Simple and rapid preparation method and application of covalent-organic framework compound solid-phase microextraction coating

Abstract

The invention provides a simple and rapid preparation method and application of a covalent-organic framework compound solid-phase microextraction coating. According to the preparation method, the covalent-organic framework compound coating is quickly formed on quartz fiber, a device needed for the entire synthesizing process is extremely easy, and the method comprises the steps of performing amino-functionalization on the quartz fiber, impregnating surface amino-functionalized quartz fiber in a ground material precursor, repeating performing impregnating for several times, performing simple baking and cleaning the coating, so that the covalent-organic framework compound solid-phase microextraction coating can be obtained. The synthesizing method of the invention is easy to operate, requires few devices, and does not need an organic solvent, and by using the method, the covalent-organic framework compound solid-phase microextraction coating with high-temperature resistance, solvent resistance, acid and alkali resistance, high specific surface area, controllable pore size, and controllable thickness can be quickly prepared. Then the extraction coating is used to enrich environmentalpollutants polychlorinated biphenyls in water and it is detected that the coating has good enriching effects by using gas chromatography-mass spectrometry, thereby showing that the coating has good application prospect in the environment and other fields.

Description

technical field

[0001] The invention relates to a simple and rapid preparation method and application of a covalent organic framework compound solid-phase microextraction coating. Background technique

[0002] Solid phase microextraction (SPME) is a rapid sample pretreatment technology first proposed by Professor Pawliszyn of Canada in 1990. Compared with the traditional technology, the solid phase microextraction technology realizes the integration of enrichment, separation and detection, greatly shortens the time of sample pretreatment and simplifies the tedious sample pretreatment operation process, and greatly reduces the use of organic solvents. It has the characteristics of high sensitivity, simple operation process and low cost, and can be used to quickly and effectively analyze trace organic compounds in samples. The many advantages of SPME enable it to be used in various fields such as the environment, food, and biology. At present, commercialized fiber coatings m...

Examples

Embodiment 1

[0030] Simple and rapid preparation method of covalent organic framework compound solid phase microextraction coating and the specific operation process of applying it to sample pretreatment:

[0031] 1. A simple and rapid preparation method of a covalent organic framework compound solid-phase microextraction coating, which comprises the following steps:

[0032] 1.1 Pretreatment of quartz fibers

[0033] (a): Take a quartz fiber with a length of 20 cm and an inner diameter of 120 μm, immerse the front end 3 cm in acetone solution for 10 minutes, peel off the polyimide coating on the surface of the fiber, wash it with deionized water three times, and dry it in the air ; (b): The exposed quartz part was activated by immersing it in a 1 M sodium hydroxide solution for 1 h, exposing a large number of silanol groups on the surface, then washing it three times with deionized water, and then immersing it in a 0.1 M hydrochloric acid solution for 15 min , remove residual lye, wash w...

Embodiment 2

[0049] A simple and rapid method for preparing a covalent organic framework compound solid-phase microextraction coating, the amine organic ligand used is 2,6-diaminoanthraquinone, and the rest of the steps are the same as in Example 1.

Embodiment 3

[0051] A simple and rapid method for preparing a covalent organic framework compound solid-phase microextraction coating, the amine organic ligand used is 4,4'-diaminoterphenyl, and the rest of the steps are the same as in Example 1.

[0052] Table 1 shows the linear regression equation, linear correlation coefficient, linear range and detection limit for the detection of PCBs by this method

[0053]

[0054] It can be seen from the data in Table 1 that the detection linear range has a wider detection range at 5-10000 (ng / L), and the detection limit has a lower detection limit between 0.001-0.007 (ng / mL).

[0055] Table 2 is the precision inspection of SPME extracted fiber

[0056]

[0057] It can be seen from Table 2 that the precision RSD is less than 11.6%, indicating that the reproducibility of the extracted fiber is good and the coating is stable.

technical field

[0001] The invention relates to a simple and rapid preparation method and application of a covalent organic framework compound solid-phase microextraction coating. Background technique

[0002] Solid phase microextraction (SPME) is a rapid sample pretreatment technology first proposed by Professor Pawliszyn of Canada in 1990. Compared with the traditional technology, the solid phase microextraction technology realizes the integration of enrichment, separation and detection, greatly shortens the time of sample pretreatment and simplifies the tedious sample pretreatment operation process, and greatly reduces the use of organic solvents. It has the characteristics of high sensitivity, simple operation process and low cost, and can be used to quickly and effectively analyze trace organic compounds in samples. The many advantages of SPME enable it to be used in various fields such as the environment, food, and biology. At present, commercialized fiber coatings m...

Examples

Embodiment 1

[0030] Simple and rapid preparation method of covalent organic framework compound solid phase microextraction coating and the specific operation process of applying it to sample pretreatment:

[0031] 1. A simple and rapid preparation method of a covalent organic framework compound solid-phase microextraction coating, which comprises the following steps:

[0032] 1.1 Pretreatment of quartz fibers

[0033] (a): Take a quartz fiber with a length of 20 cm and an inner diameter of 120 μm, immerse the front end 3 cm in acetone solution for 10 minutes, peel off the polyimide coating on the surface of the fiber, wash it with deionized water three times, and dry it in the air ; (b): The exposed quartz part was activated by immersing it in a 1 M sodium hydroxide solution for 1 h, exposing a large number of silanol groups on the surface, then washing it three times with deionized water, and then immersing it in a 0.1 M hydrochloric acid solution for 15 min , remove residual lye, wash w...

Embodiment 2

[0049] A simple and rapid method for preparing a covalent organic framework compound solid-phase microextraction coating, the amine organic ligand used is 2,6-diaminoanthraquinone, and the rest of the steps are the same as in Example 1.

Embodiment 3

[0051] A simple and rapid method for preparing a covalent organic framework compound solid-phase microextraction coating, the amine organic ligand used is 4,4'-diaminoterphenyl, and the rest of the steps are the same as in Example 1.

[0052] Table 1 shows the linear regression equation, linear correlation coefficient, linear range and detection limit for the detection of PCBs by this method

[0053]

[0054] It can be seen from the data in Table 1 that the detection linear range has a wider detection range at 5-10000 (ng / L), and the detection limit has a lower detection limit between 0.001-0.007 (ng / mL).

[0055] Table 2 is the precision inspection of SPME extracted fiber

[0056]

[0057] It can be seen from Table 2 that the precision RSD is less than 11.6%, indicating that the reproducibility of the extracted fiber is good and the coating is stable.

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