Detection method of 2, 4-diamino anisole sulfate

A technology of diaminoanisole and a detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as persistence, bioaccumulation hazards, toxicity of aquatic organisms, genetic defects, etc., and achieve sample addition and recovery High efficiency, easy operation, simple pre-processing effect

Inactive Publication Date: 2019-12-03
GUANGZHOU GRG METROLOGY & TEST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although it has good chemical properties, studies have confirmed that it may cause genetic defects and even cause cancer; and it is toxic to aquatic organisms and has long-lasting adverse effects because of its persistence, bioaccumulation and toxicity. The hazards have attracted great attention from all walks of life. On January 2, 2019, OEKO-TEX released a new version of OEKO-TEX Standard 100 for textile products, and officially included 2,4-diaminoanisole sulfate in its routine testing. project
[0006] It can be seen that it is very necessary to establish a suitable method for the determination of the content of 2,4-diaminoanisole sulfate in the product. However, its research is currently focused on the synthesis and application fields, and the detection of its residues in the product rare reports

Method used

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  • Detection method of 2, 4-diamino anisole sulfate
  • Detection method of 2, 4-diamino anisole sulfate
  • Detection method of 2, 4-diamino anisole sulfate

Examples

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Embodiment 1

[0047] A kind of detection method of 2,4-diaminoanisole sulfate, comprises the following steps:

[0048](1) Take a representative sample, cut it into pieces, the size is not more than 2mm×2mm, weigh 1.0g±0.1g sample, put it into a 60mL reaction bottle, add 10mL extraction reagent, and use first-grade water, methanol, and acetonitrile respectively , acetone and dichloromethane as extraction reagents, capped tightly and put into an ultrasonic cleaner for extraction, took it out and cooled to room temperature, took the extraction solution for centrifugation, filtered the sample with a 0.45 μm filter membrane, put it into a sample injection vial, and obtained the Test sample liquid;

[0049] (2) Dilute the 1000mg / L stock solution step by step with methanol to the standard working solution of 1, 2, 5, 10, 20 μg / L;

[0050] (3) measure the standard working solution of each concentration gradient in step (2) by ultra-high performance liquid chromatography-mass spectrometry, obtain s...

Embodiment 2

[0057] A kind of detection method of 2,4-diaminoanisole sulfate, comprises the following steps:

[0058] (1) Take a representative sample, cut it into pieces, the size is not more than 2mm×2mm, weigh 1.0g±0.1g sample, put it into a 60mL reaction bottle, add 10mL acetonitrile, cap it tightly, put it into an ultrasonic cleaner for extraction, The extraction temperature is 40-70°C, and the extraction time is 45-120 minutes. After taking it out, cool it down to room temperature, take the extraction solution for centrifugation, filter the sample with a 0.45 μm filter membrane, put it into a sample injection vial, and obtain the sample solution to be tested;

[0059] (2) Dilute the 1000mg / L stock solution step by step with methanol to the standard working solution of 1, 2, 5, 10, 20 μg / L;

[0060] (3) measure the standard working solution of each concentration gradient in step (2) by ultra-high performance liquid chromatography-mass spectrometry, obtain standard spectrogram, establi...

Embodiment 3

[0065] A kind of detection method of 2,4-diaminoanisole sulfate, comprises the following steps:

[0066] (1) Take a representative sample, cut it into pieces, the size is not more than 2mm×2mm, weigh 1.0g±0.1g sample, put it into a 60mL reaction bottle, add 10mL acetonitrile, cap it tightly, put it into an ultrasonic cleaner for extraction, The extraction temperature is 60°C, and the extraction time is 60 minutes. After taking it out, cool it to room temperature, take the extraction solution for centrifugation, filter the sample with a 0.45 μm filter membrane, put it into a sample injection vial, and obtain the sample solution to be tested;

[0067] (2) Dilute the 1000mg / L stock solution step by step with methanol to the standard working solution of 1, 2, 5, 10, 20 μg / L;

[0068] (3) measure the standard working solution of each concentration gradient in step (2) by ultra-high performance liquid chromatography-mass spectrometry, obtain standard spectrogram, establish standard ...

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Abstract

The invention discloses a detection method of 2, 4-diamino anisole sulfate. According to the method, an Agilentporoshell 120SB-Aq liquid chromatographic column is used, the setting of various parameters is optimized, the relatively high retention degree and relatively high separation efficiency of 2, 4-diamino anisole sulfate in the chromatographic column under an ultrahigh pressure condition canbe achieved, an electrospray ion source mode is employed, and the qualitative and quantitative analysis is carried out in positive ion and multi-reaction monitoring modes. The detection method of theinvention has the advantages of simple pretreatment, easy operation, high sensitivity and rapid and accurate detection, and the requirement for detecting 2, 4-diamino anisole sulfate in textile products can be met.

Description

technical field [0001] The invention relates to the field of detection of harmful substances in textiles, in particular to a detection method of 2,4-diaminoanisole sulfate. Background technique [0002] 2,4-Diaminoanisole sulfate, molecular formula C 7 h 10 N 2 O·H 2 SO 4 , is an off-white to violet or dark brown powder, easily soluble in acetone, methanol, acetonitrile, ether and other organic solvents, its basic information is shown in Table 1. [0003] Table 1 Basic information of 2,4-diaminoanisole sulfate [0004] [0005] As an important intermediate, 2,4-diaminoanisole sulfate is mainly used in the fields of organic pigment intermediates and hair dyes. Although it has good chemical properties, studies have confirmed that it may cause genetic defects and even cause cancer; and it is toxic to aquatic organisms and has long-lasting adverse effects because of its persistence, bioaccumulation and toxicity. The hazards have attracted great attention from all walks...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 李支薇严洪连张兰兰林炼锋王华钟琳
Owner GUANGZHOU GRG METROLOGY & TEST CO LTD
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