2, 4-dichlorophenoxyacetic acid standard substance preparation method and application thereof

A technology for crude extraction of dichlorophenoxyacetic acid and dichlorophenoxyacetic acid is applied in the field of preparation of 2,4-dichlorophenoxyacetic acid standard substances, and can solve the problems of cumbersome procedures, long delivery period, high cost and the like, To achieve the effect of simple process, stable product quality and good uniformity

Inactive Publication Date: 2017-02-22
CHINA NAT INST OF STANDARDIZATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the types and amounts of pesticides used in my country are the largest in the world, but there are still few corresponding reference materials, among which there are 126 types of secondary pesticide reference materials, and 17 primary pesticide reference materials, which shows that my country has the largest number of pesticide reference materials in the world. There is still a huge gap in research and development. At the same time, as of now, there is no research institution in China that can provide 2,4-dichlorophenoxyacetic acid standard substances and their preparation methods, while importing foreign-produced 2,4-dichlorophenoxyacetic acid standard substances The substance has problems such as high cost, cumbersome procedures, and long delivery cycle. Therefore, it is particularly necessary and urgent to prepare corresponding standard substances for the determination of 2,4-dichlorophenoxyacetic acid content.

Method used

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  • 2, 4-dichlorophenoxyacetic acid standard substance preparation method and application thereof
  • 2, 4-dichlorophenoxyacetic acid standard substance preparation method and application thereof
  • 2, 4-dichlorophenoxyacetic acid standard substance preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] A kind of 2,4-dichlorophenoxyacetic acid standard substance preparation method, comprises the following steps:

[0039] (1) Preparation of the test solution: Weigh an appropriate amount of crude extract of 2,4-dichlorophenoxyacetic acid, dissolve it in ultrapure water, make it fully dissolved, and filter through a 0.45um filter membrane to obtain the test solution ;

[0040] (2) Preparation by liquid chromatography: obtain high-purity 2,4-dichlorophenoxyacetic acid by semi-preparative liquid chromatography, wherein the chromatographic conditions are: the chromatographic column is PREP-ODS(H) KIT (250mm×20mm, 5μm ), mobile phase: A is 0.1% phosphoric acid aqueous solution, B is chromatographically pure methanol, gradient elution (0-11min, 0%A-80%A), flow velocity is 10mL / min, and column temperature is 25 ℃; Running time is 21min, the detection wavelength is 283nm, the injection volume is 1mL, and the fraction within 7.5-9min is collected;

[0041] (3) Collection: The r...

Embodiment 2

[0044] A kind of 2,4-dichlorophenoxyacetic acid standard substance preparation method, comprises the following steps:

[0045] (1) Preparation of the test solution: Weigh an appropriate amount of crude extract of 2,4-dichlorophenoxyacetic acid, dissolve it in ultrapure water, make it fully dissolved, and filter through a 0.45um filter membrane to obtain the test solution ;

[0046] (2) Liquid chromatography preparation: high-purity 2,4-dichlorophenoxyacetic acid was obtained by semi-preparative liquid chromatography, wherein the chromatographic conditions were: the chromatographic column was WatersXTerraRP18 (250mm×20mm, 5μm), and the mobile phase: A was 0.1% phosphoric acid aqueous solution, B is chromatographically pure methanol, gradient elution (0-11min, 0%A-80%A), flow rate is 10mL / min, column temperature is 25°C; running time is 21min, detection wavelength is 283nm, The injection volume is 1mL, and the fraction within 4.5-5.5min is collected;

[0047] (3) Collection: T...

Embodiment 3

[0049]A kind of 2,4-dichlorophenoxyacetic acid standard substance preparation method, comprises the following steps:

[0050] (1) Preparation of the test solution: Weigh an appropriate amount of crude extract of 2,4-dichlorophenoxyacetic acid, dissolve it in ultrapure water, make it fully dissolved, and filter through a 0.45um filter membrane to obtain the test solution ;

[0051] (2) Liquid chromatography preparation: high-purity 2,4-dichlorophenoxyacetic acid was obtained by semi-preparative liquid chromatography, wherein the chromatographic conditions were: chromatographic column was Wondasil C18 (250mm×20mm, 5μm), mobile phase: A 0.1% phosphoric acid aqueous solution, B is chromatographically pure methanol, gradient elution (0-11min, 0%A-80%A), flow rate is 10mL / min, column temperature is 25°C; running time is 21min, detection wavelength is 283nm , the injection volume is 1mL, and the fractions within 7-8min are collected;

[0052] (3) Collection: The receiving solution ...

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Abstract

The invention discloses a 2, 4-dichlorophenoxyacetic acid standard substance preparation method and the application thereof. The preparation method comprises the steps of (1) preparing a test solution; (2) preparing the liquid chromatography; (3) collecting. According to the technical scheme of the invention, a semi-preparative liquid chromatography system is adopted, and a prepared and separated dichlorophenoxyacetic acid standard sample is high in purity, simple in process, stable in product quality and good in uniformity. Meanwhile, involved solvents are free of pollution, so that the clean production is enabled. The 2, 4-dichlorophenoxyacetic acid standard substance preparation method has the advantages of low cost, environment-friendly extraction process, simple preparation method and the like. The prepared standard substance can make up the technical blank in the development field of 2, 4-dichlorophenoxyacetic acid standard substances in China.

Description

technical field [0001] The invention relates to a method for preparing a 2,4-dichlorophenoxyacetic acid standard substance and an application thereof, belonging to the field of compound extraction and preparation. Background technique [0002] In recent years, food safety issues have continued to turmoil, and problems such as pesticide residues and chemical additives exceeding the standard have occurred frequently, causing heavy casualties and property losses, endangering people's physical and mental health, and making food safety issues increasingly become a hot spot of concern to the whole society. Therefore, the study of pesticide residues has important theoretical and practical significance for ensuring the food safety of the people. [0003] 2,4-Dichlorophenoxyacetic Acid (2,4-Dichlorophenoxyacetic Acid) is a widely used chemical, referred to as 2,4-D. Pure 2,4-D can exist in the form of flakes, powders, crystal powders and solids. It is white with a slight tan color a...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/34
CPCG01N1/28G01N1/34G01N2001/2893
Inventor 初侨兰韬唐飞刘文席兴军董跟来杨丽燕艳华
Owner CHINA NAT INST OF STANDARDIZATION
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