Magnetic covalent organic framework compound solid phase extraction adsorbent and preparation method

A technology of covalent organic framework and adsorbent, which is applied in the field of analytical chemistry and food safety detection, can solve the problems of restricting the wide application of materials, and achieve the advantages of simple and fast preparation method, good solvent stability, low detection limit and quantification limit Effect

Active Publication Date: 2019-04-09
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, COF@Fe with core-shell structure has been 3 o 4 Materials have been reported as magnetic solid-phase extraction adsorbents, but the synthesis process needs to be strictly controlled, which limits the wide application of the materials

Method used

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  • Magnetic covalent organic framework compound solid phase extraction adsorbent and preparation method
  • Magnetic covalent organic framework compound solid phase extraction adsorbent and preparation method
  • Magnetic covalent organic framework compound solid phase extraction adsorbent and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1: Preparation of magnetic solid phase extraction adsorbent based on COF material

[0060] (1) Preparation of COF materials: Stable covalent organic framework compound materials are generated by solvothermal reaction. The selected COF material is COF-TpBD, and the raw materials used in the synthesis are 63 mg (0.3 mmol) of trialdehyde phloroglucinol (Tp) and 48 mg (0.45 mmol) of benzidine (BD). The organic solution used in the synthesis was 3 mL of mesitylene, 3 mL of 1,4-dioxane, and the catalyst was 0.3 mL of 6M acetic acid solution. The above-mentioned materials were ultrasonically mixed and then transferred into a Teflon reactor, and reacted at 120° C. for 72 hours. The material was taken out, washed repeatedly with acetone, and dried in vacuum for later use.

[0061] (2) Magnetization of COF materials: Synthesis of COF-(TpBD) / Fe by co-precipitation method 3 o 4 . Ferric chloride hexahydrate (FeCl 3 ·6H 2 O) 0.4g, ferrous sulfate heptahydrate (FeSO 4...

Embodiment 2

[0066] With reference to embodiment 1, the present invention adopts single factor test to COF-TpBD and synthetic Fe 3 o 4 The feed ratio of the iron source raw materials is optimized and inspected, by figure 1 It can be seen that the feed ratio has a great influence on the extraction and adsorption performance of the material. The adsorption effect is generally poor when the mass ratio is below 0.04:1, not exceeding 10%, and the adsorption performance is gradually improved when the mass ratio is above 0.04:1. When the ratio is 0.12:1, the adsorption effect of various compounds can reach 100%.

Embodiment 3

[0067] Example 3: Using COF-(TpBD) / Fe 3 o 4 Extraction and detection of 15 kinds of PAEs in beverage samples

[0068] (1) Standard solution preparation: PAEs-methanol standard solution with a concentration of 1000mg / mL, including DMP / DEP / DIBP / DBP / DMEP / BMPP / DEEP / DPP / DHXP / BBP / DBEP / DCHP / DEHP / DphP / DNOP gradient Dilute to 100mg / mL, 10mg / mL, respectively as stock solution and intermediate solution. The concentration of the working solution for the standard curve is 5 μg / mL, 10 μg / mL, 20 μg / mL, 50 μg / mL, 100 μg / mL, 200 μg / mL, 500 μg / mL, 1000 μg / mL, ready for use.

[0069] (2) Pretreatment of samples to be tested

[0070] Beer, carbonated drinks and alcoholic carbonated drinks are degassed in an ultrasonic bath to eliminate carbon dioxide. Then, drinks with complex matrix such as milk drinks, fruit juices and milk tea are diluted with pure water at a ratio of 1:8, and other beverages are diluted with pure water at a ratio of 1:5 to reduce matrix interference before the extraction ...

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Abstract

The invention discloses a magnetic covalent organic framework compound solid phase extraction adsorbent and a preparation method and belongs to the technical field of analytical chemistry and food safety inspection. The invention provides the magnetic covalent organic framework compound solid phase extraction adsorbent and the preparation method. By coordinating Fe ions and N atoms in TpBD and taking a COF-(TpBD) / Fe3O4 mixture obtained by a coprecipitation method as an adsorbent, the adsorbent is used for extracting and purifying aromatic compounds in a food matrix, in particular a phthalate target. The method simplifies a process of pre-treatment of a sample, and the magnetic adsorbent is synthesized by a coprecipitation method. The adsorbent is simple and quick and easily available, andthe extraction workload is reduced. The detection limit of a phthalate compound is greatly reduced.

Description

technical field [0001] The invention relates to a magnetic covalent organic framework compound magnetic solid-phase extraction adsorbent and a preparation method thereof, belonging to the technical fields of analytical chemistry and food safety detection. Background technique [0002] Magnetic solid-phase extraction (MSPE) sorbents provide fast dispersion and adsorption in sample solutions, enabling rapid separation using an external magnet. Compared with traditional solid-phase extraction (SPE), MSPE has many obvious advantages, including simple operation, reduced consumption of organic solvents, avoidance of high back pressure caused by close packing of SPE packing, and fast and simple external magnet separation of analytes, It is easy to be used with detection instruments and so on. An important component of MSPE is the adsorption material, which determines the sensitivity and selectivity of the method. Therefore, the development of magnetic solid phase extraction (MSPE...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08G01N30/02G01N30/06G01N30/72
CPCB01D15/08B01J20/06B01J20/22B01J20/28009B01J2220/46B01J2220/4806B01J2220/4812B01J2220/52B01J2220/54G01N30/02G01N30/06G01N30/7233G01N2030/025G01N2030/062
Inventor 庞月红岳琪沈晓芳杨成
Owner JIANGNAN UNIV
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