CN102114417A - Preparation method of stainless steel solid-phase microextraction fiber - Google Patents
Preparation method of stainless steel solid-phase microextraction fiber Download PDFInfo
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- CN102114417A CN102114417A CN 201010512235 CN201010512235A CN102114417A CN 102114417 A CN102114417 A CN 102114417A CN 201010512235 CN201010512235 CN 201010512235 CN 201010512235 A CN201010512235 A CN 201010512235A CN 102114417 A CN102114417 A CN 102114417A
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Abstract
The invention provides a preparation method of a stainless steel solid-phase microextraction (SPME) fiber. An absorbent is fixed on the surface of a stainless steel fiber by using synthetic high-temperature epoxy resin or organic silicon resin, wherein the absorbent is a liquid chromatogram silicon gel or chromatogram stationary phase bonded with one or more of C1 to C18, phenyl, phenmethyl, cyan, diol and amino; a coating material with good thermal stability and solvent washing resistance is formed, therefore, trace organic matters are enriched. The traditional quartz fiber is replaced with stainless steel fiber to ensure that the stainless steel solid-phase microextraction fiber has higher mechanical strength. The manner that the absorbent is combined to the extraction fiber is convenient for the absorbent to carry out static headspace collection on a sample. The invention is especially suitable for analyzing organic matters such as arene compounds, polycyclic aromatic hydrocarbon and the like; and compared with the conventional SPME solid phase coating, the stainless steel solid-phase microextraction fiber has the characteristics of large surface area, easiness for reaching balance and improved 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 preparation method 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 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, and the ability of anti-organic solvent flushing and anti-PH, high temperature resistant, salt tolerant, costs an arm and a leg
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and use on stainless steel fibre that new coating material prepares that selectivity is good, extraction efficiency is high, the method for the solid-phase micro-extraction fibre of good operation performance, long service life.
The technical scheme that the present invention takes is: a kind of preparation method of 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 N2 to dry up to neutral.
2) making of extracting fiber coating: 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 to solidification temperature and time of selected High temp. epoxy resins or organic siliconresin, 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, to remove the small molecular weight impurity in the coating in 40-80 ℃ of backflow 20-120min.
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.
Be preferably 100 parts of epoxy resin, 15 parts of pyromellitic dianhydrides, 15 parts of tertiary amines, 20 parts of flake asbestos, solvent is selected dimethylbenzene for use.
Further, before step 3, repetitive operation step 2 once more than.
Further, dense HF erosion time is 25-35min in the step 1; Synthetic high-temperature-resistant epoxy resin raw material and raw material weight ratio are epoxy resin 90-110 part, pyromellitic dianhydride 10-20 part, tertiary amine 10-20 part, flake asbestos 15-25 part in the step 2; Covering C18 bonded silica gel thickness is the 25-35 micron; Temperature hardening time in the step 3 is 160-200 ℃, and be 50-70min hardening time; Reflux temperature in the step 4 is 50-70 ℃, and return time is 30-50min.
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 selectivity and repeatability.
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.
The gas-chromatography baseline chart that does not use 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.
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 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 (4)
1. the preparation method of a stainless steel solid-phase micro-extraction fibre is characterized in that, comprises following 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) making of extracting fiber coating: 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 to solidification temperature and time of selected High temp. epoxy resins or organic siliconresin, 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, to remove the small molecular weight impurity in the coating in 40-80 ℃ of backflow 20-120min.
2. the preparation method of stainless steel solid-phase micro-extraction fibre according to claim 1, it is characterized in that: the synthetic method of high-temperature-resistant epoxy resin described in the step 2 is, take by weighing an amount of epoxy resin, add stirring solvent to dissolving fully, add curing agent, auxiliary agent, filler more successively, stirring is uniformly dispersed each component, 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.
3. the preparation method of stainless steel solid-phase micro-extraction fibre according to claim 1 and 2 is characterized in that: before step 3, repetitive operation step 2 once more than.
4. the preparation method of stainless steel solid-phase micro-extraction fibre according to claim 1 and 2 is characterized in that:
Dense HF erosion time is 25-35min in the step 1;
Synthetic high-temperature-resistant epoxy resin raw material and raw material weight ratio are epoxy resin 90-110 part, pyromellitic dianhydride 10-20 part, tertiary amine 10-20 part, flake asbestos 15-25 part in the step 2; Covering C18 bonded silica gel thickness is the 25-35 micron;
Temperature hardening time in the step 3 is 160-200 ℃, and be 50-70min hardening time;
Reflux temperature in the step 4 is 50-70 ℃, and return time is 30-50min.
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| CN 201010512235 CN102114417A (en) | 2010-10-19 | 2010-10-19 | Preparation method of stainless steel solid-phase microextraction fiber |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102631900A (en) * | 2012-04-11 | 2012-08-15 | 中国科学院化学研究所 | Method for rapidly preparing solid-phase microextraction fiber coating |
| 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 |
| CN107583629A (en) * | 2017-09-08 | 2018-01-16 | 中山大学 | Solid phase micro extraction probe prepared using octaphenyl cage-type silsesquioxane as material and its preparation method and application |
-
2010
- 2010-10-19 CN CN 201010512235 patent/CN102114417A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102631900A (en) * | 2012-04-11 | 2012-08-15 | 中国科学院化学研究所 | Method for rapidly preparing solid-phase microextraction fiber coating |
| 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 |
| CN107583629A (en) * | 2017-09-08 | 2018-01-16 | 中山大学 | Solid phase micro extraction probe prepared using octaphenyl cage-type silsesquioxane as material and its preparation method and application |
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Application publication date: 20110706 |