CN101992073A - Metal carrier Tenax coating solid-phase microextraction fiber - Google Patents
Metal carrier Tenax coating solid-phase microextraction fiber Download PDFInfo
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- CN101992073A CN101992073A CN201010270682XA CN201010270682A CN101992073A CN 101992073 A CN101992073 A CN 101992073A CN 201010270682X A CN201010270682X A CN 201010270682XA CN 201010270682 A CN201010270682 A CN 201010270682A CN 101992073 A CN101992073 A CN 101992073A
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Abstract
The invention relates to a metal carrier Tenax coating solid-phase microextraction fiber relating to the field of trace analysis of organic matters contained in food, environment and biology samples. The metal carrier Tenax coating solid-phase microextraction fiber comprises a carrier and a coating, wherein the coating is positioned on the surface of the carrier; the carrier is a metal fiber with the length of 10-40 mm and the diameter of 0.1-0.5 mm; and the coating comprises a Tenax adsorbent and a high-temperature resistant epoxy resin layer or an organic silicon resin layer. The metal carrier Tenax coating solid-phase microextraction fiber has the advantages of higher mechanical strength, good heat stability of the coating and solvent washing resistance, and is suitable for the processing of samples, i.e. soil, atmosphere, essences, flavors, indoor air, alcohol, phenol, amine aldehyde, ketone, halogenated aryl hydrocarbon, and the like.
Description
Technical field
The present invention relates to organic trace analysis field in food, environment, the biological sample, particularly a kind of metallic carrier Tenax coating solid phase micro-extraction fiber.
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 sample, extraction, concentrate, sample introduction is in one, have easy, quick, portable, efficient, need not organic solvent and be easy to analyze the advantage of Instrument crosslinkings with gas-chromatography gas-chromatography, high performance liquid chromatography, gas chromatography mass spectrometry, Capillary Electrophoresis etc.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
For solving the problems of the technologies described above, the invention provides a kind of metallic carrier Tenax coating solid phase micro-extraction fiber.
The technical solution used in the present invention is:
A kind of metallic carrier Tenax coating solid phase micro-extraction fiber, coating by carrier and surface thereof is formed, and described carrier is long 10-40mm, and diameter is the metallic fiber of 0.1-0.5mm, described coating comprises the Tenax adsorbent, also comprises high-temperature-resistant epoxy resin layer or silicone resin layer.
A kind of metallic carrier Tenax coating solid phase micro-extraction fiber, this extracting fiber is prepared by the method that comprises following 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, distilled water flushing utilizes N to neutral
2Dry up;
(b), at the surface-coated one deck high-temperature-resistant epoxy resin or the organic siliconresin of the metallic fiber of handling through step (a), pick one deck Tenax adsorbent at skin again, coating or adjust coating layer thickness by repeating step (b);
(c), the metallic fiber of coated coating is placed carry out hot setting in the baking oven;
(d), extracting fiber that hot setting is good, place in the middle of the cable type extractor according, utilize carrene in 40-80 ℃ of backflow 20-120min, to remove impurity.
Preferably, described metallic fiber is stainless steel fibre or alloy fiber.
Preferably, described Tenax adsorbent is selected from 2,6-dibenzofuran porous polymeric resins or other base polymer coatings.
Preferably, the synthetic method of described high-temperature-resistant epoxy resin is stirred to dissolving fully for add organic solvent in epoxy resin, add curing agent, auxiliary agent and filler more successively, stirring is uniformly dispersed each component, place below 5 ℃ to store for future use, wherein the weight ratio of epoxy resin, curing agent, auxiliary agent and filler is 20: 3: 3: 4.
Preferably, described organic solvent is selected from dimethylbenzene, toluene, benzene or acetone.
Preferably, described curing agent is a pyromellitic dianhydride.
Preferably, described auxiliary agent is a tertiary amine.
Preferably, described filler is selected flake asbestos, aluminium powder or titanium dioxide for use.
