CN101992074B - Metal carrier solid phase microextraction fiber - Google Patents
Metal carrier solid phase microextraction fiber Download PDFInfo
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- CN101992074B CN101992074B CN 201010270814 CN201010270814A CN101992074B CN 101992074 B CN101992074 B CN 101992074B CN 201010270814 CN201010270814 CN 201010270814 CN 201010270814 A CN201010270814 A CN 201010270814A CN 101992074 B CN101992074 B CN 101992074B
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Abstract
The invention discloses a metal carrier solid phase microextraction fiber, and relates to the field of trace analysis of organic matters in foods, environment and biological samples. The metal carrier solid phase microextraction fiber consists of a carrier, and a coating on the surface of the carrier, wherein the carrier is a metal fiber with the length of 10 to 40mm and the diameter of 0.1 to 0.5mm; the coating comprises an adsorbent layer and a heat-resistant epoxy resin layer or organic silicon resin layer; and the adsorbent is one or more of graphitized carbon black, silica gel and clay. The extraction fiber has porous surface, high thermal stability and high adsorption capacity without retaining water, and is particularly suitable for analyzing trace contaminants in water and air.
Description
Technical field
The present invention relates to organic trace analysis field in food, environment, the biological sample, particularly a kind of metallic carrier solid-phase micro-extraction fibre.
Background technology
(solid phase microextraction, SPME) technology is a kind of sample pre-treatments technology of novelty in SPME.1989, the Belardi of Canadian Waterloo university and Pawliszynl reported first the SPME technology; 1993, the Supelco company of the U.S. released commercial SPME device; Nineteen ninety-five, Chen and Pawliszynl design SPME-high performance liquid chromatography (SPME-HPLC) combination interface device, and produce commodity by Supelco company.1997, Eisert and Pawliszyn designed interior (In-tube) SPME-HPLC combined apparatus of SPME-HPLC combined apparatus-pipe of auto injection; 1997, Nguyen etc. realized the on-line coupling of SPME-Capillary Electrophoresis (SPME-CE).In addition, SPME also can with Fourier transform infrared spectroscopy (FTIR), ultra-violet absorption spectrum (UV), inductivity coupled plasma mass spectrometry couplings such as (ICP-Ms).
SPME centralized procurement appearance, extraction, concentrate, sample introduction is in one, have easy, quick, portable, efficient, need not organic solvent and be easy to the advantage with analysis Instrument crosslinkings such as gas-chromatography, high performance liquid chromatography, gas chromatography mass spectrometry, Capillary Electrophoresis.Therefore, obtained in fields such as environmental analysis, food analysis, Pharmaceutical Analysis, biological sample analysises using widely.The evaluating objects thing of SPME also comprises inorganic matter, element etc. except organic matter, can be used for the analysis of all kinds of volatilizations and half volatile substance in the samples such as gas, liquid, solid.
Commercial the earliest SPME (Fiber SPME) device shape is made up of extracting head and handle two parts like a syringe.Extracting head is that a 1cm is long, scribbles the vitreous silica fiber of different fixing phase.Therefore, extracting head in use very easily fractures.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of metallic carrier solid-phase micro-extraction fibre is provided.
The technical scheme that the present invention adopts is:
A kind of metallic carrier solid-phase micro-extraction fibre; Form by carrier and coating surfaces thereof; Said carrier is long 10-40mm, and diameter is the metallic fiber of 0.1-0.5mm, and said coating comprises adsorbent layer; Also comprise high-temperature-resistant epoxy resin layer or silicone resin layer, said adsorbent be in ketjenblack EC, silica gel or the clay one or more.
A kind of metallic carrier solid-phase micro-extraction fibre, this extracting fiber are to prepare according to the method that comprises the steps:
(a) choose long 10-40mm, diameter is the metallic fiber of 0.1-0.5mm, utilizes dense HF to corrode 10-60min, takes out, and distilled water flushing utilizes N to neutral
2Dry up;
(b) elder generation is at the surface-coated one deck high-temperature-resistant epoxy resin or the organic siliconresin of the metallic fiber of process surface preparation; Pick one deck adsorbent at skin again; Said adsorbent be in ketjenblack EC, silica gel or the clay one or more, coating or repeat to be coated with stain and pick and adjust coating layer thickness;
The extracting fiber that (c) will coat coating places and carries out hot setting in the baking oven;
(d) extracting fiber that hot setting is good places cable type extractor according, with carrene in 40-80 ℃ of backflow 20-120min, to remove impurity.
