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Solid-phase microextraction probe and preparation method thereof

An extraction and modification technology, applied in the field of analytical chemistry, can solve the problems of low preparation efficiency, cumbersome process and long time, and achieve the effect of fast speed and rapid preparation

Active Publication Date: 2021-06-01
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in these preparation techniques based on POSS / GO polymeric materials, GO-based nanosheets need to be coated on the pretreated support fibers first, and then functional POSS chemicals are anchored on the GO coating, which requires the use of conventional amine- Modification by carboxyl or amine-epoxy reaction, the process of chemically bonding POSS / GO composites to fibers is cumbersome and takes a long time, even tens of hours, and the preparation efficiency is low

Method used

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

Examples

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Embodiment 1

[0028] A preparation method of a functionalized solid-phase microextraction probe based on alkenyl-modified graphene-nanometer siloxane polymer coating is as follows:

[0029] (1) Disperse 100 mg of graphene oxide GO in deionized water (100 mL) under the action of ultrasound, and sonicate for 1 h; Added dropwise into the above GO solution within 0.5 h under the same conditions, and continued to mechanically stir at 25 °C for 24 h to prepare alkenyl-functionalized γ-MAPS@GO;

[0030] (2) The stainless steel wire was treated with hydrofluoric acid at 70 °C for 5 min to form a rough surface, and then deionized water, ethanol, and deionized water were treated in an ultrasonic machine for 15 min each and dried naturally; 0.340 g AgNO 3 and 1.980g of glucose were each dissolved in 10 mL of distilled water, in AgNO 3 Add 28% ammonia water dropwise to the solution to form Ag 2 O precipitation, continue to drop 2.8% ammonia water until the precipitation is completely dissolved, add g...

Embodiment 2

[0040] Formulas A to F in Table 1 were used to prepare alkenyl-modified graphene-nanosiloxane polymer coating functionalized solid-phase microextraction probes to adsorb and desorb polycyclic musk PCMs in environmental water, respectively. The steps are: (1) Aging: Before use, the fiber was aged at the gas chromatograph inlet at 250 °C for 0.5 h; (2) Adsorption: 10 mL of PCMs solution was injected into a 20 mL headspace bottle, and heated at 75 °C Equilibrate for 5 min; pass the fiber in the SPME device through the septum, and expose it to steam at 75 °C for 50 min; (3) Desorption: quickly remove the fiber and insert it into the GC-MS inlet, and perform 5 min at 250 °C Min thermal analysis, using GC-MS detection to collect PCMs.

[0041] Such as Figure 5 , a single caged polysiloxane polymer has poor retention of PCMs, modified graphene oxide has improved retention of PCMs, and γ-MAPS@GO / POSS-MA (Formulation B) has a significant retention of PCMs Improvement, indicating th...

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Abstract

The invention relates to a solid-phase microextraction probe and a preparation method thereof. Based on ultraviolet-initiated polymerization, modified graphene oxide containing an olefinic bond functional group and polysiloxane containing a nanocage structure are used as monomers, and a stainless steel wire with the surface modified with sulfydryl is subjected to in-situ cross-linking polymerization to form a functional coating. Meanwhile, sulfydryl on the stainless steel wire and olefin on the monomer are subjected to 'sulfydryl-alkene' click chemistry to realize the coating immobilization solid-phase microextraction probe. According to the prepared micro-extraction probe, the modified graphene is supported by a rigid framework of a polysiloxane monomer, so that the aggregation of the graphene is effectively prevented, the stable distribution of the graphene is realized, the prepared polymeric coating has a large specific surface, delocalized pi-pi bonds and strong hydrophobicity, the preparation operation is simple, the cycle time is short (5min), the probe has good adsorption performance on volatile aromatic organic pollutants in environmental water, and can provide good pretreatment materials and technical support for environmental analysis.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a functionalized solid-phase microextraction probe based on an alkenyl-modified graphene-nanometer siloxane polymer coating and a preparation method thereof. Background technique [0002] High-performance sample pretreatment is one of the keys to accurate and sensitive analysis in analytical chemistry. Solid-phase microextraction (SPME) has the advantages of being simple and solvent-free, and has been widely used in GC-MS. To date, commercial SPME coatings have been developed including traditional polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane / divinylbenzene (PDMS / DVB) . However, traditional fiber coatings still have disadvantages such as low absorption capacity and long polymerization time. Therefore, the development of efficient strategies and functional fiber coatings with good thermal stability, strong extraction ability, and easy pr...

Claims

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Application Information

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IPC IPC(8): B01D15/20B01J20/26B01J20/30
CPCB01D15/20B01J20/26
Inventor 齐国敏
Owner FUZHOU UNIV
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