysaccharide will be higher than the purity of ethanol step-by-step precipitation method.
Embodiment 5: the comparison of ethanol step-by-step precipitation method and extraction process polysaccharide yield and purity from the sea-tangle vat liquor
Get sea-tangle vat liquor 400ml, heating is concentrated into 130ml, cooling back adds dehydrated alcohol to 30% (volume/volume) under stirring, and discards precipitation after centrifugal, continues to add dehydrated alcohol to 60% (volume/volume) in the supernatant liquor, mixture is put refrigerator overnight, get precipitation after centrifugal, through washing, the dry Crude polysaccharides 0.5157g that gets, containing Fucose by analysis is 33.7%, in Fucose, output is 0.1738g.
Other gets identical sea-tangle vat liquor 400ml, and containing 7401 with 80ml is the pentyl acetate solution extraction of 3% (weight/volume), organic phase 2mol/L CaCl
2Add 1 times of volume dehydrated alcohol in the solution back extraction 2 times, strip liquor (1), put refrigerator overnight, centrifuging and taking precipitation (1) continues in the supernatant liquor to add 3 times of volumes (with the strip liquor volumeter) dehydrated alcohol, places after 2 hours centrifuging and taking precipitation (2).Strip liquor (2) heating is concentrated into half volume approximately, and the cooling back adds 4 times of volume dehydrated alcohols, puts refrigerator overnight, centrifuging and taking precipitation (3).Precipitation (1), (2) and (3) obtain the solid polysaccharide and are respectively 0.3367g, 0.0592g and 0.0983g through washing, drying.By analysis, kukersite algae sugar is respectively 45.0,27.2% and 38.4%, and in Fucose, output is 0.2053g.As seen, in Fucose, output of extraction process (0.2053g) and purity of polysaccharide (average content is 41.5%) all will be higher than the output (0.1738g) and the purity of polysaccharide (33.7%) of ethanol step-by-step precipitation method.
Claims (7)
1. a method that adopts solvent extraction separation and Extraction Sargassum polysaccharides from algae leaching liquor comprises the steps:
(A) provide a kind of and comprise that water-insoluble reagent is arquad, its concentration is that 0.2%～30% (weight/volume) and surplus are the organic phase that organic solvent is formed;
(B) organic phase that step (A) is prepared and the aqueous leaching solution of marine alga, by being in a ratio of 1: 1-1: 50 batchings, the aqueous leaching solution of organic phase and marine alga is put into common extraction plant, carry out single extraction at least by common extraction process, extraction process is at room temperature operated, starting time 10-30 minute; Centrifugal phase-splitting;
(C) being extracted into the Sargassum polysaccharides of organic phase can be with salt-containing solution back extraction backwater mutually and further obtain enrichment, be in a ratio of 1 by back extraction: 1-4: 1 batching, get organic phase and stripping workshop after the phase-splitting, its concentration is the aqueous solution of the salt of 0.5-4.0mol/L, in common extraction plant, carry out at least back extraction by common anti-extraction process, the back extraction process can at room temperature be operated, starting time 10-30 minute, carry out centrifugal phase-splitting.
2. by the method for the described employing solvent extraction of claim 1 separation and Extraction Sargassum polysaccharides from algae leaching liquor, it is characterized in that: described water-insoluble reagent quarternary ammonium salt compound structural formula is: R
1R
2R
3CH
3N
+Z
-And R
1R
2(CH
3)
2N
+Z
-
Wherein: R
1, R
2, R
3Be alkyl, its carbonatoms is identical or different, and total carbon number is 16-36; Z
-For organizing salifiable negatively charged ion, can be Cl
-Or Br
-
3. by the method for the described employing solvent extraction of claim 1 separation and Extraction Sargassum polysaccharides from algae leaching liquor, it is characterized in that: also comprise the additive that adds 0～30% (volume/volume) in the described water-insoluble reagent.
4. press the method for the described employing solvent extraction of claim 1 separation and Extraction Sargassum polysaccharides from algae leaching liquor, it is characterized in that: the additive that adds in the described water-insoluble reagent is weakly alkaline amine, comprise long-chain primary amine, secondary amine and tertiary amine, its molecular weight is between 250-600.
5. by the method for the described employing solvent extraction of claim 1 separation and Extraction Sargassum polysaccharides from algae leaching liquor, it is characterized in that: described organic solvent comprises the mixture that combines of alcohol, ketone, ester, alkane, alkyl chloride hydro carbons and aromatic hydrocarbons or described solvent.
6. by the method for the described employing solvent extraction of claim 5 separation and Extraction Sargassum polysaccharides from algae leaching liquor, it is characterized in that: described alcohol organic solvent is a 2-Ethylhexyl Alcohol; Described ester class organic solvent is a pentyl acetate; Described alkanes organic solvent is toluene, kerosene; Described alkyl chloride hydro carbons organic solvent is a tetracol phenixin; Described organic solvent of ketone is a methyl iso-butyl ketone (MIBK).
7. by the method for the described employing solvent extraction of claim 1 separation and Extraction Sargassum polysaccharides from algae leaching liquor, it is characterized in that: described water-insoluble reagent quaternary ammonium salt concentration is 1%-10% (weight/volume).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100429236C (en) * | 2006-11-03 | 2008-10-29 | 浙江大学 | Method of extracting soluble polysaccharide in bitter vegetable |
| CN101168570B (en) * | 2007-11-15 | 2010-05-26 | 暨南大学 | Method for degrading kelp polysaccharide sulfate |
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2000
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100429236C (en) * | 2006-11-03 | 2008-10-29 | 浙江大学 | Method of extracting soluble polysaccharide in bitter vegetable |
| CN101168570B (en) * | 2007-11-15 | 2010-05-26 | 暨南大学 | Method for degrading kelp polysaccharide sulfate |
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