CN102430265B - Aqueous two-phase extraction system of mixed surfactant - Google Patents
Aqueous two-phase extraction system of mixed surfactant Download PDFInfo
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- CN102430265B CN102430265B CN201110287840.7A CN201110287840A CN102430265B CN 102430265 B CN102430265 B CN 102430265B CN 201110287840 A CN201110287840 A CN 201110287840A CN 102430265 B CN102430265 B CN 102430265B
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Abstract
The invention provides an aqueous two-phase extraction system formed by anion/cation mixed surfactant which is induced by fluoroalcohol, a preparation method and an application thereof. The aqueous two-phase extraction system comprises anion surfactant sodium dodecyl sulfate, cation surfactant hexadecyl trimethyl ammonium bromide, hexafluoroisopropanol and water. The extraction system has short phase forming time, wide phase forming range, gentle and simple phase forming condition, low consumption and high efficiency, so the extraction system is a novel extraction system. The invention can extract and separate different types of compounds through the phase forming conditions of the system, so the application prospect is good.
Description
Technical field
The invention belongs to separation technology field, relate to a kind of mixed surfactant two phase aqueous extraction system of fluorinated alcohols induction.
Background technology
The aqueous two phase extraction technique growing up based on double-aqueous phase system is a kind of easy and simple to handle, eco-friendly liquid-liquid technique.This abstraction technique is proposed and is applied to extract and separate cell and cell fragment for 1956 first by Albertsson.Up to now, the research of aqueous two phase extraction technique and application have obtained very great development.
In this abstraction technique, when after double-aqueous phase system generation phase-splitting, the microstructure of phase is different up and down, thereby and extract between motive power (as hydrophobic, hydrogen bond, electrostatic force etc.) also can be different.The comprehensive function of these active forces selectively distributes extract in two-phase, separates and enrichment thereby realize.
Compared to other abstraction techniques, aqueous two phase extraction technique has many advantages, as: there is no mixing of a large amount of organic solvents, have good biocompatibility, mild condition, easily amplifies and continuous operation.At present, aqueous two-phase extraction has all obtained studying very widely and applying at the aspect such as separation detection, the extract and separate of Chinese medicine natural products of separation and purification, metal or the metal complex of bioactive ingredients.But, traditional aqueous two-phase (polymer aqueous two-phase) abstraction technique also exists some shortcomings part, as higher in polymer cost, easy emulsification etc., therefore, explores and finds one of main development direction that various novel double-aqueous phase systems are aqueous two phase extraction technique in recent years.
Aqueous two phase extraction technique based on anion/cation mixed surfactant has overcome the deficiency that traditional aqueous two phase extraction technique exists.The more important thing is, this abstraction technique also has two distinguishing features: the aggregation that (1) anion/cation mixed surfactant forms can provide hydrophobic and hydrophilic environment simultaneously, and therefore this technology can be come enrichment hydrophily or hydrophobic compound by different active forces; (2) by the proportioning of cationic and anionic surfactant in regulation system, can control the phase volume ratio of the electrically charged and aqueous two-phase of aggregate surface institute, thereby can significantly improve separation selectively and bioaccumulation efficiency.But, anion/cation mixed surfactant system form aqueous two-phase needed condition but very harsh, aqueous two-phase region is very narrow, be greatly limited in application aspect, in recent ten years, its correlative study work mainly concentrates on the aspect such as phase behavior, character, composition, micro-structural of condition, method, mechanism and aqueous two-phase that aqueous two-phase forms.Accelerate the formation of aqueous two-phase, widen aqueous two-phase region although worked out certain methods, as heated up, change change pH values, adding inorganic salts or organic molecule etc., the effect of these methods is all very limited.Especially for the equimolar ratio anion/cation surfactant hybrid system that very easily produces precipitation, the formation of aqueous two-phase is more difficult.Therefore, make anion/cation mixed surfactant aqueous two phase extraction technique be studied widely and apply, exploration and exploitation applicability are stronger, the better double-aqueous phase system of validity is very necessary.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provide a kind of become fast, the wide mixed surfactant two phase aqueous extraction system of aqueous two-phase region field width of phase velocity, and provide the application of this two phase aqueous extraction system aspect the extraction of various heterogeneity compound.
