Solid Phase Microextraction-High Performance Liquid Chromatography Online Detection Method of Oil Antioxidants

A high-performance liquid chromatography and detection method technology, which is applied in the field of solid-phase microextraction-high performance liquid chromatography on-line detection of oil antioxidants, to achieve the effects of reducing adsorption, reducing impact, and improving detection efficiency

Active Publication Date: 2021-11-30
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the use of covalent organic framework functionalized monolithic columns for online enrichment and extraction of oil antioxidants

Method used

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  • Solid Phase Microextraction-High Performance Liquid Chromatography Online Detection Method of Oil Antioxidants
  • Solid Phase Microextraction-High Performance Liquid Chromatography Online Detection Method of Oil Antioxidants
  • Solid Phase Microextraction-High Performance Liquid Chromatography Online Detection Method of Oil Antioxidants

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The covalent organic framework functionalized solid-phase microextraction monolithic column is prepared by mixing covalent organic framework nano-microspheres, urea aqueous solution, formaldehyde aqueous solution and a catalyst, wherein the covalent organic framework nano-microspheres, urea aqueous solution, and formaldehyde aqueous solution , The mass ratio of the catalyst is 2:9:11:2.

[0028] The aqueous urea solution has a concentration of 1 g / mL; the aqueous formaldehyde solution has a mass concentration of formaldehyde of 37%; the catalyst is an aqueous hydrochloric acid solution with a concentration of 0.1 mol / L.

[0029] The preparation method of the covalent organic framework functionalized solid-phase microextraction monolithic column comprises the following steps:

[0030] (1) Cleaning the empty tube: Rinse the empty PTFE tube with chromatographically pure methanol, then dry it in an oven at 60°C until use; the PTFE tube used is 10 cm in length and 750 mm in ...

Embodiment 2

[0035] The specific operation steps of the combined system are as follows:

[0036] In the first step, both the ten-way valve and the six-way valve of the online coupling system are in the LOAD position; the loading liquid passes through the pump A to balance the covalent organic framework functionalized solid-phase microextraction monolithic column (the monolithic column prepared in Example 1), and the flow rate is The flow rate is 0.1 mL / min; the mobile phase passes directly through the analytical column through pump B to obtain a stable baseline required for chromatographic separation, and the flow rate is 1.0 mL / min; at the same time, the sample solution is filled with the 0.5 mL PEEK tube quantitative loop through the injection needle;

[0037] In the second step, the six-way valve is adjusted to the INJECT position, and the online solid-phase microextraction starts. The sample in the 0.5 mL PEEK tube quantitative loop is brought into the covalent organic framework functio...

Embodiment 3

[0042] According to the technical scheme of Example 2, first prepare the covalent organic framework functionalized monolithic column of Example 1, and use the monolithic column as the solid-phase microextraction medium, refer to the relevant patent (patent number: 2018207623454) to construct solid-phase microextraction- High performance liquid chromatography online coupled analysis system. Then, relying on the on-line combined system to enrich and detect the antioxidants in oils, the optimized parameters of the combined system operation are: sample loading solution is ACN / 5 mM pH=6.0 ammonium formate solution=40% / 60% (v / v) ; eluent is acetonitrile; injection flow rate is 0.10 mL / min; elution flow rate is 0.10 mL / min; elution volume is 200 μL (eluate two minutes before collection); mobile phase is ACN / 0.05% formic acid solution= 60% / 40% (v / v); the flow rate of the mobile phase was 1.0 mL / min; the temperature of the column oven was 40 ℃; the detection wavelength was set at 201 n...

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Abstract

The invention discloses a solid-phase microextraction-high performance liquid chromatography on-line combined detection method for oil antioxidants. In the present invention, a covalent organic framework functional solid phase microextraction monolithic column is firstly prepared, and then the monolithic column is used as a solid phase microextraction medium, combined with a solid phase microextraction-high performance liquid chromatography on-line combined system, to establish an oil antioxidant Solid-phase microextraction-high performance liquid chromatography online detection method. The invention utilizes the synergistic mechanism of the hydrophilic interaction between the urea-formaldehyde resin matrix of the monolithic column and the analysis object and the π-π stacking interaction between the covalent organic framework and the analysis object to realize the efficient extraction and enrichment of oil antioxidants , and eliminate the interference of impurities in the sample matrix on the analysis and detection. The method of the invention is simple, the technique is ingenious, the required instruments are widely used, and it is easy to popularize. It can realize the efficient extraction and enrichment of trace oil antioxidants in complex actual samples, and can meet the relevant high-sensitivity detection requirements.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a solid phase microextraction-high performance liquid chromatography online combined detection method for oil antioxidants. Background technique [0002] During the processing, storage and use of oil, if it is affected by factors such as air, light, temperature, moisture, impurities, heavy metal ions and microorganisms for a long time, it will undergo oxidative rancidity. The rancidity of oil will not only affect the quality of oil products and their products, but also It will pose health risks such as aging, tumors, and cardiovascular diseases to the human body. In the food industry, antioxidants are usually added to oils to delay or eliminate oxidative rancidity of oils. Phenolic antioxidants are commonly used antioxidants in oils, and their representative substances mainly include: tert-butyl p-hydroxyanisole (BHA), propyl gallate (PG), tert-butyl hydroquinone ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08
CPCG01N30/02G01N30/06G01N30/08G01N2030/027G01N2030/062G01N2030/085
Inventor 王家斌倪碧晨
Owner FUZHOU UNIV
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