The coating layer thickness of the extracting fiber that employing the method for the invention makes is 10-2000 μ m.
The beneficial effect that the present invention had:
The present invention utilizes synthetic high-temperature-resistant epoxy resin or organic siliconresin that the Tenax adsorbent is fixed on the metallic fiber surface, obtains extracting fiber, forms Heat stability is good, thus anti-solvent washing coating material realize enrichment to trace organic substance.Replace traditional quartz fibre to make it have higher mechanical strength with metallic fiber; Adsorbent is attached to form on the metallic fiber, is convenient to adsorbent the static head space of sample is captured.Be applicable to processing to samples such as soil, atmosphere, essence and flavoring agent, room air, alcohol, phenol, amine aldehyde, ketone, halogenated aryl hydrocarbons.
Description of drawings:
Fig. 1 is not for using the gas-chromatography baseline chart of extracting fiber;
Fig. 2 is for using the gas-chromatography baseline chart under the embodiment 1 extracting fiber desorption temperature;
Fig. 3 is for utilizing the gas chromatogram of embodiment 1 extracting fiber extraction n-alkane (C8-C15).
The specific embodiment
In order to understand the present invention, further specify the present invention with embodiment below, but do not limit the present invention.
Comparison diagram 1 and Fig. 2 can draw, and can cause the loss of coating under desorption temperature hardly.As can be seen from Figure 3, visible extracting fiber of the present invention has the good adsorption performance to organic matter, is particularly suitable for the quick collection of trace, trace organic substance in soil, atmosphere, essence and flavoring agent, the room air sample and qualitative.
Embodiment 1
Choose long 20mm, diameter is the stainless steel fibre of 0.35mm, utilizes dense HF to corrode 10-60min, takes out, and distilled water flushing utilizes N2 to dry up to neutral; Take by weighing 100g epoxy resin, add dimethylbenzene and be stirred to dissolving fully, add 15g pyromellitic dianhydride, 15g tertiary amine, 20g flake asbestos more successively, stirring is uniformly dispersed each component, makes high-temperature-resistant epoxy resin; With the surface-coated one deck high-temperature-resistant epoxy resin of the stainless steel fibre of handling, pick one deck TenaxTA at skin again, place in the baking oven in 180 ℃ of hot setting 60min; With the extracting fiber that is cured, place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min, make the extracting fiber finished product.
Wherein epoxy resin is multifunctional glycidol type epoxy resin, and market is bought and obtained.
Embodiment 2
Choose long 20mm, diameter is the stainless steel fibre of 0.35mm, utilizes dense HF to corrode 10-60min, takes out, and distilled water flushing utilizes N2 to dry up to neutral; At the surface-coated one deck high temperature of the stainless steel fibre of handling organic siliconresin, pick one deck 2 at skin again, 6-dibenzofuran porous polymeric resins places in the baking oven in 180 ℃ of hot setting 60min.With the extracting fiber that is cured, place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min, make the extracting fiber finished product.
Embodiment 3
Utilize the extracting fiber of making among the embodiment 1 that aldehydes matter in the water is analyzed, take the immersion mode to extract.
Embodiment 4
Utilize the extracting fiber of making among the embodiment 2 that meat flavor is fragrant component analysis, 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 (9)
1. metallic carrier Tenax coating solid phase micro-extraction fiber, coating by carrier and surface thereof is formed, it is characterized in that, described carrier is long 10-40mm, diameter is the metallic fiber of 0.1-0.5mm, described coating comprises the Tenax adsorbent, also comprises high-temperature-resistant epoxy resin layer or silicone resin layer.