The anion surfactant using in the anion/cation mixed surfactant two phase aqueous extraction system of fluorinated alcohols induction provided by the invention is lauryl sodium sulfate (SDS), the cationic surfactant using is softex kw (CTAB), and the fluorinated alcohols of use is hexafluoroisopropanol (HFIP).
Mixed surfactant two phase aqueous extraction system provided by the invention is made up of anionic, cationic surfactant softex kw, hexafluoroisopropanol and water;
And the mol ratio of two kinds of surfactants is 1:1, surfactant total concentration is 25 ~ 200 mmol/L, and the addition of hexafluoroisopropanol is 10% ~ 40%(v/v of cationic and anionic surfactant and water cumulative volume);
Or the addition of hexafluoroisopropanol is the 10%(v/v of cationic and anionic surfactant and water cumulative volume), surfactant total concentration≤200 mmol/L, the molar ratio of lauryl sodium sulfate and softex kw is 86:14 ~ 1:99.
Aqueous two-phase forms with the addition of hexafluoroisopropanol, the relation of surfactant total concentration:
In the time that the mol ratio of two kinds of surfactants in this system is 1:1, the addition that is 25 ~ 200 mmol/L, hexafluoroisopropanol in surfactant total concentration is 10% ~ 40%(v/v of cationic and anionic surfactant and water cumulative volume) scope in can form aqueous two-phase.And surfactant total concentration is less, hexafluoroisopropanol addition is when fewer, and the volume of lower floor's condensed phase is less.As shown in Figure 1.
Ternary phase diagrams Fig. 2 of double-aqueous phase system provided by the present invention, is according to lever rule, leg-of-mutton three summits is decided to be respectively to the pure water solution (HFIP:H of hexafluoroisopropanol
2o=10:100, v/v), the sodium dodecyl sulfate solution of 200 mmol/L and the softex kw solution of 200 mmol/L draws.In ternary phase diagrams, get a little, configure the sample of different proportionings, different total concentrations, all samples is after centrifugal 30 min of 2000 rpm, and room temperature leaves standstill 24 h, observe phenomena, drawing diagram.The sample of same phenomenon is positioned at the same area, and phase region border is intensive joining a little around, the parallel repetition of each sample point 3 times.In this system gained ternary phase diagrams, the region that forms aqueous two-phase is very broad, when the addition of hexafluoroisopropanol is the 10%(v/v of cationic and anionic surfactant and water cumulative volume) time, in the scope that the molar ratio that is≤200 mmol/L, lauryl sodium sulfate and softex kw in surfactant total concentration is 86:14 ~ 1:99, can form aqueous two-phase.And surfactant total concentration more hour, and the volume of lower floor's condensed phase is less.
Step when the anion/cation mixed surfactant two phase aqueous extraction system of fluorinated alcohols induction provided by the present invention is applied to the extraction of variety classes compound is:
1, two kinds of surfactant solutions are mixed;
2, add hexafluoroisopropanol and be extracted the solution of compound;
3, mix, with centrifugal 30 min of rotating speed of 2000 rpm, room temperature leaves standstill.Be extracted in the condensed phase that compound is enriched to lower floor.
The compound that is extracted in above-mentioned steps comprises neutral compound, electronegative compound and amphoteric compound.
The concentration of surfactant and ratio in above-mentioned steps, be extracted the pH value of compound solution, and the addition of hexafluoroisopropanol all can be adjusted, to realize the selectivity efficient enrichment to variety classes compound.
This extraction system leaves standstill in the temperature range of 4 ~ 45 degrees Celsius, and the enrichment times and the extraction yield that are extracted compound are all unaffected.
The beneficial effect of the anion/cation mixed surfactant two phase aqueous extraction system of fluorinated alcohols induction provided by the present invention is embodied in:
1, this system becomes phase mild condition, simple, and compared with other anion/cation Aqueous Surfactant Two system, this system becomes without long-time heating, gets final product rapid phase-splitting (in 15 seconds) under room temperature, and becomes phase effect good.
2, this system becomes phase wide ranges.In the time that the mol ratio of two kinds of surfactants is 1:1, the addition that is 25 ~ 200 mmol/L, hexafluoroisopropanol in surfactant total concentration is 10% ~ 40%(v/v) scope in can form aqueous two-phase; When the addition of hexafluoroisopropanol is 10%(v/v) time, in the scope that the molar ratio that is≤200 mmol/L, lauryl sodium sulfate and softex kw in surfactant total concentration is 86:14 ~ 1:99, can form aqueous two-phase.
