CN101757898B - Preparation method of titanium oxide extraction bar for solid phase microextraction - Google Patents
Preparation method of titanium oxide extraction bar for solid phase microextraction Download PDFInfo
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- CN101757898B CN101757898B CN2008101844793A CN200810184479A CN101757898B CN 101757898 B CN101757898 B CN 101757898B CN 2008101844793 A CN2008101844793 A CN 2008101844793A CN 200810184479 A CN200810184479 A CN 200810184479A CN 101757898 B CN101757898 B CN 101757898B
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- titanium oxide
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- extraction bar
- hollow fiber
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Abstract
The invention discloses a preparation method of a titanium oxide extraction bar for solid phase microextraction; in the method, a plurality of titanium oxide layers are deposited on the surface of polypropylene hollow fiber by adopting a sol-gel method, and then polypropylene matrix is removed by high-temperature firing, so as to obtain the titanium oxide hollow fiber extraction bar, realize extraction preenrichment to polar compounds with micro and trace amount in medicine and environment samples and carry out separation analysis to gas chromatography or high performance liquid chromatography; the extraction bar has a three-dimensional porous stricture, has larger specific surface area, controllable coating thickness, good chemical and heat stability, wide pH stabilization range (pH=1-14) and high extraction efficiency to the polar compounds.
Description
Technical field
The present invention relates to the preparation method of the novel titanium oxide doughnut of a kind of solid-phase microextraction extraction bar, particularly a kind of preparation method who is used for the titanium oxide doughnut extraction bar of sample trace such as food, medicine, environment, inspection and quarantine and trace polar compound extraction preenrichment.
Background technology
SPME (SPME) (R.P, Belardi and Pawlisyn, Water Pollution Research J.Canada.1989,24,179) has developed into a kind of ripe relatively sample pretreatment technology.This technology centralized procurement sample, extraction, concentrate and sample introduction in one, it is few to have amount of samples, hardly with an organic solvent, is easy to other analytical instrument couplings, easy and simple to handle fast, install many advantages such as small and exquisite and be widely used in various sample detection.Yet up to the present, the coating kind of solid phase micro-extraction extraction head is limited, and serviceability temperature is on the low side (200～280 ℃), and a little less than the anti-solvent washing ability, service life is short, frangibility, and the extracting and enriching multiple is low, has limited its range of application greatly.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of titanium oxide extraction bar for solid phase microextraction.
For achieving the above object, the technical solution adopted in the present invention is as follows:
The preparation method of titanium oxide extraction bar for solid phase microextraction of the present invention, adopt the surface deposition multilayer titanium oxide of sol-gal process at polypropylene hollow fiber, high temperature sintering is removed polypropylene-base then, obtain titanium oxide doughnut extraction bar, realizing extraction preenrichment, and finish compartment analysis by gas-chromatography or efficient liquid phase to trace in medicine, the environmental sample and trace polar compound.
A kind of preparation method of titanium oxide extraction bar for solid phase microextraction is characterized in that may further comprise the steps:
A, polypropylene hollow fiber is put into the acetone ultrasonic cleaning, dry stand-by after the taking-up;
B, the polypropylene hollow fiber after will cleaning immerse in the titanium oxide sol, leave standstill after ultrasonic, and oven dry, polypropylene-base is removed in calcining, obtains anatase-type titanium oxide doughnut extraction bar finished product.
Calcining heat is 778～923K among the preparation process B of the present invention, constant temperature is more than 200 minutes, the titanium oxide that obtains at high temperature changes into Detitanium-ore-type, the form that presents nanoparticle under the ESEM, former polypropylene media is removed fully, stay a large amount of holes, so this material has bigger specific area.
Extraction bar of the present invention has three-dimensional porous structure, and bigger specific area is arranged, and coating layer thickness is controlled, chemistry and Heat stability is good, and pH stability range wide (pH=1～14) has higher extraction efficiency to polar compound.
The titanium oxide doughnut extraction bar that the present invention is prepared, can directly from liquid sample, carry out extracting and enriching to target compound, the extraction back only needs to use the micro updating solvent desorption, need not independent thermal desorption device, gas phase can be entered directly or liquid chromatogram is carried out compartment analysis, reduced the consumption of organic solvent and loaded down with trivial details pre-treatment step to the full extent, extracting mode is simple, has wide range of applications.
The specific embodiment
Embodiment 1
Get butyl titanate 50ml in the 100ml beaker, slowly add 15ml acetate, add absolute ethyl alcohol 175ml then, after other gets absolute ethyl alcohol 200ml and 10ml deionized water and mixes, slowly pour in the beaker, magnetic agitation evenly back sealing placement is spent the night, and obtains the titanium colloidal sol of 0.2mol/L.
Polypropylene hollow fiber is cut into the segment of 7.5mm, immersed in the acetone supersound washing 10 minutes, dry in the air then.
Above-mentioned polypropylene hollow fiber is immersed in the prepared titanium colloidal sol of 5ml, and ultrasonic concussion was left standstill 2 hours after 0.5 hour, took out the baking oven of putting into 393K and dried 2 hours, and repeated impregnations process 10 times obtains titanium oxide and coats the polypropylene hollow fiber extraction bar.Put into Muffle furnace, the control heating rate is 2K/min, and calcining heat is 798K, keeps under this temperature 5 hours, obtains titanium oxide doughnut extraction bar finished product.
