CN101632918B - Grafting fiber material with adsorptive action and use method thereof - Google Patents
Grafting fiber material with adsorptive action and use method thereof Download PDFInfo
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- CN101632918B CN101632918B CN2008101320514A CN200810132051A CN101632918B CN 101632918 B CN101632918 B CN 101632918B CN 2008101320514 A CN2008101320514 A CN 2008101320514A CN 200810132051 A CN200810132051 A CN 200810132051A CN 101632918 B CN101632918 B CN 101632918B
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- 239000002657 fibrous material Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000000274 adsorptive effect Effects 0.000 title abstract 2
- 239000000463 material Substances 0.000 claims abstract description 77
- 239000000835 fiber Substances 0.000 claims abstract description 76
- -1 polyethylene Polymers 0.000 claims abstract description 41
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 34
- 239000000194 fatty acid Substances 0.000 claims abstract description 34
- 229930195729 fatty acid Natural products 0.000 claims abstract description 34
- 239000004743 Polypropylene Substances 0.000 claims abstract description 17
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 17
- 229920001155 polypropylene Polymers 0.000 claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 229920001577 copolymer Polymers 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 6
- 239000004698 Polyethylene Substances 0.000 claims abstract description 5
- 229920000573 polyethylene Polymers 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- 238000005406 washing Methods 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 29
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 125000000217 alkyl group Chemical group 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 229920002401 polyacrylamide Polymers 0.000 claims description 13
- 229920000058 polyacrylate Polymers 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 7
- 239000005416 organic matter Substances 0.000 claims description 7
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 125000003368 amide group Chemical group 0.000 claims description 4
- 238000012545 processing Methods 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 6
- 238000012546 transfer Methods 0.000 abstract description 5
- 238000005070 sampling Methods 0.000 abstract description 2
- 238000004587 chromatography analysis Methods 0.000 abstract 1
- 239000010419 fine particle Substances 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- 238000004949 mass spectrometry Methods 0.000 abstract 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 20
- 239000007788 liquid Substances 0.000 description 14
- 238000002360 preparation method Methods 0.000 description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 11
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 9
- 230000005855 radiation Effects 0.000 description 9
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 8
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000010828 elution Methods 0.000 description 7
- 238000010992 reflux Methods 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- 229920003023 plastic Polymers 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 238000002470 solid-phase micro-extraction Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- BHHGXPLMPWCGHP-UHFFFAOYSA-N Phenethylamine Chemical compound NCCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-N 0.000 description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FHNINJWBTRXEBC-UHFFFAOYSA-N Sudan III Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC(C=C1)=CC=C1N=NC1=CC=CC=C1 FHNINJWBTRXEBC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000036765 blood level Effects 0.000 description 1
- 230000035568 catharsis Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 1
- 229940107698 malachite green Drugs 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 description 1
- 229940080818 propionamide Drugs 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a grafting fiber material with adsorptive action, which comprises the materials of: 1) a fiber body and 2) a grafting material on the fiber body, wherein the fiber body is polyethylene, polypropylene or a copolymer of the two; the grafting material is fatty acid ester, fatty acid amide, the mixture of the fatty acid ester and the fatty acid amide, or a polymer of the fatty acid ester and the fatty acid amide; and the grafting material accounts for 1 to 35 percent of the entire fiber material in percentage by weight. The grafting fiber material can perform the process of solid-phase extraction stably and quickly, avoids the pollutions to samples, has a quick mass transfer velocity, can use a large-aperture (1 to 100 microns) film made from a non-porous fiber material to accelerate the processing of the samples, and avoids the pollution caused by fine particle falling; and simultaneously, the application of a grafting technique ensures the sampling volume of the samples. The grafting fiber material can be applied to extraction and purification of sample directly introduced in liquid phase chromatography or mass spectrometric analysis.
Description
Technical field
The present invention relates to a kind of fibrous material and method for using thereof, especially relate to a kind of have adsorbing graft fibres material and method for using thereof.
