CN109126737A - A kind of solid phase extraction material - Google Patents
A kind of solid phase extraction material Download PDFInfo
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- CN109126737A CN109126737A CN201810659251.9A CN201810659251A CN109126737A CN 109126737 A CN109126737 A CN 109126737A CN 201810659251 A CN201810659251 A CN 201810659251A CN 109126737 A CN109126737 A CN 109126737A
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- solid phase
- phase extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/50—Aspects relating to the use of sorbent or filter aid materials
- B01J2220/54—Sorbents specially adapted for analytical or investigative chromatography
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Abstract
The present invention relates to a kind of solid phase extraction material, especially solid phase microextraction material, the material is it is characterized in that core-shell structure, stratum nucleare are polarity solid phase extraction material, and shell is dimethyl silicone polymer coating, and shell thickness is at 1 nanometer~10 microns.For low pole, nonpolar small organic molecule, such as phenols, nitrobenzene, polycyclic aromatic hydrocarbon, organic phosphorus, organochlorine compound, extraction efficiency caused by shell declines, and is not more than 30%.For highly polar small molecule compound, adsorbance can be reduced, wherein absorption of the water in stratum nucleare polarity solid phase extraction material can reduce 80% or more.Material preparation method of the present invention is simple, and low pole, nonpolar small molecule extraction efficiency remain unchanged substantially, while the absorption residual of water is greatly lowered, and extends the service life of solid phase extraction material, improves the efficiency of subsequent chromatographic isolation and Mass Spectrometer Method.
Description
Technical field
The invention belongs to solid phase extraction material fields, especially solid phase microextraction material.
Background technique
Solid Phase Extraction is a kind of separation process based on chemical distribution/adsorption mechanism, in particular in liquid/extraction material
On material, gas/fiber material interface, the compound in fluid can be in fiber material adsorption, or is extracted material sheet
Body absorbs, to realize enrichment, separation, the purification to specific compound in fluid.Solid Phase Extraction is in chemical separating, chemical analysis
Especially sample pre-treatments field is widely used.
Solid phase microextraction is a kind of solid phase extraction techniques of micromation, and basic principle is identical with Solid Phase Extraction, is mainly used for
The extracting and enriching of compound in aqueous sample.For volatile organic matter (VOCs), semi-volatile organic matter (SVOCs), Gu
Phase extraction can be combined with Thermal desorption, gas-chromatography: after solid phase microextraction, solid phase microextraction material being directly placed into heat
In resolver, high temperature directly is desorbed out the VOCs of extraction or SVOCs enters chromatography, completes subsequent separation analysis.Gu
Phase extraction-Thermal desorption-gas-chromatography combination concentrates on extracting and enriching, desorption parsing, separation detection one step and completes, improves
Analysis throughput.And organic solvent is not used, it is environmentally protective.
Fiber material is the core of solid phase micro-extraction method.Analysis of compounds is first adsorbed from sample solution, is enriched to extraction
On drawing materials, then by thermal desorption or organic solvent elution, enter subsequent analysis instrument.Generally selected with rule of similarity
Fiber material, i.e. fiber material should be matched with analyte property.Currently, for low pole hydrophobic compound, polydimethylsiloxanes
Alkane (PDMS) be property preferably, using most common fiber material, it is polyacrylate (PA), poly- for polar organic compound
Ethylene glycol (PEG, Carbowax, CW) is relatively common commercialization extraction phase material.In addition, extracted for polar organic matter,
The preferable fiber material of scientific research report has polyimides (PI), polyethersulfone ketone (PPESK).
Adsorbance of the water on polar extraction material PA, PEG, PI, PPESK is bigger, and general saturated extent of adsorption is 10%
Left and right.If the quality of micro-extraction phase material is 1 milligram, in extraction process, the water of absorption has 0.1 milligram, and organic matter
Adsorbance there was only nanogram rank.
The water adsorbed in solid phase microextraction can reduce subsequent separation detection efficiency, or even damage instrument and equipment.It is being pyrolyzed
During analysis-is chromatograph joint used, the high temperature moment of Thermal desorption makes the water of absorption be gasified totally, and may cause the broken of extraction phase material
It splits, falls off；After steam enters gas-chromatography, it may cause swelling, the failure of chromatographic stationary phases, reduce chromatographic isolation efficiency；Water
After vapour enters flame ionization ditector (FID), it is flame-out to will lead to FID；It is examined into electron capture detector (ECD), thermal conductivity
After surveying device (TCD), it can greatly shorten the service life of ECD, TCD detector；Into after mass detector (MS), electronics hair may cause
Shot-light silk (EI's) burns.
