CN101992062B - Method for preparing metal carrier stirring extraction rod - Google Patents
Method for preparing metal carrier stirring extraction rod Download PDFInfo
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- CN101992062B CN101992062B CN 201010270672 CN201010270672A CN101992062B CN 101992062 B CN101992062 B CN 101992062B CN 201010270672 CN201010270672 CN 201010270672 CN 201010270672 A CN201010270672 A CN 201010270672A CN 101992062 B CN101992062 B CN 101992062B
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Abstract
The invention discloses a method for preparing a metal carrier stirring extraction rod, and relates to the field of trace analysis of organic matters in foods, environment and biological samples. The method comprises the following steps of: (a) selecting a metal rod with the length of 10 to 40mm and the diameter of 0.5 to 5mm, and performing surface pretreatment; and (b) coating a layer of heat-resistant epoxy resin or organic silicon resin on the surface of the metal rod subjected to surface pretreatment, and dipping a layer of adsorbent on the outer layer to obtain a coat, or repeatedly coating and dipping to adjust the thickness of the coat, wherein the adsorbent is one ore more of graphitized carbon black, silica gel and clay. The stirring extraction rod prepared by the method has high mechanical strength, is firm and durable, is favorable for the adsorbent to perform treatment on a liquid sample and static headspace capture, 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 stirs the preparation method of extraction bar.
Background technology
Because the matrix of most of analytic sample is quite complicated with composition, sample pre-treatments becomes important step indispensable in the sample analysis under normal conditions.It plays and concentrates tested trace components, the effect of sensitivity of raising method and cleaning sample.
Traditional sample-pretreating method has liquid-liquid extraction, soxhlet extraction, chromatography, distillation, absorption, centrifugal and filtration etc., but these methods generally have and use a large amount of organic solvents, the processing time is long and operating procedure is many shortcoming.These methods are not only lost sample easily, are produced than mistake, and the use of toxic solvent can influence operator ' s health, contaminated environment.For this reason, the research of the sample-pretreating method that solvent-free or few solvent, the degree of accuracy are high, quick, easy has become one of forward position research topic of current analytical chemistry.
Solid phase micro-extraction technique (Solid Phase Micro Extraction; SPME) be the sample pre-treatments and the beneficiation technologies of a novelty of the rise nineties in 20th century; It developed research by the Pawliszyn professor's of Canadian Waterloo university research group in 1989 at first first, belonged to non-solvent selective extraction method.It almost can be used for the analysis of all kinds of volatility of sample such as gas, liquid, biology, solid or half volatile material.The maximum characteristics of SPME integrate sampling, extraction, enrichment, sample introduction exactly; Thereby it is easy and simple to handle; And do not need solvent; Rate of extraction is fast, running cost is low, free from environmental pollution, be convenient to realize automation and be easy to and high efficiency separation detection means couplings such as chromatogram, electrophoresis, therefore, in chemistry, medicine, food, environmental area and Pharmaceutical Analysis, obtained using widely.
(Stir bar sorptive extraction SBSE) is proposed in 1999 by people such as Erik Baltussen Stir Bar Sorptive Extraction, is a kind of novel sample pre-treatments technology that on the SPME basis, grows up.This technology is the same with SPME have simple, efficient, fast, favorable reproducibility, green advantage such as solvent-free; And absorption stirring rod self is accomplished stirring in extraction process; Avoided the competitive Adsorption of stirrer in Fiber SPME; And its extraction fixedly the volume ratio SPME of phase is big more than 50 times, so the enrichment multiple obviously improves very suitable trace analysis.Abroad should technology successfully be applied to the analysis of pollutant, drugs, medicine and residues of pesticides in environmental sample, the food, human endocrine interfering material, polycyclic aromatic hydrocarbon, benzene series thing and Polychlorinated biphenyls etc.
Germany Gerstel GnlbH company selects for use dimethyl silicone polymer (PDMS) as the extraction coating, has released commercial stirring rod (Twister Gerstel GnlbH).Twister is the PDMS silicone rubber tube by 0.5mm or 1mm, is enclosed within on the glass tube that seals magnetic core in to process.
Commercial SBSE device is a carrier with the glass bar, and material is frangible, and has only this a kind of fixedly phase coating of PDMS, and commercialization SBSE device price is higher, and the SBSE The Application of Technology has received bigger restriction.For this reason, be the work that an extremely has novelty and practical significance to the SBSE Study on Technology.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of metallic carrier to stir the preparation method of extraction bar, the stirring extraction bar that makes is used for trace analysis, is particularly suitable in the branch bleed and airborne trace contaminant.