Background technology
The detection of chemistry and biotic component becomes and the closely-related content of people's daily life gradually in human body, food and the environment.This comprises that the patient takes medicine the back medicine in the mensuration of blood level, the mensuration of metabolin in the urine; The mensuration (like malachite green, tonyred) of residual or other harmful substance of food middle peasant, the mensuration of nutriment; The mensuration of harmful substance in the water and air.No matter all above testing processes are to use which kind of means, and great majority will pass through sample extraction, the process of enrichment and purification earlier.Film extraction and be that the SPME on basis is a comparatively leading technical products in this field in the world at present with the glass fibre has the advantages that program is simple, efficient is high, highly sensitive.But present SPME only can be used for the gas-chromatography check, has limited its range of application.Aspect environmental analysis, needs are done further processing and analysis after a large amount of soil samples, water sample and air sample are delivered to the laboratory at present, not only need long period and higher expense, and impact analysis result's reliability and reproduction type in addition.
The spe membrane that present SPME is used is that the particulate with bonded silica gel or high polymer sorbing material is fixed on the film.This material is widely used in the analytical method of EPA.Major vendor has 3M in the world, JT Baker and WATERS etc.; The major defect of this product comprises:
1) because sorbing material particle diameter less (to obtain mass transfer velocity faster) requires membrane pore size less (3-10um), causes thickness or dirtier sample easy blocking film;
2) granule comes off from film easily, pollutes the sample of collecting;
3) although use granule to accelerate mass transfer velocity, its absorption and desorption rate remain the principal element that appearance and elution speed are gone up in restriction, make the extraction required time further to shorten.
Summary of the invention
The technical problem that the present invention will solve provides a kind of adsorbing graft fibres material that has; This material can overcome above shortcoming, thereby guarantees stable and SPE process fast and the pollution of avoiding sample; Because this material mainly reaches absorption and the purpose of separating through grafted, so this material has mass transfer velocity faster; Simultaneously, because there is not the restriction of particulate, can use bigger membrane pore size (1-100 μ m) to quicken the processing of sample, the pollution of having avoided particulate to come off and cause.That is to say that this material can be used for the sample extraction and the purification of liquid chromatogram or mass spectral analysis direct injected.
Another technical problem that the present invention will solve provides a kind of use and has the method that adsorbing graft fibres material carries out SPE; Simple, the convenient and reliable on-the-spot sample pre-treatments of this method after the preliminary enrichment of sample purified, is adsorbed/is stored in certain material easy to carry and transport, afterwards again easily direct injected analyze the result to required analytical instrument.
For solving the problems of the technologies described above, the present invention is a kind of to have adsorbing graft fibres material, and it comprises following raw material:
1) fiber bodies;
2) graft materials on the fiber bodies;
Said fiber bodies is polyethylene, polypropylene or the copolymer of the two;
Said graft materials is the polymer of fatty acid ester, fatty acid amide, fatty acid ester and fatty acid amide or the mixture of fatty acid ester and fatty acid amide;
The percentage by weight that said graft materials accounts for whole fibrous material is 1～35%.
Further improved technical scheme, said graft fibres diameter is between the 1-100 micron.
Further improved technical scheme, said fatty acid ester has formula:
——CH
2-CH
2-COOR
Said R is the straight chained alkyl that contains 8-20 carbon.
Further improved technical scheme, said fatty acid amide has formula:
---CH
2-CH
2-COONHR or
Said R is the straight chained alkyl that contains 8-20 carbon; Said R ' is for containing the straight chained alkyl of 1-20 carbon.
Further improved technical scheme, described graft materials are polyacrylate, polyacrylamide or the copolymer of the two.
Further improved technical scheme, the alkoxyl in the said polyacrylate are the alkoxyl that contains 8-20 carbon, and the amido in the said polyacrylamide is the fatty amido that contains 8-20 carbon.
