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High-performance liquid chromatography detection method of 2,6-ditertbutyl-4-dimethylaminomethylphenol

A technology of dimethylaminomethylphenol and high performance liquid chromatography, which is applied in the field of chemical analysis, can solve problems such as no clear and reliable methods, and achieve the effects of thorough sample separation, good specificity, and easy operation

Inactive Publication Date: 2018-07-06
江苏迈达新材料股份有限公司
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  • Abstract
  • Description
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Problems solved by technology

However, corresponding to research and development, the existing high-performance liquid chromatography detection method for 2,6-di-tert-butyl-4-dimethylaminomethylphenol is not mature, and it has been reported in the literature that Fourier transform infrared spectroscopy and liquid mass spectrometry Use an instrument to detect and analyze 2,6-di-tert-butyl-4-dimethylaminomethylphenol, but only for qualitative analysis, for quantitative analysis to detect 2,6-di-tert-butyl-4-dimethylaminomethylphenol There is still no clear and reliable method for the purity of

Method used

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  • High-performance liquid chromatography detection method of 2,6-ditertbutyl-4-dimethylaminomethylphenol
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  • High-performance liquid chromatography detection method of 2,6-ditertbutyl-4-dimethylaminomethylphenol

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Experimental program
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Effect test

Embodiment 1

[0021] Instruments and reagents: High performance liquid chromatography with ultraviolet detector, octadecylsilane bonded silica gel column (5μm, 4.6mm I.D.×250mm); 2,6-di-tert-butyl-4-dimethylamine Methyl phenol sample, methanol (analytical grade), deionized water.

[0022] Chromatographic conditions: column temperature 30°C, mobile phase methanol-water, mobile phase volume ratio methanol: water = 8:2, mobile phase flow rate 1.0mL min -1 , isocratic elution, the detection wavelength of the ultraviolet detector is 260nm; the injection volume is 10μL.

[0023] Preparation of 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample solution: 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample was dissolved in methanol to prepare 2, 6-di-tert-butyl-4-dimethylaminomethylphenol sample solution, wherein the mass concentration of 2,6-di-tert-butyl-4-dimethylaminomethylphenol is 6%.

[0024] Under the above conditions, 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample was injected a...

Embodiment 2

[0029] Instruments and reagents: High performance liquid chromatography with ultraviolet detector, octadecylsilane bonded silica gel column (5μm, 4.6mm I.D.×250mm); 2,6-di-tert-butyl-4-dimethylamine Methyl phenol sample, methanol (analytical grade), deionized water.

[0030] Chromatographic conditions: column temperature 35°C, mobile phase methanol-water, mobile phase volume ratio methanol: water = 9:1, mobile phase flow rate 1.2mL min -1 , isocratic elution, the detection wavelength of the ultraviolet detector is 270nm, and the injection volume is 10 μL.

[0031] Preparation of 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample solution: 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample was dissolved in methanol to prepare 2, 6-di-tert-butyl-4-dimethylaminomethylphenol sample solution, wherein the mass concentration of 2,6-di-tert-butyl-4-dimethylaminomethylphenol is 8%, and the solvent is methanol.

[0032] Under the above conditions, 2,6-di-tert-butyl-4-dimethylamino...

Embodiment 3

[0037] Instruments and reagents: High performance liquid chromatography with ultraviolet detector, octadecylsilane bonded silica gel column (5μm, 4.6mm I.D.×250mm); 2,6-di-tert-butyl-4-dimethylamine Methyl phenol sample, ethanol (analytical grade), deionized water.

[0038] Chromatographic conditions: column temperature 25°C, mobile phase ethanol-water, mobile phase volume ratio is ethanol: water = 7:3, mobile phase flow rate is 0.8mL min -1 , isocratic elution, the detection wavelength of the ultraviolet detector is 290nm, and the injection volume is 10 μL.

[0039] Detection method: Preparation of 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample solution: Dissolve 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample in ethanol to prepare A 2,6-di-tert-butyl-4-dimethylaminomethylphenol sample solution was obtained, wherein the mass concentration of 2,6-di-tert-butyl-4-dimethylaminomethylphenol was 10%.

[0040] Under the above conditions, 2,6-di-tert-butyl-4-dimethylami...

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Abstract

The invention discloses a high-performance liquid chromatography detection method of 2,6-ditertbutyl-4-dimethylaminomethylphenol. The high-performance liquid chromatography conditions are as follows:a chromatographic column is made of octadecyl silane bonded silica, the column temperature is 25-40 DEG C, a mobile phase is methanol-water solution with the volume ratio of (70-90):(30-10) or alcohol-water solution with the volume ratio of (70-90):(30-10), the flow speed of the mobile phase is 0.8-1.5mL.min<-1>, the elution mode is isocratic elution, and the detection wavelength of an ultravioletdetector is 260-290nnm. The high-performance liquid chromatography detection method disclosed by the invention has the advantages of simple operation, good specificity, high sample separation degree,high accuracy and good analysis-result reproducibility.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and in particular relates to a high performance liquid chromatography detection method for 2,6-di-tert-butyl-4-dimethylaminomethylphenol. Background technique [0002] In a large number of polymer materials and various organic substances, there are oxidation problems. The most effective and convenient way to prevent the oxidation of organic substances is to add antioxidants, of which phenolic antioxidants are the most widely used, 2,6-ditertiary Butyl-4-dimethylaminomethylphenol is a new type of hindered phenolic antioxidant, and a dimethylaminomethyl group with certain reactivity is introduced at the para-position of the phenolic hydroxyl group. It is currently reported that the research on the synthesis of 2,6-di-tert-butyl-4-dimethylaminomethylphenol has been basically completed. However, corresponding to research and development, the existing high-performance liquid chromatography ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 陈福新陈琦朱志宏索潇萌
Owner 江苏迈达新材料股份有限公司
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