CN102068963B - Stainless steel solid phase micro extraction fiber - Google Patents
Stainless steel solid phase micro extraction fiber Download PDFInfo
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- CN102068963B CN102068963B CN 201010510043 CN201010510043A CN102068963B CN 102068963 B CN102068963 B CN 102068963B CN 201010510043 CN201010510043 CN 201010510043 CN 201010510043 A CN201010510043 A CN 201010510043A CN 102068963 B CN102068963 B CN 102068963B
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Abstract
The invention provides a stainless steel solid phase micro extraction fiber. Adsorbent is fixed on the surface of the stainless steel fiber by utilizing synthetic high-temperature epoxy resin or organic silicon resin; and the adsorbent is a liquid-chromatography silica gel or chromatographic stationary-phase silica gel which is bonded with one or more of C1 to C18, phenyl, benzyl, cyan, diol and amino, and forms a coating material with good heat stability and solvent flushing resistance so as to enrich trace-level organic compounds. The stainless steel fibers are adopted instead of the traditional quartz fibers, thus the extraction fiber has higher mechanical strength; and the adsorbent is combined on the extraction fiber, thereby being convenient for static headspace capture of samples. The stainless steel solid phase micro extraction fiber is particularly applicable to analysis of organic compounds such as aromatic compounds, polycyclic aromatic hydrocarbons and the like in water; and compared with the conventional SPME (Solid-Phase Micro-Extraction) coating, the coating in the invention is characterized by large surface area, easy balance and capability of improving the detection sensitivity.
Description
Technical field
The present invention relates to organic trace analysis field in food, environment, the biological sample, particularly relate to a kind of stainless steel 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 one 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 one pipe of auto injection; 1997, Nguyen etc. realized the on-line coupling of SPME one 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 with gas-chromatography gas-chromatography, high performance liquid chromatography, gas chromatography mass spectrometry, Capillary Electrophoresis etc. the advantage of Instrument crosslinkings.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 SPME the earliest (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, and the ability of anti-organic solvent flushing and anti-PH, high temperature resistant, salt tolerant, and is expensive
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of stainless steel fibre use new coating material preparation selectively good, extraction efficiency is high, the solid-phase micro-extraction fibre of good operation performance, long service life and preparation method thereof.
The technical scheme that the present invention takes is:
A kind of stainless steel solid-phase micro-extraction fibre, comprise stainless steel fibre, with the adsorbent coating, it is characterized in that: described adsorbent coating is that bonding has one or more liquid-phase chromatographic silica gel or the chromatographic grade fixedly phase of C1 in C18, phenyl, benzyl, cyano group, glycol-based, the amino, and the fire resistant resin layer is arranged in the middle of described adsorbent coating and the stainless steel fibre.
Further, described fire resistant resin is High temp. epoxy resins or organic siliconresin.
Further, described adsorbent coating is at least 2 layers, and the fire resistant resin layer is arranged in the middle of the adsorbent coating.
Wherein, the preparation method of above-mentioned extracting fiber comprises the steps:
1) choosing and preliminary treatment of solid-phase micro-extraction fibre: choose long 10-40mm, diameter is the stainless steel fibre of 0.1-0.5mm, utilizes dense HF to corrode 10-60min, takes out, and distilled water flushing utilizes N2 to dry up to neutral.
2) making of extracting fiber coating: the surface-coated one deck High temp. epoxy resins of the extracting fiber that will handle or organic siliconresin earlier, pick one deck adsorbent at skin again, described adsorbent is that bonding has one or more liquid-phase chromatographic silica gel or the chromatographic grade fixedly phase of C1 in C18, phenyl, benzyl, cyano group, glycol-based, the amino.
3) curing of coating is handled: according to the requirement of selected High temp. epoxy resins to solidification temperature and time, coated stainless steel fibre placed carry out hot setting in the baking oven.
4) removal of extracting fiber impurity: with the extracting fiber of making, place in the middle of the cable type extractor according, utilize carrene in 40-80 ℃ of backflow 20-120min, to remove the small molecular weight impurity in adsorbent and the epoxy resin.
Further, the synthetic method of high-temperature-resistant epoxy resin described in the step 2 is, takes by weighing an amount of epoxy resin, adds stirring solvent to dissolving fully, adds curing agent, auxiliary agent, filler more successively, stirs each component is uniformly dispersed, and places below 5 ℃ to store for future use; Described solvent is selected a kind of in dimethylbenzene, toluene, benzene, the acetone and other organic solvent for use; Described curing agent is selected a kind of in the acid anhydrides type agent such as pyromellitic dianhydride for use; Filler is selected a kind of in flake asbestos, aluminium powder, the titanium dioxide for use.
Further, before step 3, repetitive operation step 2 once more than.
The invention has the beneficial effects as follows: utilize synthesizing high temperature epoxy resin or organic siliconresin that adsorbent is fixed on the stainless steel fibre surface, form Heat stability is good, thereby anti-solvent washing coating material realize enrichment to trace organic substance.Adsorbent is attached to form on the extracting fiber, is convenient to adsorbent the static head space of sample is captured.Be specially adapted to organic components such as arene compound in the branch bleed and polycyclic aromatic hydrocarbon, with the SPME solid phase coating of routine relatively, the characteristics of this coating are that surface area is big, are easy to reach balance, can make detection sensitivity improve.Simultaneously, in many food analyses, environmental analysis experiment, show good selective and repeated.