2. metallic carrier Tenax coating solid phase micro-extraction fiber is characterized in that this extracting fiber is prepared by the method that comprises following 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, distilled water flushing utilizes N to neutral
2Dry up;
(b), at the surface-coated one deck high-temperature-resistant epoxy resin or the organic siliconresin of the metallic fiber of handling through step (a), pick one deck Tenax adsorbent at skin again, coating or adjust coating layer thickness by repeating step (b);
(c), the metallic fiber of coated coating is placed carry out hot setting in the baking oven;
(d), extracting fiber that hot setting is good, place in the middle of the cable type extractor according, utilize carrene in 40-80 ℃ of backflow 20-120min, to remove impurity.
3. metallic carrier Tenax coating solid phase micro-extraction fiber according to claim 1 and 2 is characterized in that described metallic fiber is stainless steel fibre or alloy fiber.
4. metallic carrier Tenax coating solid phase micro-extraction fiber according to claim 1 and 2 is characterized in that described Tenax adsorbent is 2,6-dibenzofuran porous polymeric resins.
5. metallic carrier Tenax coating solid phase micro-extraction fiber according to claim 1 and 2, it is characterized in that, the synthetic method of described high-temperature-resistant epoxy resin is stirred to dissolving fully for add organic solvent in epoxy resin, add curing agent, auxiliary agent and filler more successively, stirring is uniformly dispersed each component, place below 5 ℃ to store for future use, wherein the weight ratio of epoxy resin, curing agent, auxiliary agent and filler is 20: 3: 3: 4.
6. metallic carrier Tenax coating solid phase micro-extraction fiber according to claim 5 is characterized in that described organic solvent is selected from dimethylbenzene, toluene, benzene or acetone.
7. metallic carrier Tenax coating solid phase micro-extraction fiber according to claim 5 is characterized in that described curing agent is a pyromellitic dianhydride.
8. metallic carrier Tenax coating solid phase micro-extraction fiber according to claim 5 is characterized in that described auxiliary agent is a tertiary amine.
9. metallic carrier Tenax coating solid phase micro-extraction fiber according to claim 5 is characterized in that described filler is selected flake asbestos, aluminium powder or titanium dioxide for use.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010270682XA CN101992073A (en) | 2010-09-02 | 2010-09-02 | Metal carrier Tenax coating solid-phase microextraction fiber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010270682XA CN101992073A (en) | 2010-09-02 | 2010-09-02 | Metal carrier Tenax coating solid-phase microextraction fiber |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105699569A (en) * | 2016-03-10 | 2016-06-22 | 上海福劳斯检测技术有限公司 | Self-cleaning type thermal-desorption gas chromatographic system for online total hydrocarbon analysis |
| CN108034055A (en) * | 2017-12-29 | 2018-05-15 | 中国烟草总公司郑州烟草研究院 | A kind of covalent organic framework solid-phase micro-extraction fibre and preparation method thereof |
| CN108079979A (en) * | 2017-12-15 | 2018-05-29 | 晋江瑞碧科技有限公司 | The preparation method of perforated activity carbon film coating solid phase micro-extracting head |
-
2010
- 2010-09-02 CN CN201010270682XA patent/CN101992073A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105699569A (en) * | 2016-03-10 | 2016-06-22 | 上海福劳斯检测技术有限公司 | Self-cleaning type thermal-desorption gas chromatographic system for online total hydrocarbon analysis |
| CN108079979A (en) * | 2017-12-15 | 2018-05-29 | 晋江瑞碧科技有限公司 | The preparation method of perforated activity carbon film coating solid phase micro-extracting head |
| CN108079979B (en) * | 2017-12-15 | 2020-06-09 | 武夷学院 | Preparation method of solid-phase micro-extraction head with multi-layer porous active carbon film coating |
| CN108034055A (en) * | 2017-12-29 | 2018-05-15 | 中国烟草总公司郑州烟草研究院 | A kind of covalent organic framework solid-phase micro-extraction fibre and preparation method thereof |
| CN108034055B (en) * | 2017-12-29 | 2021-04-06 | 中国烟草总公司郑州烟草研究院 | Covalent organic framework solid phase micro-extraction fiber and preparation method thereof |
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Application publication date: 20110330 |