For solving above-mentioned second technical problem, a kind of use of the present invention has the method that adsorbing graft fibres material carries out SPE, comprises the steps:
1) the graft fibres sorbing material was soaked into 1～60 minute with acetonitrile, methyl alcohol, ethanol or acetone, use the drip washing of washing water solution again;
2) will treat that the fibrous material after extraction solution and the drip washing contacts, and extracts;
3) fiber after will extracting is with " washing water solution " drip washing;
4) be adsorbed on the organic matter on the fiber with solvent elution;
Said eluting solvent is the mixture of one or more arbitrary proportions in acetonitrile, methyl alcohol, ethanol, oxolane, ethyl acetate or the carrene;
Said " washing water solution " is for containing the aqueous solution of volume ratio 0～5% organic solvent; Said organic solvent is the mixture of one or more arbitrary proportions among methyl alcohol, ethanol, acetonitrile or the acetone.
The purposes of graft fibres material in SPE that the present invention makes; The material preparation of use graft fibres goes out various different shapes; Various devices as SPE:, process the SPE film of various difformities (box size length, side, circle) and different sizes (areas) after the multilayer stack 1) with the fiber after the grafting processing; 2) with behind the fibrous material strands after the grafting processing, prepare the extracting head that can be used for SPME; 3) the back fibrous material is handled in grafting or fiber membrane places syringe, processed and can be used for SPE and on-the-spot example enrichment, purify device.
Operation principle of the present invention is following:
Most of example enrichments and purification are based on the process of certain material chosen property surface adsorption and parsing.Be the selective absorption measured matter first, the drip washing of a large amount of matrix interference thing is fallen, wash-out measured matter under given conditions again, and reach the enrichment catharsis; Perhaps anti-its road will disturb matrix to be adsorbed in material surface, and the drip washing of measured object selectivity will be got off.The enrichment purification effects depends on the selectivity of material surface, absorption/parsing balancing speed, adsorption capacity.The granular materials of porous high-ratio surface is adopted in traditional SPE, is filled in a cast container.Sample solution is added in the pipe, and chaff interference is removed in washing then, uses particular solution wash-out measured object again, concentrate eluant, and sampling detects then.Be characterized in that sample capacity is high, favorable reproducibility; But process is long, and efficient is low, and the sample requirement is big, and sensitivity is low.Present SPME adopts solid fiberglass surfacing to scribble one deck semifluid sorbing material, after the selective absorption measured object, and in the gas chromatograph injection port, the high temperature desorption.Its advantage is to use process simple, and is highly sensitive; But because specific surface is low, and the absorption/parsing balancing speed of sample in the semifluid sorbing material is slow, causes sample capacity low, poor reproducibility, and only be applicable to gas chromatographic detection.Of the present invention is that novel quick extraction and sample introduction product and the technology of carrier is to be material of main part with novel high functionalisation of surfaces graft fibres with functionalized fiber; After stranded, process; Both had high functionalized surfaces; Kept absorption/fast advantage of parsing balance again, and favorable mechanical stability has been arranged.Be processed into needle-based and form of film product, thereby can be used for liquid chromatogram or mass spectrum direct injected, expanding application scope.New product is having traditional SPE high power capacity simultaneously, high reappearance and unique high sensitivity, use simple, the advantage that desorption rate is fast.Its occupation mode is: with the fiber adsorbing material of sample solution after extraction for several times is through processing; Measured object is adsorbed in functionalized fiber surface, then uses particular elutriated liquid, with the direct wash-out of sample in; Gas phase, liquid chromatogram or mass spectrum injector, or adopt alternate manner to measure behind the some plate.
The present invention has following beneficial effect: graft fibres material of the present invention can be stablized and carry out the SPE process fast, has avoided the pollution of sample; Have mass transfer velocity faster, can use bigger aperture (1-100 μ m) to quicken the processing of sample, the pollution of having avoided particulate to come off and cause; This material can be used for the sample extraction and the purification of liquid chromatogram or mass spectral analysis direct injected.Method of the present invention is simple, convenient, and on-the-spot sample pre-treatments is reliable, and direct injected analyzes the result to required analytical instrument easily.
