Sample pretreatment and detection method for detecting aromatic amine reduced by azo dye

A sample pretreatment and azo dye technology, which is applied in the sample pretreatment method and detection field, can solve the problems of sample destruction, reductant heating, mass spectrometry detection, etc., to improve detection accuracy, strong mass spectrometry compatibility, and realize Effects of Mass Spectrometry Imaging

Active Publication Date: 2021-06-11
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method has milder conditions for the reduction reaction and fewer side reactions, it still requires a large amount of reducing agent (50 mg / mL) and requires heating
Due to these limitations, the traditional reduction method is destructive to the sample and a large amount of reaction reagents will make it impossible to perform mass spectrometry detection directly on-line. The reaction reagents will produce strong ion suppression. The traditional method needs to use liquid chromatography-mass spectrometry. Perform separation detection

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  • Sample pretreatment and detection method for detecting aromatic amine reduced by azo dye
  • Sample pretreatment and detection method for detecting aromatic amine reduced by azo dye
  • Sample pretreatment and detection method for detecting aromatic amine reduced by azo dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Example 1: Photocatalytic azo reduction decomposition using different reducing agents in a homogeneous solution to produce aromatic amines

[0051] 1) Photocatalytic reduction: Four reducing solutions were used, namely: 1mM methanolic solution of sodium dithionite, methanol solution of 1mM sodium sulfite, mixed methanol solution of 0.5mM sodium dithionite and 0.5mM sodium sulfite, and pure methanol. Azo dyes (Disperse Red 1, Disperse Blue 106, Disperse Orange 37, and Sudan III) were added to the four solutions to 30 μg / mL, respectively. Finally, 1.6 g / L titanium dioxide nanoparticles (5 nm) were added to the solution to obtain a dispersed solution. The solution was irradiated under a mercury lamp filtered at 356 nm for 30 min, and the current of the mercury lamp was kept at 8 mA and the irradiation distance was 10 cm.

[0052] 2) Collection of sample solution: centrifuge the titanium dioxide dispersion solution after irradiation at 8000 rpm for 10 min in a centrifuge. ...

Embodiment 2

[0055] Example 2: Reaction time curve of aromatic amine produced by photocatalytic (356nm wavelength) reduction decomposition of azo in homogeneous solution

[0056] 1) Photocatalytic reduction: 1 mM methanol solution of sodium sulfite and pure methanol were used as reducing reagents. The light reaction time is 5s, 10s, 30s, 1min, 2min, 5min, 10min, 30min, 60min. Other reducing conditions are with embodiment 1.

[0057] 2) Collection of sample solution: same as in Example 1.

[0058] 3) Liquid chromatography-mass spectrometry analysis: the same as in Example 1.

[0059] 4) Result analysis: the change curve of the product signal of different azos with the reaction time is as follows: Figure 5 shown. It can be seen from the results that the reaction rates of the two photocatalytic systems are basically similar, and for Sudan III, the reaction rate of the system without the inorganic reducing agent is even faster. And from the point of view of the repeatability of the react...

Embodiment 3

[0060] Example 3: Comparison of the reaction time curve of photocatalytic (200-400nm wavelength passband) azo reduction decomposition to produce aromatic amine in homogeneous solution and traditional chemical reaction

[0061] 1) Photocatalytic reduction: pure methanol was used as the reducing agent. The light reaction time is 5s, 10s, 30s, 1min, 2min, 5min, 10min, 30min, 60min. The solution was irradiated under a mercury lamp without a filter, and the current of the mercury lamp was kept at 8mA and the irradiation distance was 10cm. Other reducing conditions are with embodiment 1.

[0062] 2) Traditional chemical reduction: 20 mM sodium dithionate-pH 5 citric acid buffer (0.06 mol / L) was used as the reducing agent. The four azos were likewise added to the solution to 30 ppm. The solution was placed in a water bath and heated at 70°C for different times (1 min, 5 min, 10 min, 30 min, 60 min). After cooling, take it out and wait for liquid mass analysis.

[0063] 3) Collec...

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Abstract

The invention discloses a sample pretreatment and detection method for detecting aromatic amine reduced by an azo dye, which comprises the steps of contacting a sample containing the azo dye with an alcohol solvent, and dissolving the azo dye in the alcohol solvent to obtain an extracting solution; dispersing titanium dioxide nano particles in the extracting solution; and carrying out a photocatalytic reaction under ultraviolet irradiation to reduce and decompose the azo dye in the extracting solution into aromatic amine, and controlling the reaction time and the illumination wavelength to prevent the aromatic amine from being further decomposed, thereby obtaining a sample solution for detection. After the titanium dioxide particles in the sample solution are separated out, the sample is fed into a mass spectrum or liquid chromatography-mass spectrometer for detection. The method disclosed by the invention has the characteristics of rapidness, mildness, no need of a high-concentration reducing agent and no need of high temperature on reduction treatment of the sample, can realize direct mass spectrometric detection of aromatic amine generated by azo reduction decomposition in the sample, and does not need tedious and tedious chromatographic separation or solid-phase extraction pretreatment.

Description

technical field [0001] The invention relates to a sample pretreatment and detection technology for chemical substance detection, in particular to a pretreatment method and detection method for detecting samples containing prohibited azo dyes. Background technique [0002] Azo dyes refer to dyes containing azo groups (—N=N—) in their molecular structure. It is a widely used coloring agent, often used in dyeing of chemical fibers, leather, paper, etc., as well as in inks, plastics, cosmetics, etc. of coloring. Some azo dyes synthesized with "aryl amine intermediates" may undergo a reduction reaction during long-term contact with the human body, causing the double bond of the azo group to break, thereby releasing aromatic amine compounds that are harmful to the human body, or entering the In the human body, it will be reduced to aromatic amines under the action of enzymes in the body. Some of these aromatic amines are carcinogenic. Therefore, such dyes that can release carci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72
Inventor 吴倩周世文
Owner CENT SOUTH UNIV
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