Currently, it is seldom to adsorb remaining correlative study on polar extraction material for water, to inhibiting water absorption remaining
The report of fiber material is less.
Summary of the invention
The present invention relates to a kind of solid phase extraction materials, especially solid phase microextraction material.Solid Phase Extraction material of the present invention
Material is core-shell structure, and the stratum nucleare is polarity solid phase extraction material, and shell is dimethyl silicone polymer.
Another aspect of the present invention provides the preparation method of the solid phase extraction material, includes the following steps:
(1) stratum nucleare, including stratum nucleare film and stratum nucleare particle are prepared:
1a. prepares stratum nucleare film: solid phase extraction material is prepared as 0.1%~30% polymer solution；With infusion process
(dip-coating), spray coating method (spray-coating) or spin-coating method (spin-coating) are formed in support carrier surface
0.01 micron~1 millimeter of stratum nucleare film；And curing and drying；
1b. prepares stratum nucleare particle: solid phase extraction material is prepared as 0.1%~50% polymer solution, to be spray-dried,
Emulsification, the method being mechanically pulverized prepare 0.1 micron~1 mm granules, and curing and drying；
(2) preparation of shell: dimethyl silicone polymer and crosslinking agent 1:2~50 in mass ratio is miscible, then use hydro carbons
Solvent is diluted to 0.1~50% according to volume ratio；The stratum nucleare film or stratum nucleare particle of soaking step (1) preparation；It then takes out solid
Change drying.
The solid phase extraction material of the invention of the method preparation is for low pole, nonpolar small organic molecule
(logP >=0), such as phenols, nitrobenzene, polycyclic aromatic hydrocarbon, organic phosphorus, organochlorine compound, under extraction efficiency caused by shell
Drop is not more than 30%.For highly polar small molecule compound (logP < 0), adsorbance can be reduced, wherein water is in stratum nucleare polarity
Absorption in solid phase extraction material can reduce 80% or more.Material preparation method of the present invention is simple, low pole, small point nonpolar
Sub- extraction efficiency remains unchanged substantially, while the absorption residual of water is greatly lowered, and extends the service life of solid phase extraction material,
Improve the efficiency of subsequent chromatographic isolation and Mass Spectrometer Method.
Based on this, the present invention further provides application of the material in Solid Phase Extraction or solid phase microextraction.
Characteristically, the solid phase extraction material can be with the hydrophobic organic micromolecule compound of extracting and enriching (logP >=0)；
It can also inhibit the absorption of polar hydrophilic small molecule compound (logP < 0), particularly water.
In the described application, the step of may also include the recycling after the completion of extraction to the solid phase extraction material.
Specific mode, including organic solvent parsing, high-temperature heating parsing are used, the compound of extraction is desorbed, for subsequent
Analysis.
Detailed description of the invention
Attached drawing 1 is that the spectrogram of combination gas chromatographic detection is desorbed through Thermal desorption in the test of organic phenol extraction test, in which:
(A) be PI extraction stirring rod test result；(B) be PDMS/PI extraction stirring rod test result.
Attached drawing 2 is that the spectrum of combination gas chromatographic detection is desorbed through Thermal desorption in the test of nitrobenzene compounds extraction test
Figure, in which: (A) is the test result of PI extraction stirring rod；(B) be PDMS/PI extraction stirring rod test result.
Specific embodiment
The present invention provides a kind of solid phase extraction material, and the material is core-shell structure, and the stratum nucleare is polarity solid phase extraction
It draws materials, shell is dimethyl silicone polymer.In the present specification, the solid phase extraction material with core-shell structure is not constrained in tool
The shape of body can be graininess or film-like material.In the material of any form, the dimethyl silicone polymer shell
With a thickness of 1 nanometer~10 microns.
In specific embodiment, the polarity solid phase extraction material is selected from polyimides (PI), polybenzimidazoles
(PBI), polyethersulfone ketone (PPESK), polyethylene glycol (PEG), polyacrylate (PAA), poly- divinylbenzene (PDVB), graphitized charcoal
Black (GCB), carbon molecular sieve and its derivative or composition.It is preferably selected from polyimides, polyethersulfone ketone, polybenzimidazoles, poly- second
Two pure and mild polyacrylate.
Further, the present invention provides the preparation method of above-mentioned solid phase fiber material, and the method includes stratum nucleare preparation and shells
The step of layer preparation.