Technical scheme of the present invention is following:
A kind of metallic carrier stirs the preparation method of extraction bar, and this method comprises the steps:
(a) choose long 10-40mm, diameter is the metal bar of 0.5-5mm, carries out surface preparation;
(b) elder generation is at the surface-coated one deck high-temperature-resistant epoxy resin or the organic siliconresin of the metal bar 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.
Preferably, a kind of metallic carrier stirs the preparation method of extraction bar, and this method comprises the steps:
(a) choose long 10-40mm, diameter is the metal bar of 0.5-5mm, with dichloromethane solvent preliminary treatment is carried out on its surface;
(b) elder generation is at the surface-coated one deck high-temperature-resistant epoxy resin or the organic siliconresin of the metal bar 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 stirring extraction bar that (c) will coat coating places and carries out hot setting in the baking oven;
(d) stirring extraction bar that hot setting is good places cable type extractor according, with carrene in 40-80 ℃ of backflow 20-120min, to remove impurity.
Preferably, use with alr mode, said metal bar is that iron staff, nickel rod, cobalt are excellent, a kind of in stainless steel bar or the alloy bar; Use with head space or ultrasonic power, said metal bar is a kind of in stainless steel bar, copper rod, aluminium bar or the alloy bar.
Preferably, said adsorbent is a ketjenblack EC, further is preferably Carbograph.
Preferably, the synthetic method of said high-temperature-resistant epoxy resin is stirred to dissolving fully in epoxy resin, adding organic solvent, adds curing agent, auxiliary agent and filler more successively; Stirring is uniformly dispersed each component, prepares high-temperature-resistant epoxy resin, and wherein the consumption of each material does; Calculate 20 parts of epoxy resin, 3 parts in curing agent by weight; 3 parts of auxiliary agents, 4 parts of fillers place below 5 ℃ to store for future use.
Preferably, said organic solvent is a kind of in xylenes, toluene, benzene or the acetone; Said curing agent is the agent of acid anhydrides type; Said auxiliary agent is a tertiary amine; Said filler is a kind of in flake asbestos, aluminium powder or the titanium white powder.
Preferably, said curing agent is a pyromellitic dianhydride.
The coating layer thickness of the stirring extraction bar that preparation method of the present invention makes is 10-5000 μ m.
The beneficial effect that the present invention had is:
The present invention is carrier with the metal bar; Utilize synthetic high-temperature-resistant epoxy resin or organic siliconresin that adsorbent is fixed on the metal bar surface, make the stirring extraction bar, this stirs the coating Heat stability is good of extraction bar; Anti-solvent washing, thus realize enrichment to trace organic substance.The characteristics of the stirring extraction bar that makes are porous surfaces, and heat endurance is high, does not keep water, and adsorption capacity is big.Barred body self is accomplished and is stirred in extraction process, has avoided the competitive Adsorption of stirrer in Fiber SPME; Replace the conventional glass rod to make it have higher mechanical strength, sturdy and durable with metal bar; Adsorbent is attached to the form that stirs on the extraction bar, more helps adsorbent the processing of fluid sample and static head space are captured; 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 that stirs extraction bar;
Fig. 2 is the gas-chromatography baseline chart under the stirring extraction bar desorption temperature that uses embodiment 1 method and make;
Fig. 3 is the gas chromatogram that utilizes the stirring extraction bar extraction benzene series thing that embodiment 1 method makes.
1 is benzene among Fig. 3, 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.
Comparison diagram 1 can draw with Fig. 2; Under desorption temperature, can cause the loss of coating hardly; It is thus clear that the stirring extraction bar crosslinking degree of the present invention's preparation is fine, nothing runs off; Fig. 3 is the gas chromatogram that utilizes the stirring extraction bar extraction benzene series thing that embodiment 1 method makes, and the stirring extraction bar of visible the present invention's preparation is particularly suitable for the detection of trace, contaminant trace species in the environment.
Embodiment 1
Choose long 25mm, diameter is the iron staff of 2mm, utilizes carrene that preliminary treatment is carried out on its surface.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 pretreated barred body; Pick one deck Carbograph at skin again, place baking oven interior, the stirring extraction bar that hot setting is good in 180 ℃ of hot setting 60min; Place in the middle of the cable type extractor according, with carrene in 60 ℃ of backflow 40min.
Wherein epoxy resin is multifunctional glycidol type epoxy resin, and market is bought and obtained.
