Solid-phase microextraction probe, and preparation method and application thereof

A probe and extraction technology, applied in the field of solid-phase microextraction probe and its preparation, can solve the problems of small acid-base range, insufficient use temperature, high analysis cost, etc., achieve high recovery rate, good linear range, detection low limit effect

Active Publication Date: 2014-05-28
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current commercialized solid-phase microextraction probe costs about 800-900 yuan, and its service life is only about 100 times. Therefore, the analysis cost of using solid-phase microextraction technology for detection and analysis is relatively high; Micro-extraction probes mostly use quartz fibers as carriers, and quartz fibers are also easy to break; more importantly, the maximum allowable temperature of some commercial solid-phase micro-extraction probes is not high enough to adapt to the acid-base range of the extraction solution is small
These unfavorable conditions largely limit the further development and application of solid phase microextraction technology.
[0004

Method used

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  • Solid-phase microextraction probe, and preparation method and application thereof
  • Solid-phase microextraction probe, and preparation method and application thereof
  • Solid-phase microextraction probe, and preparation method and application thereof

Examples

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Embodiment 1

[0037] Preparation of carbon nanospheres: The carbon nanospheres are synthesized according to the literature (Sci Rep. 2013, 3, 1430), and the synthesis method is as follows:

[0038] (1) Synthesis of monodisperse polystyrene nanospheres: In a three-necked flask, 25 mg sodium dodecylsulfonate was dissolved in 100 mL ultrapure water, stirred for 15 min, and then filled with nitrogen in the three-necked flask . Then, 2.5 mL and 0.25 mL of divinylbenzene were added into the three-necked flask, and after stirring for 5 min, 100 mg of potassium persulfate was added, kept at 75 °C for 3 h, and then 0.25 mL of divinylbenzene was added for 24 h. Finally, the samples were washed with ethanol and dried under vacuum at 50 °C.

[0039] (2) Synthesis of microporous monodisperse polystyrene nanospheres: 1.0 g monodisperse polystyrene nanospheres synthesized above were dissolved in 30 mL tetrachloromethane, 2.8 g aluminum chloride was dissolved in 30 mL tetrachloromethane , the two solutio...

Embodiment 2

[0043] The preparation of carbon nanosphere / PDMS solid-phase microextraction probe, the preparation process is as follows figure 1 , including the following steps:

[0044] S1. Preparation of sol-gel solution: Weigh 5 mg carbon nanospheres, add 300 μL methyltrimethoxysilane, 20 μL ultrapure water, 20 mg polymethylsiloxane (PDMS), and sonicate for 30 min , and then add 20 μL of trifluoroacetic acid, sonicate for 10 min, observe the viscous state of the sol-gel solution, and let it stand for 10 min before use.

[0045] S2. Pretreatment of stainless steel fibers: cut the stainless steel fibers to a length of 3 cm, soak in acetone for 1 h, soak in 1 mol / L NaOH solution for 2 h, and soak in 0.1 mol / L hydrochloric acid soak in the solution for 2 h, and finally soak in ultrapure water for 1 h. Remove the stainless steel fiber from the ultrapure water and let it dry naturally.

[0046] S3. When the sol-gel solution described in S1 is in a viscous state, insert the stainless steel f...

Embodiment 3

[0050] The preparation of carbon nanosphere / PDMS solid-phase microextraction probe specifically comprises the following steps:

[0051] S1. Preparation of sol-gel solution: Weigh 15 mg carbon nanospheres, add 400 μL methyltrimethoxysilane, 50 μL ultrapure water, 50 mg polymethylsiloxane (PDMS), and sonicate for 30 min , and then add 50 μL of trifluoroacetic acid, sonicate for 10 min, observe the viscous state of the sol-gel solution, and let it stand for 20 min before use.

[0052] S2. Pretreatment of stainless steel fibers: cut the stainless steel fibers to a length of 3 cm, soak in acetone for 1 h, soak in 1 mol / L NaOH solution for 2 h, and soak in 0.1 mol / L hydrochloric acid soak in the solution for 2 h, and finally soak in ultrapure water for 1 h. Remove the stainless steel fiber from the ultrapure water and let it dry naturally.

[0053] S3. When the sol-gel solution described in S1 is in a viscous state, insert the stainless steel fiber treated in S2 into the sol-gel s...

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Abstract

The invention relates to the field of solid-phase microextraction and in particular discloses a solid-phase microextraction probe, and a preparation method and application of the solid-phase microextraction probe. The solid-phase microextraction probe prepared by the preparation method comprises a stainless steel fiber and a surface coating which coats one end of the stainless steel fiber. The surface coating contains carbon nanospheres; the material has the advantages of great specific surface area being 1357m<2>/g, porosity with a pore volume being 1.02cm<3>/g, high dispersion degree with PDI (Polydispersity Index) being 0.05, small grain diameter being 246nm and the like. The material is an excellent absorption material. The probe is prepared through a sol-gel method; the preparation method is simple in preparation steps and low in preparation cost; the solid-phase microextraction probe prepared by the method is controllable in thickness and not easy to damage; when the solid-phase microextraction probe is applied to analysis and detection, the solid-phase microextraction probe has the advantages of good absorption effect, strong acid-base resistance, good thermal stability, good reproducibility and the like.

Description

technical field [0001] The present invention relates to the field of solid-phase microextraction, more specifically, to a solid-phase microextraction probe and its preparation method and application. Background technique [0002] Solid-phase micro-extraction (solid-phase micro-extraction, SPME) technology is a sample pretreatment technology that integrates sampling, extraction, concentration, and sample injection, and is a non-solvent selective extraction method. This technology can be combined with high-efficiency separation and detection techniques such as chromatography and mass spectrometry, so it has the advantages of easy automation, easy operation, no need for solvents, and environmental friendliness. It has been widely used in environmental protection, food testing, drug analysis and field of clinical analysis. [0003] Currently, SPME devices have been commercialized. The commercialized SPME device is mainly composed of a handle and an extraction head, and the sol...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/20B01J20/32B01D15/10G01N30/02
Inventor 欧阳钢锋郑娟吴丁财朱芳
Owner SUN YAT SEN UNIV
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