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Solid phase microextraction fiber for polycyclic aromatic hydrocarbon enriching detection and manufacturing method thereof

A technology for polycyclic aromatic hydrocarbons and fiber extraction, applied in the field of pollutant detection, can solve the problems of poor high temperature resistance, etc., and achieve the effect of not easy to fall off, uniform coating, and firm synthesis

Active Publication Date: 2018-09-28
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention successfully combines solid-phase microextraction without solvent, which integrates separation and enrichment with the excellent characteristics of large specific surface area and strong adsorption capacity of COF materials, and first forms a polydopamine coating to form a composite coating for COF materials on the substrate. The layer provides covalent and non-covalent forces to make the coating more uniform and firm. The excellent thermal stability of COF materials can effectively overcome the defects of poor high temperature resistance of commercial PDMS and increase its service life; and the covalent organic framework contains There is a π-π interaction between the large π-conjugated system and the benzene ring structure of polycyclic aromatic hydrocarbons, which enhances the adsorption of polycyclic aromatic hydrocarbons by the prepared solid-phase microextraction fibers, and plays a certain role in separation while enriching , can effectively simplify the sample matrix pretreatment steps; at the same time, it can greatly improve the enrichment ability of polycyclic aromatic hydrocarbon pollutants and reduce the detection limit of polycyclic aromatic hydrocarbon pollutants

Method used

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  • Solid phase microextraction fiber for polycyclic aromatic hydrocarbon enriching detection and manufacturing method thereof
  • Solid phase microextraction fiber for polycyclic aromatic hydrocarbon enriching detection and manufacturing method thereof
  • Solid phase microextraction fiber for polycyclic aromatic hydrocarbon enriching detection and manufacturing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Embodiment 1: The manufacture method of the solid-phase microextraction device based on polydopamine-TpBD composite coating

[0047] Corrode a 17cm-long stainless steel wire in newly prepared aqua regia for about 30 minutes, and the corrosion length is 3cm, and then immerse it in a 2mg / mL dopamine solution with a pH=8.5Tris-HCL, stir it in a water bath at 35°C for 12 hours, and then Rinse the surface with distilled water and oven dry at 80°C for 12 hours. Place the prepared polydopamine stainless steel wire in a reaction kettle of 63mg 1,3,5-trimethylresorcinol solution dissolved in 4mL mesitylene, and react at 80°C for 4 hours, then add 4mL dioxane A solution of 83mg of benzidine dissolved in the ring was reacted at 120°C for 48 hours. After removal, the fibers were soaked in acetone for 3 days, soaked in ethanol for 1 day, and dried in vacuum. The solid-phase microextraction device was fabricated by using the stainless steel wire fiber with a composite layer instead...

Embodiment 2

[0048] Example 2: Optimization of enrichment conditions for the detection of polycyclic aromatic hydrocarbons in barbecued meat by solid-phase microextraction device

[0049] During solid-phase microextraction, the extraction temperature, organic solvent ratio, extraction time, solution pH, rotation speed and analysis time all have an impact on the extraction results. In this experiment, direct (immersion) extraction method was used to enrich PAHs in barbecued meat. The conditions were optimized, and the proportion of organic solvent, rotation speed, solution pH, extraction time and analysis time were respectively optimized. The enrichment conditions were optimized by using 100ppt PAH mixed standard solution. The organic solvent is acetonitrile, the optimal range is between 0.1%-10%, the rotation speed is 300rpm, the temperature is 40°C, pH=6, the enrichment time is 30min, and the analysis time is 5min; the optimal rotation speed range is between 300-700rpm, and the acetonitri...

Embodiment 3

[0050] Example 3: Solid-phase microextraction device is used for the detection of polycyclic aromatic hydrocarbons in barbecue

[0051] (1) Preparation of standard samples: Prepare polycyclic aromatic hydrocarbon standard solution with acetonitrile, and gradiently dilute to 100 ppb for use. The 16 PAHs are naphthalene, acenaphthylene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene, Benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, indeno[1,2,3-c,d]pyrene, dibenzo[a,h]anthracene and benzo[a]pyrene [g,h,i] perylene.

[0052] (2) Configuration of the enrichment solution: distilled water was used to prepare the enrichment solution, the proportion of organic solvent was 0.1%, and the total volume was 10 mL.

[0053] (3) Sample preparation: Add 10 mL of acetonitrile to 1 g of grilled mutton for ultrasonic extraction for 20 min, centrifuge at 10,000 rpm for 10 min, take the supernatant, add 10 mL of acetonitrile to the residu...

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Abstract

The invention discloses a solid phase microextraction fiber for polycyclic aromatic hydrocarbon enriching detection and a manufacturing method thereof, and belongs to the technical field of contaminant detection. The invention provides a method capable of being used for manufacturing a solid phase microextraction coating on different fiber substrates and realizing combined use with gas chromatography or gas chromatography-mass spectrum, and the method is used for polycyclic aromatic hydrocarbon contaminant detection. Metal fiber is used as a substrate; dopamine is polymerized on the surface ofthe substrate so as to provide functional groups for polydopamine; the polydopamine is firstly combined with COF material single ligands so as to provide an anchor point; a PDA-COP composite layer isfinally synthesized and is used for solid phase microextraction. The solid phase microextraction fiber has the advantages that through the great pi bond effects between the solid phase microextraction fiber and the polycyclic aromatic hydrocarbon, the adsorption effect on the polycyclic aromatic hydrocarbon can be enhanced; during the enrichment, a certain separation effect is achieved; the substrate pretreatment step of samples can be effectively simplified; meanwhile, the enriching capability of the polycyclic aromatic hydrocarbon contaminants can be greatly improved; the detection limit ofthe polycyclic aromatic hydrocarbon contaminants can be reduced.

Description

technical field [0001] The invention relates to a solid-phase microextraction fiber for enrichment detection of polycyclic aromatic hydrocarbons and a production method thereof, belonging to the technical field of pollutant detection. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are hydrocarbons containing two or more conjugated benzene rings in their molecules. They are the earliest and most numerous carcinogens, which interfere with gene expression and induce cancer, deformity or other diseases. PAHs are widely distributed in the environment and food media, especially smoked, roasted, fried and other foods. Many countries have clear limits on polycyclic aromatic hydrocarbons, such as: the European Union stipulates four kinds of polycyclic aromatic hydrocarbons (benzo(a) pyrene, benzo(a) anthracene, benzo(b) fluoranthene and )) is 12μg / kg; the German Society for Fat Science recommends that the maximum residue limit of total PAHs is 25ppb, and the ...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30G01N30/02G01N30/06G01N30/08
CPCB01J20/286G01N30/02G01N30/06G01N30/08G01N2030/062
Inventor 庞月红马甜甜严秀平杨成沈晓芳
Owner JIANGNAN UNIV
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