Embodiment 2
Get butyl titanate 10ml in the 100ml beaker, slowly add 3ml acetate, add absolute ethyl alcohol 44ml then, draw the 1ml deionized water with syringe, slowly pour in the beaker, magnetic agitation evenly back sealing placement is spent the night, and obtains the titanium colloidal sol of 0.5mol/L.
Polypropylene hollow fiber is cut into the segment of 5mm, immersed in the acetone supersound washing 10 minutes, dry in the air then.
Above-mentioned polypropylene hollow fiber is immersed in the prepared titanium colloidal sol of 5ml, and ultrasonic concussion was left standstill 2 hours after 0.5 hour, took out the baking oven of putting into 393K and dried 2 hours, and repeated impregnations process 6 times obtains titanium oxide and coats the polypropylene hollow fiber extraction bar.Put into Muffle furnace, the control heating rate is 2K/min, and calcining heat is 823K, keeps under this temperature 5 hours, obtains titanium oxide doughnut extraction bar finished product.
Embodiment 3
Adopt titanium oxide doughnut extraction bar prepared among the embodiment 1 to N in the water sample, the N-dimethylacetylamide extracts analysis.
The titanium oxide doughnut extraction bar of preparation among the embodiment 1 is put into and contained N, in the water sample of N-dimethylacetylamide, ultrasonic concussion extraction 3 hours is taken out and is dried moisture content, with desorb under the absolute ethyl alcohol normal temperature of 50 microlitres 2 hours, the ethanol after the desorb directly entered gas-chromatography (GC-FID) analysis.
GC conditions: Agilent GC 6890 adopts AT SE-54 post (50 * 0.25 * 0.33); Temperature programming: 160 ℃ of initial temperatures, 20 ℃/min of heating rate, temperature is 250 ℃ eventually; Carrier gas: nitrogen, pressure 17.16psi, split sampling not, hydrogen ion flame (FID) detector, 250 ℃ of preceding detector temperatures.
Claims (2)
1. the preparation method of a titanium oxide extraction bar for solid phase microextraction is characterized in that may further comprise the steps:
A, polypropylene hollow fiber is put into the acetone ultrasonic cleaning, dry stand-by after the taking-up;
B, the polypropylene hollow fiber after will cleaning immerse in the titanium oxide sol, leave standstill after ultrasonic, and oven dry, polypropylene-base is removed in calcining, obtains anatase-type titanium oxide doughnut extraction bar finished product.
2. the method for claim 1, it is characterized in that: calcining heat is 778～923K among the step B, and constant temperature is more than 200 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101844793A CN101757898B (en) | 2008-12-25 | 2008-12-25 | Preparation method of titanium oxide extraction bar for solid phase microextraction |
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| CN2008101844793A CN101757898B (en) | 2008-12-25 | 2008-12-25 | Preparation method of titanium oxide extraction bar for solid phase microextraction |
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| CN101757898A CN101757898A (en) | 2010-06-30 |
| CN101757898B true CN101757898B (en) | 2011-10-19 |
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| CN2008101844793A Expired - Fee Related CN101757898B (en) | 2008-12-25 | 2008-12-25 | Preparation method of titanium oxide extraction bar for solid phase microextraction |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105709457B (en) * | 2014-12-05 | 2018-01-09 | 中国科学院大连化学物理研究所 | A kind of solid-phase extraction device and its application |
| CN106769344A (en) * | 2017-03-15 | 2017-05-31 | 天津工业大学 | A kind of method of trace charged contaminants in pretreating sewage |
| CN112095175B (en) * | 2020-04-14 | 2023-06-30 | 淄博市疾病预防控制中心 | Preparation method and application of rare earth doped oxide hollow extraction fiber |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000017429A1 (en) * | 1998-09-21 | 2000-03-30 | University Of South Florida | Solid phase microextraction fiber structure and method of making |
| US6759126B1 (en) * | 1998-09-21 | 2004-07-06 | University Of South Florida | Solid phase microextraction fiber structure and method of making |
| US6905031B1 (en) * | 1999-09-13 | 2005-06-14 | The Regents Of The University Of California | Solid phase microextraction device using aerogel |
| CN101306351A (en) * | 2008-07-09 | 2008-11-19 | 厦门大学 | Solid phase micro-extraction extraction head using odd-tube carbon nano-tube as coating and its preparation method |
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2008
- 2008-12-25 CN CN2008101844793A patent/CN101757898B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000017429A1 (en) * | 1998-09-21 | 2000-03-30 | University Of South Florida | Solid phase microextraction fiber structure and method of making |
| US6759126B1 (en) * | 1998-09-21 | 2004-07-06 | University Of South Florida | Solid phase microextraction fiber structure and method of making |
| US6905031B1 (en) * | 1999-09-13 | 2005-06-14 | The Regents Of The University Of California | Solid phase microextraction device using aerogel |
| CN101306351A (en) * | 2008-07-09 | 2008-11-19 | 厦门大学 | Solid phase micro-extraction extraction head using odd-tube carbon nano-tube as coating and its preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 冯雪等.固相微萃取技术的研究与应用现状.《化工环保》.2002,第22卷(第3期),146-150. * |
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Granted publication date: 20111019 Termination date: 20201225 |