In specific embodiment, the preparation of stratum nucleare selection method according to specific needs, come prepare film-form stratum nucleare or
Graininess stratum nucleare:
1a. prepares stratum nucleare film: solid phase extraction material is prepared as 0.1%~30% polymer solution；With infusion process
(dip-coating), spray coating method (spray-coating) or spin-coating method (spin-coating) are formed in support carrier surface
0.01 micron~1 millimeter of stratum nucleare film；And curing and drying；Wherein the solvent of the polymer solution be selected from dimethyl sulfoxide,
Diethyl sulfoxide, N-methyl pyrrolidones and its mixed system；
1b. prepares stratum nucleare particle: solid phase extraction material is prepared as 0.1%~50% polymer solution, to be spray-dried,
Emulsification, the method being mechanically pulverized prepare 0.1 micron~1 mm granules, and curing and drying；The wherein solvent of the polymer solution
Selected from dimethyl sulfoxide, diethyl sulfoxide, N-methyl pyrrolidones and its mixed system.
In some specific embodiments, stratum nucleare granular materials can be obtained by directly buying commercial goods, can also
For the present invention.It can illustrate herein but be not limited to poly- divinylbenzene (PDVB), Graphon (GCB), carbon molecular sieve particles.
On the basis of prepared stratum nucleare, further prepare shell coating, shell the preparation method comprises the following steps: by polydimethylsiloxanes
Alkane and crosslinking agent 1:2~50 in mass ratio are miscible, are then diluted to 0.1~50% according to volume ratio with hydrocarbon solvent；Impregnate step
Suddenly the stratum nucleare film or stratum nucleare particle of (1) preparation；Then take out solidification drying.In specific embodiment, the crosslinking agent is
The Sylgard 184 of DOW CORNING.The hydrocarbon solvent is selected from or mixtures thereof n-hexane, hexamethylene, pentane, benzene, toluene.
The present invention will be further described in a manner of specific embodiment below, but is not construed as appointing of the invention
The restriction of meaning form.
Embodiment 1
It prepares PPESK and extracts stirring rod
20%PPESK (Dalian polymer new material company) is substantially dissolved in dimethylacetamide solvent, by quartz pushrod
(long 40mm, diameter 2.5mm) is cleaned with ethyl alcohol, water respectively, and is dried at 100 DEG C.Czochralski method prepares PPESK fiber material: will
Quartz pushrod is inserted into PPESK solution, at the uniform velocity lifts, is then directly immersed in pure water, carries out inversion of phases.It is taken out after 24 hours, it is empty
It is dried in gas.Under 20mL/min nitrogen purging, high temperature ageing PPESK fiber material: 40 DEG C of maintenance 30min, 5 DEG C/min are raised to
100 DEG C of maintenance 30min, 5 DEG C/min are raised to 200 DEG C of maintenance 30min, 5 DEG C/min and are raised to 280 DEG C of maintenance 300min, naturally ring to
Room temperature.
Embodiment 2
It prepares PI and extracts stirring rod
10%PI (P84, Evonic) is substantially dissolved in solvent dimethylformamide, other operating conditions are same
Embodiment 1.
Embodiment 3
It prepares PDMS/PPESK, PDMS/PI and extracts stirring rod
10:1 in mass ratio prepares 184 solution of PDMS Sylgard, after miscible, be diluted to 0.5% with n-hexane, 1%,
2%, 5%, 10%, 20%, 50%v/v concentration.PPESK prepared by embodiment 1 is extracted into stirring rod, PI prepared by embodiment 2
Stirring rod is extracted, is immersed in 184 solution of PDMS Sylgard of respective concentration respectively, immersion is taken out after ten minutes, is dried in the air in air
It does, in an oven 60 DEG C of crosslinking curing PDMS.Then again under nitrogen protection, aging PDMS/PPESK, PDMS/PI extraction stirring
Stick.Aging procedure: 40 DEG C of maintenance 30min, 5 DEG C/min are raised to 100 DEG C of maintenance 30min, 5 DEG C/min and are raised to 200 DEG C of maintenances
30min, 5 DEG C/min are raised to 280 DEG C of maintenance 300min, naturally ring to room temperature.
Embodiment 4
Measure surface contact angle
Through detecting: PI extraction bar itself, 67 ° ± 5 ° of the contact angle of water；0.5% prepared by embodiment 3,1%, 2%,
112 ° ± 10 of the contact angle of the water of 5%, 10%, 20%, 50%v/v PDMS/PPESK extraction bar；This shows that PDMS is coated
To the surface PPESK, and concentration is down to 0.5% PDMS, so that it may effectively coating PI outer surface.
