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A kind of solid phase microextraction coating preparation method

An extraction and coating technology, applied in the field of solid-phase microextraction coating preparation, can solve the problems of large environmental pollution, low mechanical strength, and poor thermal stability in the preparation process, and achieve reduced environmental pollution, high mechanical strength, and extraction of coatings. stable effect

Active Publication Date: 2020-12-25
JIANGSU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The coatings in the prior art, such as polydimethylsiloxane, divinylbenzene, methylvinylsiloxane, etc., and their composite coatings, have weak enrichment ability and large environmental pollution in the preparation process. Low mechanical strength, poor thermal stability, high cost, short service life and other disadvantages

Method used

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  • A kind of solid phase microextraction coating preparation method
  • A kind of solid phase microextraction coating preparation method
  • A kind of solid phase microextraction coating preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The solid-phase microextraction coating preparation method of the present embodiment comprises the steps:

[0024] (1) Preparation of straw powder: cut corn straw into small pieces of about 0.5 cm, dry, crush, and pass through a 100-mesh sieve;

[0025] (2) Preparation of ionic liquid aqueous solution: 30% (W / V%) ionic liquid aqueous solution: take 30g ionic liquid 1-ethyl-3-methylimidazole diethyl phosphate salt, add 100ml deionized water;

[0026] (3) Preparation of straw solution: take 100g of 30% ionic liquid aqueous solution, add 1g of straw, add 0.01g of cellulase and pectinase, stir at 50°C for 30min, filter to obtain straw, dry, add 80% 1-ethyl- 100 g of a mixed solution of 3-methylimidazolium phosphate diethyl ester salt and 20% DMSO was heated at 150° C. for 1 hour, and cooled for later use to obtain a straw solution;

[0027] (4) Preparation of graphene oxide derivatives: Add 1g of graphite powder to 100g of acidic ionic liquid 1-ethyl-3-methylimidazole diet...

Embodiment 2

[0032] The solid-phase microextraction coating preparation method of the present embodiment comprises the steps:

[0033] (1) Preparation of straw powder: cut mulberry straw into small pieces of about 0.5 cm, dry, crush, and pass through a 100-mesh sieve;

[0034] (2) Preparation of ionic liquid aqueous solution: 30% (W / V%) ionic liquid aqueous solution: take 30g ionic liquid 1-butyl-3-methylimidazolium chloride salt, add 100ml deionized water;

[0035] (3) Preparation of straw solution: Take 100g of 30% ionic liquid aqueous solution, add 1g of straw, add 0.01g of cellulase, stir at 50°C for 30min, filter to obtain straw, dry, add 90% 1-ethyl-3-methylimidazole 100 g of a mixed solution of diethyl phosphate salt and 10% DMSO was heated at 160° C. for 30 min, and cooled for later use to obtain a straw solution;

[0036] (4) Preparation of graphene oxide derivatives: Add 1g of graphite powder to 100g of acidic ionic liquid 1-ethyl-3-methylimidazole diethyl phosphate salt, add it t...

Embodiment 3

[0041] The solid-phase microextraction coating preparation method of the present embodiment comprises the steps:

[0042] (1) Preparation of straw powder: cut wheat straw into small pieces of about 0.5 cm, dry, crush, and pass through a 100-mesh sieve;

[0043] (2) Preparation of ionic liquid aqueous solution: 30% (W / V%) ionic liquid aqueous solution: get 30g 1-ethyl-3-methylimidazole phosphate dimethyl salt and 1-butyl-3-methylimidazole acetic acid Add 100ml of deionized water to the ionic liquid in which the salt is mixed according to 1:1 (W / W);

[0044] (3) Preparation of straw solution: Take 100g of 30% ionic liquid aqueous solution, add 1g of straw, add 0.01g of pectinase, stir at 50°C for 30min, filter to obtain straw, dry, add 85% 1-ethyl-3-methylimidazole 100 g of a mixed solution of dimethyl phosphate salt and 15% DMSO was heated at 160° C. for 30 min, and cooled for later use to obtain a straw solution;

[0045] (4) Preparation of graphene oxide derivatives: Add 1g...

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Abstract

The invention discloses a method for preparing a solid-phase microextraction coating, which comprises the following steps: adding straw and biological enzymes to an aqueous ionic liquid solution, adding a mixed solution of acidic ionic liquid and DMSO after the reaction is completed, and heating to obtain a straw solution; Add graphite powder to the ionic liquid, ultrasonic pretreatment, add sulfuric acid and potassium permanganate, ultrasonic treatment again, introduce oxygen, centrifuge, wash and precipitate and dry to obtain graphene oxide, add it to the acidic ionic liquid, and then add 1‑methylimidazole, N‑picoline or pyrrolidone, heated to obtain graphene oxide derivatives; mixing and heating straw solution and graphene oxide derivatives to obtain sol solution; extracting fibers to form a rough surface, organic solvent After washing, ultrasonication and drying, it is immersed in a sol solution, then immersed in a polar solvent, and dried. The invention has the advantages of good biocompatibility, strong enrichment ability, stable extraction coating, long service life and the like.

Description

technical field [0001] The invention relates to a preparation method of a solid phase microextraction coating, in particular to a preparation method of a solid phase microextraction coating. Background technique [0002] Solid Phase Microextraction (Solid Phase Microextraction, SPME) was first developed in 1990 by the research team of Professor Pawliszyn of the University of Waterloo, Canada, and is a non-solvent selective extraction method. The technology has the advantages of simple operation, no solvent, fast extraction speed, easy automation, easy to combine with high-efficiency separation and detection methods such as chromatography and electrophoresis, and is suitable for gas, liquid and solid sample analysis. The novel sample pretreatment technology is outstanding. The advantages. Compared with solid phase extraction (SPE), SPME method has the characteristics of less extraction phase, higher selectivity of analytes, and easier eluting of solutes. Or in practice have...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
CPCG01N1/28
Inventor 李强季更生胡学健黄帆曹喜涛范史寅马静
Owner JIANGSU UNIV OF SCI & TECH
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