3, this system phase behavior is stable, and after phase-splitting, a month two-phase of room temperature placement still can keep stable, and aqueous two-phase region changes very little.
4, this system adopts raw material is simple and easy to get, cost is low, and phase process is easy, be easy to control.
5, this system can realize the selective extraction to variety classes compound by changing over phase condition, can be for neutral compound, electronegative compound, amphoteric compound in complex sample are carried out to preenrichment, and show the feature that extraction efficiency is high, enrichment times is large, separating rate is fast.The extraction yield (up to 94.4%) of this system to both sexes micromolecular compound tryptophan be the extraction yield (50%) to tryptophan apparently higher than other anion/cation Aqueous Surfactant Two system.
accompanying drawing explanation:
Fig. 1 is hexafluoroisopropanol (HFIP) addition and the impact (binary phase diagraml) of surfactant total concentration to SDS/CTAB (1:1, mol/mol) mixed system phase behavior, and S representative only exists single-phase; B representative forms aqueous two-phase (two-phase is all transparent); CW represents that solution becomes muddy, time adularescent solid exist; CWB representative forms two-phase, but two-phase is all muddy; WB representative forms two-phase, but wherein one has mutually white solid.
Fig. 2 is the ternary phase diagrams of the SDS/CTAB mixed system of HFIP induction, wherein, HFIP addition is 10% (v/v), surfactant total concentration is≤200 mmol/L, black region represents the region that aqueous two-phase forms, (A) be fresh preparation, (B) for placing 1 month.
The specific embodiment
Below embodiments of the invention are elaborated: the present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
Under room temperature, get the sodium dodecyl sulfate solution that concentration is 100 mmol/L and mix (2.5 mL SDS with softex kw solution etc. mole, 2.5 mL CTAB), add mixed system cumulative volume 10%(v/v) hexafluoroisopropanol (0.5 mL), mix, with the rotating speed of 2000 rpm, centrifugal and room temperature obtains after leaving standstill that interface is clear, the double-aqueous phase system of the equal clear of two-phase.The material composition that detects two-phase, its material percentage is as shown in table 1, and upper strata viscosity is less, water content is very large, and lower floor's viscosity is large, the content of surfactant and hexafluoroisopropanol is all very large.
table 1material composition and the content thereof of SDS/CTAB (1:1, the mol/mol) double-aqueous phase system of HFIP induction
Embodiment 2:
Under room temperature, getting the sodium dodecyl sulfate solution that concentration is 200 mmol/L mixes by 86:14 molar ratio with softex kw solution, add mixed system cumulative volume 10%(v/v) hexafluoroisopropanol, mix, after centrifugal and room temperature leaves standstill with the rotating speed of 2000 rpm, obtain that interface is clear, the double-aqueous phase system of the equal clear of two-phase.
Embodiment 3:
Under room temperature, getting the sodium dodecyl sulfate solution that concentration is 200 mmol/L mixes by 85:15 molar ratio with softex kw solution, add mixed system cumulative volume 10%(v/v) hexafluoroisopropanol, mix, after centrifugal and room temperature leaves standstill with the rotating speed of 2000 rpm, obtain that interface is clear, the double-aqueous phase system of the equal clear of two-phase.
Embodiment 4:
Under room temperature, getting the sodium dodecyl sulfate solution that concentration is 200 mmol/L mixes by 2:98 molar ratio with softex kw solution, add mixed system cumulative volume 10%(v/v) hexafluoroisopropanol, mix, after centrifugal and room temperature leaves standstill with the rotating speed of 2000 rpm, obtain that interface is clear, the double-aqueous phase system of the equal clear of two-phase.
Embodiment 5:
Under room temperature, getting the sodium dodecyl sulfate solution that concentration is 200 mmol/L mixes by 1:99 molar ratio with softex kw solution, add mixed system cumulative volume 10%(v/v) hexafluoroisopropanol, mix, after centrifugal and room temperature leaves standstill with the rotating speed of 2000 rpm, obtain that interface is clear, the double-aqueous phase system of the equal clear of two-phase.