Embodiment 5
Observe PDMS coating microscopic appearance
Electronic scanner microscope observes material section obtained by embodiment 3, discovery: 0.5%, 1%, 2%, 5%,
10%, 20%PDMS coating layer thickness are less than 1 micron, and 50%PDMS coating layer thickness is less than 5-10 microns.
Electronic scanner microscope observes material surface, and discovery: there is intensive nano-pore on PI extraction bar surface, as PDMS is dense
The increase of degree, PDMS coating gradually enclose the nano-pore on surface, and in 10%PDMS coating, nano surface hole disappears substantially,
But still the micron-sized fluctuating of visible surface；In 50%DMS coating, nanometer range is down in surface undulation.
Embodiment 6
Measure the water absorption of PI extraction stirring rod, PDMS/PI extraction stirring rod
The 0.5%PDMS/PI extraction of the PI extraction stirring rod and the preparation in embodiment 3 that prepare in Example 2 is stirred
Stick is mixed, extraction phase size is identical: 60 microns of phase thickness of extraction, length 2cm.Extraction conditions: it in 10mL pure water solution, 40 DEG C, stirs
Mix speed 600rpm, extraction time 30min.It is directly placed into hot parser after the completion of extraction, 260 DEG C of high-temperature heating 7min, heat
The water vapour of parsing desorption is directly entered Agilent 7890B, carries out later separation analysis.
Chromatographic separation condition: HP-PLOT/Q chromatographic column, 20.0 μm of the μ m of 30m × 320, carrier gas are helium (99.999%),
3mL/min under constant current mode；300 DEG C of injection port.Column temperature: 40 DEG C of holding 9min are warming up to 200 with the heating rate of 8 DEG C/min
DEG C keep 5min；TCD detector.
Chromatographic quantitative analysis shows: PI extracts stirring rod and adsorbs 1.4 milligrams of water, and 0.5%PDMS/PI adsorpting water quantity only has
0.098 milligram, water absorption has dropped 93%；5%PDMS/PI adsorpting water quantity is 0.042 milligram, and water absorption has dropped 97%.
Embodiment 7
PDMS/PI extracts stirring rod, separating phenols compounds.
Detection material is that the PI prepared in embodiment 2 extracts the 0.5%PDMS/ of stirring rod and the preparation in embodiment 3
PI extracts stirring rod.Organic phenol standard sample: phenol, 2-chlorophenol, 2- nitrophenols, 2,4- dimethyl phenol, 2,4- Dichlorophenol, 4- it is chloro-
3- sylvan, 2,4,6- trichlorophenol.It is identical to extract phase size: 60 microns of phase thickness of extraction, length 2cm.Extraction conditions:
100ppb, 10mL organic phenol aqueous sample, 40 DEG C, mixing speed 600rpm, pH 3, extraction time 30min.After the completion of extraction
It is directly placed into hot parser, 260 DEG C of high-temperature heating 7min, the phenolic compound of Thermal desorption desorption is directly entered Agilent
7890B carries out separation analysis.
Chromatographic separation condition: Agilent DB-5 chromatographic column, 1.0 μm of the μ m of 30m × 250, carrier gas is helium
(99.999%), 3mL/min under constant current mode；300 DEG C of injection port.Column temperature: 40 DEG C of holding 9min, with the heating speed of 8 DEG C/min
Rate is warming up to 280 DEG C of holding 5min；FID temperature is 300 DEG C, H2Flow velocity 38mL/min, air velocity 400mL/min.
Chromatography spectrogram is as shown in Fig. 1.(A) as shown in figure 1, PI extraction bar adsorb a large amount of water, and in Thermal desorption
Gasification generates a large amount of water vapours, causes FID flame-out multiple；Phenol, 2-chlorophenol, the chromatography peak height of 2- nitrophenols are relatively low；2,4- bis-
Sylvan, 2, the division of 4- Dichlorophenol chromatographic peak.And 0.5%PDMS/PI extraction bar absorption water is few, a small amount of steam is without result in FID
Flame-out, also without reducing chromatographic isolation efficiency, chromatographic peak is sharp symmetrically, does not divide, (B) as shown in figure 1.
Embodiment 8
PDMS/PI extracts stirring rod, extracts nitrobenzene compound.