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 of embodiment 1 preparation
Fig. 3 is the gas chromatogram of the extracting fiber extracting polyaromatic hydrocarbon of embodiment 1 preparation
The specific embodiment
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 N to neutral
2Dry up.Take by weighing an amount of epoxy resin, add dimethylbenzene and be stirred to dissolving fully, add pyromellitic dianhydride, tertiary amine, flake asbestos more successively, stirring is uniformly dispersed each component.With the surface-coated one deck High temp. epoxy resins of the stainless steel fibre of handling, pick one deck C18 at skin again, place in the baking oven in 180 ℃ of hot setting 60min.With the fiber of making, place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min.
Utilize the stainless steel fibre of making among the embodiment 1 that aldehydes matter in the environmental water sample is analyzed, take the immersion mode to extract.
Do not use the gas-chromatography baseline chart of extracting fiber as shown in Figure 1, the gas-chromatography baseline chart under the extracting fiber desorption temperature as shown in Figure 2, the gas chromatogram of extracting fiber extracting polyaromatic hydrocarbon is as shown in Figure 3.
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 N to neutral
2Dry up.With the surface-coated one deck high temperature of the stainless steel fibre of handling organic siliconresin, pick one deck C18 at skin again, place in the baking oven in 180 ℃ of hot setting 60min.With the fiber of making, place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min.
Utilize the stainless steel fibre of making among the embodiment 2 that perfume ingredient is fragrant and analyze, take the head space mode to extract.
Other embodiment:
Claims (2)
1. the preparation method of a stainless steel solid-phase micro-extraction fibre comprises the steps:
1), choosing and preliminary treatment of solid-phase micro-extraction fibre: choose long 10-40mm, diameter is the stainless steel fibre of 0.1-0.5mm, utilizes dense HF to corrode 10-60min, takes out, and distilled water flushing utilizes N to neutral
2Dry up;
2), the making of extracting fiber coating: the surface-coated one deck high-temperature-resistant epoxy resin of the extracting fiber that will handle earlier, pick one deck adsorbent at skin again, described adsorbent is that bonding has one or more liquid-phase chromatographic silica gel or the chromatographic grade fixedly phase of C1 in C18, phenyl, benzyl, cyano group, glycol-based, the amino; The synthetic method of described high-temperature-resistant epoxy resin is, takes by weighing an amount of epoxy resin, adds stirring solvent to dissolving fully, adds curing agent, auxiliary agent, filler more successively, stirs each component is uniformly dispersed, and places below 5 ℃ to store for future use; Described solvent is selected a kind of in dimethylbenzene, toluene, benzene, the acetone for use; Described curing agent is pyromellitic dianhydride; Filler is selected a kind of in flake asbestos, aluminium powder, the titanium dioxide for use;
3), the curing of coating handles: according to the requirement of selected High temp. epoxy resins to solidification temperature and time, coated stainless steel fibre placed carry out hot setting in the baking oven;
4), the removal of extracting fiber impurity: with the extracting fiber of making, place in the middle of the cable type extractor according, utilize carrene in 40-80 ℃ of backflow 20-120min, to remove the small molecular weight impurity in adsorbent and the epoxy resin.
2. the preparation method of stainless steel solid-phase micro-extraction fibre according to claim 1, it is characterized in that: described adsorbent coating is at least 2 layers, and the fire resistant resin layer is arranged in the middle of the adsorbent coating.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108579708A (en) * | 2018-04-28 | 2018-09-28 | 江南大学 | A kind of polycyclic aromatic hydrocarbon enrichment detection solid-phase micro-extraction fibre and production method |
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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 |
| CN107096516A (en) * | 2017-05-18 | 2017-08-29 | 安徽众诚环境检测有限公司 | A kind of water quality detection solid-phase micro-extraction coating optical fiber and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1500540A (en) * | 2002-11-15 | 2004-06-02 | 中国科学院大连化学物理研究所 | Capillary solid phase microextraction device and extracting method |
| CN1951577A (en) * | 2005-10-19 | 2007-04-25 | 中国科学院大连化学物理研究所 | Preparation method of solid phase micro-extraction coat layer |
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| CN101496958B (en) * | 2009-01-14 | 2011-03-16 | 南开大学 | Solid phase micro-extraction device and method for preparing fibre extraction head thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1500540A (en) * | 2002-11-15 | 2004-06-02 | 中国科学院大连化学物理研究所 | Capillary solid phase microextraction device and extracting method |
| CN1951577A (en) * | 2005-10-19 | 2007-04-25 | 中国科学院大连化学物理研究所 | Preparation method of solid phase micro-extraction coat layer |
Non-Patent Citations (2)
| Title |
|---|
| Porous Layer Solid Phase Microextraction Using Silica Bonded Phases;Yu Liu et al.;《Anal. Chem.》;19970115;第69卷;第190页左栏第1-6行，第191页左栏第4段，表1，2 * |
| Yu Liu et al..Porous Layer Solid Phase Microextraction Using Silica Bonded Phases.《Anal. Chem.》.1997,第69卷第190-195页. |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108579708A (en) * | 2018-04-28 | 2018-09-28 | 江南大学 | A kind of polycyclic aromatic hydrocarbon enrichment detection solid-phase micro-extraction fibre and production method |
| CN108579708B (en) * | 2018-04-28 | 2020-03-06 | 江南大学 | Solid-phase micro-extraction fiber for polycyclic aromatic hydrocarbon enrichment detection and manufacturing method thereof |
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