The specific embodiment
Embodiment 1
A kind of to have adsorbing graft fibres preparation methods following: get polypropylene fibre 10 grams, through radiation gamma 10 minutes, put into 500ml and contain the acrylic acid aqueous solution of 1% (weight ratio), stirred 4 hours down at 50 ℃; Taking out the back uses pure water rinsing to be neutrality to collecting liquid; Vacuum drying weigh 10.6 the gram; Dried fibrous material is put into and is contained 2 gram N, in the 200ml tetrahydrofuran solution of N ' dicyclohexylcarbodiimide, adds 5 gram octadecanol reflux again 4 hours; Make polyacrylate grafting fiber 12 grams.
Embodiment 2
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into 500ml and contain the acrylic acid aqueous solution of 1% (weight ratio) and stirred 4 hours down at 52 ℃; Taking out the back uses pure water rinsing to be neutrality to collecting liquid.Vacuum drying weigh 10.6 the gram.Dried fibrous material is put into and is contained 2 gram N, in the 200ml tetrahydrofuran solution of N ' dicyclohexylcarbodiimide, adds 5 grams, 12 carbon alcohol reflux again 4 hours, makes polyacrylate grafting fiber 11.8 grams.
Embodiment 3
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into 500ml and contain the acrylic acid aqueous solution of 1% (weight ratio) and stirred 4 hours down at 54 ℃; Taking out the back uses pure water rinsing to be neutrality to collecting liquid; Vacuum drying weigh 10.6 the gram; Dried fibrous material is put into and is contained 2 gram N, in the 200ml tetrahydrofuran solution of N ' dicyclohexylcarbodiimide, adds 5 gram octanol reflux again 4 hours, makes polyacrylate grafting fiber 11.5 grams.
Embodiment 4
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into 500ml and contain the acrylic acid aqueous solution of 1% (weight ratio) and stirred 4 hours down at 56 ℃; Taking out the back uses pure water rinsing to be neutrality to collecting liquid; Vacuum drying weigh 10.6 the gram; Dried fibrous material is put into and is contained 2 gram N, in the 200ml tetrahydrofuran solution of N ' dicyclohexylcarbodiimide, adds 5 grams, 18 carbon amine reflux again 4 hours, makes Polyacrylamide Grafted fiber 12.3 grams.
Embodiment 5
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into 500ml and contain the acrylic acid aqueous solution of 1% (weight ratio) and stirred 4 hours down at 58 ℃; Taking out the back uses pure water rinsing to be neutrality to collecting liquid; Vacuum drying weigh 10.6 the gram; Dried fibrous material is put into and is contained 2 gram N, in the 200ml tetrahydrofuran solution of N ' dicyclohexylcarbodiimide, adds 5 gram octylame reflux again 4 hours, makes Polyacrylamide Grafted fiber 11.9 grams
Embodiment 6
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into 500ml and contain the acrylic acid aqueous solution of 5% (weight ratio) and stirred 3 hours down at 59 ℃; Taking out the back uses pure water rinsing to be neutrality to collecting liquid.Vacuum drying weigh 11.5 the gram; Dried fibrous material is put into and is contained 4 gram N, in the 200ml tetrahydrofuran solution of N ' dicyclohexylcarbodiimide, adds 10 gram octylame reflux again 4 hours, makes Polyacrylamide Grafted fiber 13.4 grams.
Embodiment 7
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into 500ml and contain the acrylic acid aqueous solution of 5% (weight ratio) and stirred 3 hours down at 57 ℃; Taking out the back uses pure water rinsing to be neutrality to collecting liquid.Vacuum drying weigh 11.5 the gram.Dried fibrous material is put into and is contained 4 gram N, in the 200ml tetrahydrofuran solution of N ' dicyclohexylcarbodiimide, adds 10 gram octanol reflux again 4 hours, makes polyacrylate grafting fiber 13.1 grams.
Embodiment 8
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into the tetrahydrofuran solution that 500ml contains 3% (weight ratio) acrylic acid octadecyl acid amides and stirred 8 hours down at 55 ℃; Do not contain raw material or polymer with methyl alcohol and oxolane flushing in the liquid to collecting respectively after the taking-up, vacuum drying-obtain Polyacrylamide Grafted fiber 12.7 to restrain.
