Detection method for content of p-phenetidine impurity in ethoxyquinoline product

A technology of p-aminophenethyl ether and ethoxyquin, which is used in measurement devices, instruments, scientific instruments and other directions to achieve the effects of good stability and strong data reproducibility

Inactive Publication Date: 2017-12-01
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no relevant patent or literature report on the method for analyzing the impurity content of p-aminophenethyl ether in ethoxyquin products by high performance liquid chromatography

Method used

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  • Detection method for content of p-phenetidine impurity in ethoxyquinoline product
  • Detection method for content of p-phenetidine impurity in ethoxyquinoline product
  • Detection method for content of p-phenetidine impurity in ethoxyquinoline product

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Experimental program
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Effect test

Embodiment 1

[0029] Detection equipment and chromatographic conditions:

[0030] High performance liquid chromatography: Thermo Scientific, Dionex Ultimate 3000 DAD detector

[0031] Chromatographic column: reversed-phase column silica C18 packed column (150mm×10mm, 10μm), mobile phase: volume ratio of 80:20

[0032] Acetonitrile aqueous solution, mobile phase: 1mL / min, DAD detector detection wavelength: 200-400nm, column temperature: 30°C. Experimental steps:

[0033] (1) Sample preparation:

[0034] Take each 2.5g of p-aminophenethyl ether pure product and ethoxyquin pure product, place in a 50mL volumetric flask, add organic solvent acetonitrile to dissolve and then constant volume, after ultrasonic filtration, dilute and prepare to contain p-aminophenethyl ether pure product and ethoxyquinoline Quinoline pure product 250mg / L sample solution to be tested;

[0035] (2) Detection:

[0036] Take the above sample solution, inject 20 μL of sample, and record the peak time respectively. ...

Embodiment 2

[0038] Detection equipment and chromatographic conditions:

[0039] High performance liquid chromatography: Thermo Scientific, Dionex Ultimate 3000 DAD detector

[0040] Chromatographic column: Reverse-phase column silica C18 packed column (150mm×10mm, 10μm), mobile phase: 1mL / min, mobile phase:

[0041] The volume ratio of acetonitrile to water is 90:10, 80:20, 70:30, 60:40, 50:50 in aqueous solution of acetonitrile, DAD

[0042] Detector detection wavelength: 238nm, column temperature: 30°C.

[0043] Experimental steps:

[0044] (1) Sample preparation:

[0045] Take each 2.5g of p-aminophenethyl ether pure product and ethoxyquin pure product, place in a 50mL volumetric flask, add organic solvent acetonitrile to dissolve and then constant volume, after ultrasonic filtration, dilute and prepare to contain p-aminophenethyl ether pure product and ethoxyquinoline Quinoline pure product 250mg / L sample solution to be tested;

[0046] (2) Detection:

[0047] Take the above sam...

Embodiment 3

[0049] Detection equipment and chromatographic conditions:

[0050] High performance liquid chromatography: Thermo Scientific, Dionex Ultimate 3000DAD detector

[0051] Chromatographic column: Reversed-phase column silica C18 packed column (150mm×10mm, 10μm), mobile phase: 1mLmin, mobile phase:

[0052] Acetonitrile aqueous solution with a volume ratio of acetonitrile and water of 80:20, DAD detector detection wavelength: 238nm, column temperature: 30°C. Experimental steps:

[0053] (1) Sample preparation:

[0054] Take 2.5g of p-aminophenethyl ether pure product, put it in a 50mL volumetric flask, add the organic solvent acetonitrile to dissolve it, make it constant volume, and dilute it after ultrasonic filtration to prepare p-aminophenethyl ether containing 1000, 800, 600, 500, 250, 200, 100, 50, 20, 10, 5, 2.5, 1.0, 0.5, 0.25 mg / L sample solutions to be tested;

[0055] (2) Detection:

[0056] Take the above sample solution, inject 20 μL, and record the liquid chromatog...

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Abstract

A high performance liquid chromatography analysis method for a p-phenetidine impurity in an ethoxyquinoline product includes the steps of: 1) preparation of an ethoxyquinoline product solution: weighing 1 g of a sample solution in a 50 ml volumetric flask, and diluting the sample solution with an acetonitrile organic solvent to certain volume, and filtering the solution to prepare a to-be-detected sample; 2) performing HPLC quantitative analysis to the ethoxyquinoline product and the p-phenetidine impurity therein by using a non-polar HPLC column with an ultraviolet detector being 200-400 nm in wavelength, wherein the stationary phase is a 10 [mu]m reversed-phase chromatographic column silica gel filler and the mobile phase is a mixture liquid of liquid chromatography-pure acetonitrile and deionized water, liquid chromatography detection conditions including: column temperature being 30 DEG C, sampling size being 100 [mu]L and wavelength being 238 nm. The analysis method can completely separate the ethoxyquinoline and p-phenetidine, has accurate analysis result and high analysis efficiency, and is simple in sample treatment.

Description

technical field [0001] The invention relates to an analysis method for the purity of high-efficiency antioxidants and the content of impurities therein, in particular to a high-performance liquid chromatography analysis method for the purity of ethoxyquinoline products and the content of p-aminophenethyl ether impurities therein. Background technique [0002] Ethoxyquin (ethoxyquin), the chemical name is 6-ethoxy-2,2,4-trimethyl-1,2 dihydroquinoline, the chemical structural formula is as follows formula (I): [0003] [0004] Vitamins A, D, E, K, carotene and fatty acids in the feed, fish meal, meat meal, bone meal, blood meal, feather meal and other main nutrients are easily oxidized during the production, transportation and storage of the feed and affect the food quality of the feed. Efficacy and safety performance, it is necessary to add antioxidants. Among various antioxidants, ethoxyquinoline is recognized as the most effective, economical and practical antioxidant ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 吴一江任云华宋兴福褚伟华于建国
Owner EAST CHINA UNIV OF SCI & TECH
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