Embodiment 6:
Under room temperature, getting certain density sodium dodecyl sulfate solution mixes by certain mol proportion example with softex kw solution, add cortisol methanol solution 0.02 mL of a certain amount of hexafluoroisopropanol and 1 mg/mL, mix, obtain after centrifugal and standing with the rotating speed of 2000 rpm that interface is clear, the double-aqueous phase system of the equal clear of two-phase.After phase-splitting, neutral compound cortisol is enriched in lower floor's condensed phase, and the phase volume ratio under 15 kinds of different extraction conditions and enrichment times, the extraction yield of cortisol are as shown in table 2.
table 2the extraction results of the SDS/CTAB double-aqueous phase system of HFIP induction to cortisol under different extraction conditions
Embodiment 7:
Under room temperature, getting certain density sodium dodecyl sulfate solution mixes by certain mol proportion example with softex kw solution, add mixed system cumulative volume 10%(v/v) hexafluoroisopropanol and the Sodium Benzoate aqueous solution 0.02 mL of 1 mg/mL, mix, with the rotating speed of 2000 rpm, centrifugal and room temperature obtains after leaving standstill that interface is clear, the double-aqueous phase system of the equal clear of two-phase.After phase-splitting, electronegative compound Sodium Benzoate is enriched in lower floor's condensed phase, and the phase volume ratio under 10 kinds of different extraction conditions and enrichment times, the extraction yield of Sodium Benzoate are as shown in table 3.
table 3the extraction results of the SDS/CTAB double-aqueous phase system para Toluic Acid sodium of HFIP induction under different extraction conditions
Embodiment 8:
Under room temperature, getting the sodium dodecyl sulfate solution that concentration is 100 mmol/L mixes by certain mol proportion example with softex kw solution, add mixed system cumulative volume 10%(v/v) hexafluoroisopropanol and the tryptophan aqueous solution 0.6 mL of the different pH values of 2 mg/mL, mix, with the rotating speed of 2000 rpm, centrifugal and room temperature obtains after leaving standstill that interface is clear, the double-aqueous phase system of the equal clear of two-phase.Enrichment times, the extraction yield of the phase volume ratio under 15 kinds of different extraction conditions and both sexes micromolecular compound tryptophan are as shown in table 4.
table 4the extraction results of the SDS/CTAB double-aqueous phase system of HFIP induction to tryptophan under different extraction conditions
Claims (3)
1. a mixed surfactant two phase aqueous extraction system, is characterized in that: be made up of anionic, cationic surfactant softex kw, hexafluoroisopropanol and water;
And the mol ratio of two kinds of surfactants is 1:1, surfactant total concentration is 25 ~ 200 mmol/L, and the addition of hexafluoroisopropanol is 10% ~ 40% of cationic and anionic surfactant and water cumulative volume;
Or the addition of hexafluoroisopropanol is 10% of cationic and anionic surfactant and water cumulative volume, surfactant total concentration≤200 mmol/L, the molar ratio of lauryl sodium sulfate and softex kw is 86:14 ~ 1:99.
2. the application of two phase aqueous extraction system claimed in claim 1 in the extract and separate of neutral compound, electronegative compound, amphoteric compound.
3. application according to claim 2, is characterized in that: described neutral compound is cortisol; Described electronegative compound is Sodium Benzoate; Described amphoteric compound is tryptophan.
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| CN106749340B (en) * | 2016-11-25 | 2018-11-02 | 陕西师范大学 | A kind of method of surfactant collaboration aqueous two-phase extraction nimbin |
| CN107789861B (en) * | 2017-10-23 | 2019-11-08 | 武汉大学 | A kind of small molecule fluorine alcohol-salt double-aqueous phase system and its extracting process |
| CN107875671B (en) * | 2017-10-31 | 2020-02-14 | 武汉大学 | Salt-free mixed surfactant supramolecular solvent extraction system |
| CN108191657B (en) * | 2017-12-27 | 2020-09-22 | 武汉大学 | Method for extracting and separating chlorogenic acid from ramie leaves |
| CN113564357A (en) * | 2021-07-29 | 2021-10-29 | 南昌航空大学 | Composite medicament for hydrometallurgy and preparation method and application thereof |
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