Embodiment 9
It is a kind of that to have adsorbing graft fibres preparation methods following: polypropylene fibre 10 grams, and through radiation gamma 10 minutes, put into the tetrahydrofuran solution that 500ml contains 3% (weight ratio) dodecylacrylate and stirred 8 hours down at 53 ℃; Do not contain raw material or polymer with methyl alcohol and oxolane flushing in the liquid to collecting respectively after the taking-up, vacuum drying-obtain polyacrylate grafting fiber 12.6 to restrain.
Embodiment 10
A kind of have an adsorbing graft fibres material, and fiber bodies is a polypropylene, and the graft materials on the fiber bodies is the mixture of polyacrylate/polyacrylamide.Its preparation method is following: get polyacrylate grafting fiber 12 grams that obtain among the embodiment 1, insert 500 milliliters and contain 2% (weight ratio) N, the tetrahydrofuran solution of N ' dicyclohexylcarbodiimide and 5% (weight ratio) propylamine refluxed 8 hours; With oxolane and methanol wash, drying obtains polyacrylate/polyacrylamide mixed grafting fiber 12.3 grams.
Embodiment 11
A kind of have an adsorbing graft fibres material, and the preparation method is following: Polyacrylamide Grafted fiber 10 grams that obtain among the embodiment 4, insert 500 milliliters of tetrahydrofuran solutions that contain 2%DCC and 5% propylamine, and refluxed 8 hours; With oxolane and methanol wash, drying obtains polypropylene stearamide/polypropylene propionamide mixed grafting fiber 10.4 grams.
Embodiment 12
A kind of use has the method that adsorbing graft fibres material carries out SPE; Comprise the steps: the polyacrylate that obtains in the instance 10/polyacrylamide mixed grafting fiber is placed 6 milliliters of plastic tubes for 500 milligrams, soak into the back with 2 ml methanol and clean with 2 ml deionized water; With 100 milliliters of aqueous solution that contain each 100 microgram of naphthalene, anthracene, phenyl ethylamine through the plastic tube of fiber is housed; Clean fiber and plastic tube for 5 milliliters with 5% methanol aqueous solution; Naphthalene, anthracene and the phenyl ethylamine that will be attracted on the fiber with 2 milliliters of acetonitriles wash and receive.
Embodiment 13
A kind of use has the method that adsorbing graft fibres material carries out SPE; Comprise the steps: 500 milligrams of the polyacrylamide mixed grafting fibers that obtains in the instance 11 are placed 6 milliliters of plastic tubes, soak into the back with 2 ml methanol and clean with 2 ml deionized water; With 100 milliliters of aqueous solution that contain each 100 microgram of naphthalene, anthracene, phenyl ethylamine through the plastic tube of fiber is housed; Clean fiber and plastic tube for 5 milliliters with 5% methanol aqueous solution; Naphthalene, anthracene and the phenyl ethylamine that will be attracted on the fiber with 2 milliliters of acetonitriles wash and receive.
Embodiment 14
A kind of have an adsorbing graft fibres material, and it comprises following raw material:
1) fiber bodies;
2) graft materials on the fiber bodies;
Said fiber bodies is a polyethylene; Said graft materials is a fatty acid ester;
The percentage by weight that said graft materials accounts for whole fibrous material is 1%;
Said fatty acid ester molecular formula is:---CH
2-CH
2-COOC
8H
17
A kind of use has the method that adsorbing graft fibres material carries out SPE, comprises the steps:
1) the graft fibres sorbing material was soaked into 1 minute with acetonitrile, use " washing water solution " drip washing again;
2) will treat that the fibrous material after extraction solution and the drip washing contacts, and extracts;
3) fiber after will extracting is with the drip washing of washing water solution;
4) be adsorbed on the organic matter on the fiber with solvent elution;
Said solvent is an acetonitrile;
Said " washing water solution " is for containing the organic solvent of volume ratio 1%; Said organic solvent is a methyl alcohol.