Preferably, said metallic fiber is stainless steel fibre or alloy fiber.
Preferably, said adsorbent is a ketjenblack EC, and particularly, said adsorbent is Carbograph.
Preferably; The synthetic method of said high-temperature-resistant epoxy resin is stirred to dissolving fully in epoxy resin, adding organic solvent; Add curing agent, auxiliary agent and filler more successively, stirring is uniformly dispersed each component, prepares high-temperature-resistant epoxy resin; Wherein the ratio of weight and number of each material is: epoxy resin: curing agent: auxiliary agent: filler=20: 3: 3: 4, place below 5 ℃ to store for future use.
Preferably, said organic solvent is a kind of in xylenes, toluene, benzene or the acetone.
Preferably, said curing agent is the agent of acid anhydrides type, is preferably pyromellitic dianhydride.
Preferably, said auxiliary agent is a tertiary amine.
Preferably, said filler is a kind of in flake asbestos, aluminium powder or the titanium white powder.
The beneficial effect that the present invention had
The invention provides a kind of metallic carrier solid-phase micro-extraction fibre; Utilize synthetic high-temperature-resistant epoxy resin or organic siliconresin that adsorbent is fixed on the metallic fiber surface; Form Heat stability is good, thus anti-solvent washing coating material realize enrichment to trace organic substance.Replace traditional quartz fibre to make extracting fiber have higher mechanical strength with metallic fiber; Adsorbent is attached to the form on the extracting fiber, is convenient to the static head space capture of adsorbent sample.Extracting fiber porous surface of the present invention, heat endurance is high, does not keep water, adsorption capacity is big, be particularly suitable in the branch bleed with air in trace contaminant.
Description of drawings
Fig. 1 is not for using the gas-chromatography baseline chart of extracting fiber;
Fig. 2 is the gas-chromatography baseline chart under the extracting fiber desorption temperature that uses embodiment 1;
Fig. 3 is the gas chromatogram that utilizes the extracting fiber extraction benzene series thing of embodiment 1.
Among Fig. 3,1 is benzene, and 2 is toluene, and 3 is ethylbenzene, and 4 is paraxylene, and 5 is ortho-xylene.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is described further.
Embodiment 1
Choose long 20mm, diameter is the stainless steel fibre of 0.35mm, utilizes dense HF to corrode 30min, takes out, and distilled water flushing utilizes N to neutral
2Dry up; Take by weighing 100g epoxy resin, add xylenes and be stirred to dissolving fully, add 15g pyromellitic dianhydride, 15g tertiary amine and 20g flake asbestos more successively, stirring is uniformly dispersed each component, makes high-temperature-resistant epoxy resin; At the surface-coated one deck high-temperature-resistant epoxy resin of the stainless steel fibre of handling, pick one deck Carbograph at skin again, place in the baking oven in 180 ℃ of hot setting 60min; The extracting fiber that hot setting is good places in the middle of the cable type extractor according, utilizes carrene in 60 ℃ of backflow 40min, makes extracting fiber.
Wherein epoxy resin is multifunctional glycidol type epoxy resin, and market is bought and obtained.
Choose long 20mm, diameter is the stainless steel fibre of 0.35mm, utilizes dense HF to corrode 40min, takes out, and distilled water flushing utilizes N to neutral
2Dry up; At the surface-coated one deck organic siliconresin of the stainless steel fibre of handling, pick one deck clay at skin again, place in the baking oven in 180 ℃ of hot setting 60min; The extracting fiber that hot setting is good; Place in the middle of the cable type extractor according, utilize carrene, make extracting fiber in 60 ℃ of backflow 40min.
Utilize the extracting fiber of making among the embodiment 1 that the organic substance in the river is analyzed, take the immersion mode to extract.
Embodiment 4
Utilize the extracting fiber of making among the embodiment 2 that the fruit essence component is fragrant and analyze, take the head space mode to extract.