Detection material is that the PI prepared in embodiment 2 extracts the 0.5%PDMS/ of stirring rod and the preparation in embodiment 3
PI extracts stirring rod.Nitrobenzene standard sample: nitrobenzene, 2- nitrobenzene, 2- nitrotoleune, 3- nitrotoleune, 4- nitrobenzene, 2.4-
Dinitrobenzene, 2.6- dinitrobenzene.Extraction conditions: 20ppb, 10mL nitrobenzene aqueous sample, 40 DEG C, mixing speed
600rpm, pH 7；Extraction time 30min.It is directly placed into hot parser after the completion of extraction, 250 DEG C of high-temperature heating 7min, pyrolysis
The nitrobenzene compounds of analysis desorption are directly entered Agilent 7890B chromatographic column, carry out separation analysis.Chromatographic separation condition with
Embodiment 7 is identical.
Chromatography spectrogram is as shown in Fig. 2.Such as (A) in Fig. 2, PI extraction bar adsorbs a large amount of water, leads to nitrobenzene, 2-
Nitrobenzene, 2- nitrotoleune, the chromatography peak height of 3- nitrotoleune are relatively low, and the fluctuation of 4- nitrotoleune or so Chromatogram Baseline is very
Greatly.And 5%PDMS/PI extraction bar absorption water is few, chromatographic peak is sharp, baseline is steady, such as (B) in Fig. 2.
Claims (10)
1. a kind of solid phase extraction material, the material is core-shell structure, which is characterized in that the stratum nucleare is polarity Solid Phase Extraction
Material, shell are dimethyl silicone polymer.
2. material according to claim 1, which is characterized in that the polarity solid phase extraction material be selected from polyimides,
Polybenzimidazoles, polyethersulfone ketone, polyethylene glycol, polyacrylate, poly- divinylbenzene, Graphon, carbon molecular sieve and its spread out
Biology or composition.
3. material according to claim 2, which is characterized in that the polarity solid phase extraction material be selected from polyimides,
Polyethersulfone ketone, polybenzimidazoles, polyethylene glycol, polyacrylate.
4. material according to claim 1, it is characterised in that the dimethyl silicone polymer shell with a thickness of 1 nanometer
~10 microns.
5. the preparation method of solid phase extraction material described in claim 1, includes the following steps:
(1) stratum nucleare, including stratum nucleare film and stratum nucleare particle are prepared:
1a. prepares stratum nucleare film: solid phase extraction material is prepared as 0.1%~30% polymer solution；With infusion process, spray coating method
Or spin-coating method, 0.01 micron~1 millimeter of stratum nucleare film is formed in support carrier surface；And curing and drying；
1b. prepares stratum nucleare particle: solid phase extraction material being prepared as 0.1%~50% polymer solution, with spray drying, cream
The method change, being mechanically pulverized prepares 0.1 micron~1 mm granules, and curing and drying；
(2) preparation of shell: dimethyl silicone polymer and crosslinking agent 1:2~50 in mass ratio is miscible, then use hydrocarbon solvent
It is diluted to 0.1~50%；The stratum nucleare film or stratum nucleare particle of soaking step (1) preparation；Then take out solidification drying.
6. preparation method according to claim 5, which is characterized in that the solvent of the polymer solution of the step 1a and 1b
Selected from dimethyl sulfoxide, diethyl sulfoxide, N-methyl pyrrolidones and its mixed system.
7. preparation method according to claim 5, which is characterized in that crosslinking agent is DOW CORNING in the step (2)
Sylgard 184。
8. preparation method according to claim 5, which is characterized in that in the step (2) hydrocarbon solvent be selected from n-hexane,
Or mixtures thereof hexamethylene, pentane, benzene, toluene.
9. application of the material described in claim 1 in Solid Phase Extraction or solid phase microextraction.
10. applying according to claim 9, which is characterized in that including being returned after the completion of extraction to the solid phase extraction material
Receive the step of utilizing.
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Citations (5)
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| CN102883805A (en) * | 2010-04-28 | 2013-01-16 | 株式会社日立高新技术 | Adsorbent and method for producing same |
| CN102489249A (en) * | 2011-11-25 | 2012-06-13 | 中国检验检疫科学研究院 | Composite solid-phase extraction column used in vegetable pesticide removing, and preparation method thereof |
| CN106669446A (en) * | 2017-01-06 | 2017-05-17 | 宁波大学 | SVOCs solid-phase extraction membrane |
| CN106918660A (en) * | 2017-02-20 | 2017-07-04 | 安徽建筑大学 | A kind of organic pollution extracting process |
| CN108148112A (en) * | 2018-03-02 | 2018-06-12 | 中国科学院理化技术研究所 | A kind of glycopeptide enrichment method based on amphipathic porous core-shell particles |
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Application publication date: 20190104 |