Embodiment 15
A kind of have an adsorbing graft fibres material, and it comprises following raw material:
1) fiber bodies;
2) graft materials on the fiber bodies;
Said fiber bodies is a polypropylene;
Said graft materials is a fatty acid amide;
Said fatty acid amide molecular formula is:
---CH
2-CH
2The said R of-COONHR is the straight chained alkyl that contains 20 carbon;
The percentage by weight that said graft materials accounts for whole fibrous material is 7%;
A kind of use has the method that adsorbing graft fibres material carries out SPE, comprises the steps:
1) the graft fibres sorbing material was soaked into 60 minutes with methyl alcohol, use " washing water solution " drip washing again;
2) will treat that the fibrous material after extraction solution and the drip washing contacts, and extracts;
3) fiber after will extracting is with the drip washing of washing water solution;
4) be adsorbed on the organic matter on the fiber with solvent elution;
Said solvent is a methyl alcohol; Said " washing water solution " is for containing the organic solvent of volume ratio 2%; Said organic solvent is an ethanol.
Embodiment 16
A kind of have an adsorbing graft fibres material, and it comprises following raw material:
1) fiber bodies;
2) graft materials on the fiber bodies;
Said fiber bodies is a polypropylene;
Said graft materials is a fatty acid ester, and said fatty acid ester has following molecular formula:
——CH
2-CH
2-COOR
Said R is the straight chained alkyl that contains 20 carbon.
The percentage by weight that said graft materials accounts for whole fibrous material is 16%.
A kind of use has the method that adsorbing graft fibres material carries out SPE, comprises the steps:
1) the graft fibres sorbing material was soaked into 40 minutes with methyl alcohol, use " washing water solution " drip washing again;
2) will treat that the fibrous material after extraction solution and the drip washing contacts, and extracts;
3) fiber after will extracting is with the drip washing of washing water solution;
4) be adsorbed on the organic matter on the fiber with solvent elution;
Said solvent is an ethanol; Said " washing water solution " is for containing the organic solvent of volume ratio 3% acetonitrile.
Embodiment 17
A kind of have an adsorbing graft fibres material, and it comprises following raw material:
1) fiber bodies;
2) graft materials on the fiber bodies;
Said fiber bodies is polyethylene and polyacrylic copolymer;
Said graft materials is a fatty acid amide; The molecular formula of said fatty acid amide:
Said R is the straight chained alkyl that contains 12 carbon; Said R ' is for containing the straight chained alkyl of 14 carbon.The percentage by weight that said graft materials accounts for whole fibrous material is 25%;
A kind of use has the method that adsorbing graft fibres material carries out SPE, comprises the steps:
1) the graft fibres sorbing material was soaked into 20 minutes with acetone, use " washing water solution " drip washing again;
2) will treat that the fibrous material after extraction solution and the drip washing contacts, and extracts;
3) fiber after will extracting is with the drip washing of washing water solution;
4) be adsorbed on the organic matter on the fiber with solvent elution;
Said solvent is an oxolane; Said " washing water solution " is for containing the organic solvent of volume ratio 5% acetone;
Embodiment 18
A kind of have an adsorbing graft fibres material, and it comprises following raw material:
1) fiber bodies;
2) graft materials on the fiber bodies;
Said fiber bodies is polypropylene or the copolymer of the two; Said graft materials is the mixture of fatty acid ester and fatty acid amide;
Said fatty acid ester molecular formula is:---CH
2-CH
2-COOR; Said R is the straight chained alkyl that contains 16 carbon;
Said fatty acid amide molecular formula is:---CH
2-CH
2-COONHR; Said R is the straight chained alkyl that contains 16 carbon; Said R ' is for containing the straight chained alkyl of 16 carbon.
The percentage by weight that said graft materials accounts for whole fibrous material is 35%.