The above only is preferred embodiment of the present invention, is not technical scheme of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (8)
1. a metallic carrier solid-phase micro-extraction fibre is characterized in that, this extracting fiber is to prepare according to the method that comprises the steps:
(a) choose long 10-40mm, diameter is the metallic fiber of 0.1-0.5mm, utilizes dense HF to corrode 10-60min, takes out, and distilled water flushing utilizes N to neutral
2Dry up;
(b) elder generation is at the surface-coated one deck high-temperature-resistant epoxy resin or the organic siliconresin of the metallic fiber of process surface preparation; Pick one deck adsorbent at skin again; Said adsorbent be in ketjenblack EC, silica gel or the clay one or more, coating or repeat to be coated with stain and pick and adjust coating layer thickness;
The extracting fiber that (c) will coat coating places and carries out hot setting in the baking oven;
(d) extracting fiber that hot setting is good places cable type extractor according, with carrene in 40-80 ℃ of backflow 20-120min, to remove impurity.
2. a kind of metallic carrier solid-phase micro-extraction fibre according to claim 1 is characterized in that: said metallic fiber is an alloy fiber.
3. a kind of metallic carrier solid-phase micro-extraction fibre according to claim 2 is characterized in that: said metallic fiber is a stainless steel fibre.
4. a kind of metallic carrier solid-phase micro-extraction fibre according to claim 1 and 2 is characterized in that: said adsorbent is a ketjenblack EC.
5. a kind of metallic carrier solid-phase micro-extraction fibre according to claim 1 and 2; It is characterized in that: the synthetic method of said high-temperature-resistant epoxy resin is stirred to dissolving fully in epoxy resin, adding organic solvent; Add curing agent, auxiliary agent and filler more successively, stirring is uniformly dispersed each component, prepares high-temperature-resistant epoxy resin; Wherein the ratio of weight and number of each material is: epoxy resin: curing agent: auxiliary agent: filler=20: 3: 3: 4, place below 5 ℃ to store for future use.
6. a kind of metallic carrier solid-phase micro-extraction fibre according to claim 5 is characterized in that: said organic solvent is a kind of in xylenes, toluene, benzene or the acetone.
7. a kind of metallic carrier solid-phase micro-extraction fibre according to claim 5 is characterized in that: said curing agent is a pyromellitic dianhydride.
8. a kind of metallic carrier solid-phase micro-extraction fibre according to claim 5 is characterized in that: said auxiliary agent is a tertiary amine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010270814 CN101992074B (en) | 2010-09-02 | 2010-09-02 | Metal carrier solid phase microextraction fiber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010270814 CN101992074B (en) | 2010-09-02 | 2010-09-02 | Metal carrier solid phase microextraction fiber |
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| CN101992074A CN101992074A (en) | 2011-03-30 |
| CN101992074B true CN101992074B (en) | 2012-09-26 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102366718A (en) * | 2011-06-28 | 2012-03-07 | 天津春发食品配料有限公司 | Stir extraction bar with carbon nanofiber coating and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6905031B1 (en) * | 1999-09-13 | 2005-06-14 | The Regents Of The University Of California | Solid phase microextraction device using aerogel |
| CN1736581A (en) * | 2005-07-29 | 2006-02-22 | 中国科学院长春应用化学研究所 | Carbon-ceramic utilized absorption material |
| CN1967240A (en) * | 2006-11-23 | 2007-05-23 | 浙江大学 | Method applied for analysis gas or liquid sample in sealed system |
| CN101693539A (en) * | 2009-10-23 | 2010-04-14 | 北京市农业环境监测站 | Nanometer fibrous white carbon black and preparation method and application thereof |
-
2010
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6905031B1 (en) * | 1999-09-13 | 2005-06-14 | The Regents Of The University Of California | Solid phase microextraction device using aerogel |
| CN1736581A (en) * | 2005-07-29 | 2006-02-22 | 中国科学院长春应用化学研究所 | Carbon-ceramic utilized absorption material |
| CN1967240A (en) * | 2006-11-23 | 2007-05-23 | 浙江大学 | Method applied for analysis gas or liquid sample in sealed system |
| CN101693539A (en) * | 2009-10-23 | 2010-04-14 | 北京市农业环境监测站 | Nanometer fibrous white carbon black and preparation method and application thereof |
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