Choose long 25mm, diameter is the nickel rod of 2mm, utilizes carrene that preliminary treatment is carried out on its surface.At the surface-coated one deck organic siliconresin of pretreated barred body; Pick one deck Carbograph at skin again, place in the baking oven in 180 ℃ of hot setting 60min, with the stirring extraction bar of making; Place in the middle of the cable type extractor according, with carrene in 60 ℃ of backflow 40min.
Choose long 25mm, diameter is the stainless steel bar of 2mm, utilizes carrene that preliminary treatment is carried out on its surface.At the surface-coated one deck organic siliconresin of pretreated barred body; Pick one deck clay at skin again, place in the baking oven in 180 ℃ of hot setting 60min, with the stirring extraction bar of making; Place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min.
Utilize the stirring extraction bar of making among the embodiment 1 that all kinds of organic substances in the river are analyzed, take to stir the extraction mode, the solvent method desorb.
Utilize the stirring extraction bar of making among the embodiment 1 that the fruit essence component is fragrant and analyze, take the head space mode to extract, the desorb of thermal desorption method.
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 (5)
1. the preparation method of a metallic carrier stirring extraction bar is characterized in that this method comprises the steps:
(a) choose long 10-40mm, diameter is the metal bar of 0.5-5mm, with dichloromethane solvent preliminary treatment is carried out on its surface;
(b) elder generation is at the surface-coated one deck high-temperature-resistant epoxy resin or the organic siliconresin of the metal bar of process surface preparation; Pick one deck adsorbent at skin again; Said adsorbent be ketjenblack EC, silica gel or affix in one or more, coating or repeat to be coated with stain and pick and adjust coating layer thickness;
The stirring extraction bar that (c) will coat coating places and carries out hot setting in the baking oven;
(d) stirring extraction bar 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 according to claim 1 stirs the preparation method of extraction bar, it is characterized in that: use with alr mode, said metal bar is iron staff, nickel rod, cobalt is excellent or alloy bar in a kind of; Use with head space or ultrasonic power, said metal bar is a kind of in copper rod, aluminium bar or the alloy bar.
3. a kind of metallic carrier according to claim 2 stirs the preparation method of extraction bar, it is characterized in that: use with alr mode, said metal bar is iron staff, nickel rod, cobalt is excellent or stainless steel bar in a kind of; Use with head space or ultrasonic power, said metal bar is a kind of in copper rod, aluminium bar or the alloy bar.
4. a kind of metallic carrier according to claim 1 and 2 stirs the preparation method of extraction bar, and it is characterized in that: said adsorbent is a ketjenblack EC.
5. a kind of metallic carrier according to claim 1 and 2 stirs the preparation method of extraction bar, 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, adds curing agent, auxiliary agent and filler more successively; Stirring is uniformly dispersed each component, prepares high-temperature-resistant epoxy resin, and wherein the consumption of each material does; Calculate by weight; 20 parts of epoxy resin, 3 parts in curing agent, 3 parts of auxiliary agents; 4 parts of fillers place below 5 ℃ to store for future use.
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| CN 201010270672 CN101992062B (en) | 2010-09-02 | 2010-09-02 | Method for preparing metal carrier stirring extraction rod |
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| CN 201010270672 CN101992062B (en) | 2010-09-02 | 2010-09-02 | Method for preparing metal carrier stirring extraction rod |
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| CN101992062B true CN101992062B (en) | 2012-09-05 |
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| CN110115991A (en) * | 2018-02-06 | 2019-08-13 | 爱普香料集团股份有限公司 | A kind of preparation and application method of GC/MS joint thermal desorption Solid Phase Extraction stick |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239302A (en) * | 2008-03-11 | 2008-08-13 | 中山大学 | Extraction head of carbon nano-tube solid phase micro-extraction and preparation thereof |
| CN101532993A (en) * | 2009-04-11 | 2009-09-16 | 吉林化工学院 | Method used for analyzing and detecting organic trace impurity in high-purity phenol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7259019B2 (en) * | 2002-03-11 | 2007-08-21 | Pawliszyn Janusz B | Multiple sampling device and method for investigating biological systems |
| WO2009144725A1 (en) * | 2008-05-29 | 2009-12-03 | Technion Research And Development Foundation Ltd. | Carbon nanotube structures in sensor apparatuses for analyzing biomarkers in breath samples |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101239302A (en) * | 2008-03-11 | 2008-08-13 | 中山大学 | Extraction head of carbon nano-tube solid phase micro-extraction and preparation thereof |
| CN101532993A (en) * | 2009-04-11 | 2009-09-16 | 吉林化工学院 | Method used for analyzing and detecting organic trace impurity in high-purity phenol |
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