A kind of use of the present invention has the method that adsorbing graft fibres material carries out SPE, comprises the steps:
1) the graft fibres sorbing material was soaked into 10 minutes with ethanol, use " washing water solution " drip washing again;
2) will treat that the fibrous material after extraction solution and the drip washing contacts, and extracts;
3) fiber after will extracting is with the drip washing of washing water solution;
4) be adsorbed on the organic matter on the fiber with solvent elution;
Said solvent is the mixture of ethyl acetate and carrene;
Said " washing water solution " is for containing the organic solvent of volume ratio 4% ethanol.
Embodiment 19
Prepared through embodiment 1-18 at the graft fibres material; Prepare various different shapes; The various devices that are used for SPE:, process the SPE film of various difformities (box size length, side, circle) and different sizes (areas) after the multilayer stack 1) with the nonwoven after the grafting processing; 2) with behind the fibrous material strands after the grafting processing, prepare the extracting head that can be used for SPME; 3) the back fibrous material is handled in grafting or fiber membrane places syringe, processed and can be used for SPE and on-the-spot example enrichment, purify device.
Obviously, the above embodiment of the present invention only be for clearly the present invention is described and is done for example, and be not to be qualification to embodiment of the present invention.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or change.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (5)
1. a use has the method that adsorbing graft fibres material carries out SPE, it is characterized in that, comprises the steps:
1) the graft fibres sorbing material was soaked into 1～60 minute with acetonitrile, methyl alcohol, ethanol or acetone, use " washing water solution " drip washing again;
2) will treat that the fibrous material after extraction solution and the drip washing contacts, and extracts;
3) fiber after will extracting is with " washing water solution " drip washing;
4) be adsorbed on the organic matter on the fiber with the eluting solvent wash-out;
Said " washing water solution " is the aqueous solution that contains the organic solvent of volume ratio 0～5%; Said organic solvent is the mixture of more than one arbitrary proportions among methyl alcohol, ethanol, acetonitrile or the acetone;
Said have an adsorbing graft fibres material, and it comprises:
1) fiber bodies;
2) graft materials on the fiber bodies;
Said fiber bodies is polyethylene, polypropylene or the copolymer of the two;
Said graft materials is a kind of in fatty acid ester, the fatty acid amide, perhaps is the polymer of fatty acid ester and fatty acid amide, perhaps is the mixture of fatty acid ester and fatty acid amide;
Said fatty acid ester has formula:
——CH
2-CH
2-COOR
Said R is the straight chained alkyl that contains 8-20 carbon;
Said fatty acid amide has formula:
---CH
2-CH
2-CONHR or
Said R is the straight chained alkyl that contains 8-20 carbon; Said R ' is for containing the straight chained alkyl of 1-20 carbon;
The percentage by weight that said graft materials accounts for whole fibrous material is 1～35%.
2. method according to claim 1 is characterized in that, said graft fibres diameter is between the 1-100 micron.
3. method according to claim 1 is characterized in that, described graft materials is polyacrylate, polyacrylamide or the copolymer of the two.
4. method according to claim 3 is characterized in that, the alkoxyl in the said polyacrylate is the alkoxyl that contains 8-20 carbon, and the amido in the said polyacrylamide is the fatty amido that contains 8-20 carbon.
5. method according to claim 1 is characterized in that: said eluting solvent is the solvent of more than one arbitrary proportions in acetonitrile, methyl alcohol, ethanol, oxolane, ethyl acetate or the carrene.
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| CN1584188A (en) * | 2004-06-11 | 2005-02-23 | 上海大学 | Preparing method for temperature controlling ionic absorbing fibre |
| CN1843619A (en) * | 2006-03-31 | 2006-10-11 | 胡秀峰 | Method for preparing high-selective absorbing and separating fiber material |
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| CN1584188A (en) * | 2004-06-11 | 2005-02-23 | 上海大学 | Preparing method for temperature controlling ionic absorbing fibre |
| CN1843619A (en) * | 2006-03-31 | 2006-10-11 | 胡秀峰 | Method for preparing high-selective absorbing and separating fiber material |
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