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Use and detection method of 3,3'-diaminobenzidine and its quinoxaline analogs in the detection of diacetyl

A technology of diaminobenzidine and its analogues, which is applied in the field of diacetyl detection and can solve the problems of only seeing selenium in the application

Active Publication Date: 2019-04-05
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in countries with developed aerospace and military industries, DAB has been focused on research and used as a monomer for the preparation of high-grade polymer materials, mainly for the synthesis of heat-resistant polymer resins and synthetic fibers, but it is used as a color developer in analytical chemistry. The field of application is only found in the photometric determination of selenium

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  • Use and detection method of 3,3'-diaminobenzidine and its quinoxaline analogs in the detection of diacetyl
  • Use and detection method of 3,3'-diaminobenzidine and its quinoxaline analogs in the detection of diacetyl
  • Use and detection method of 3,3'-diaminobenzidine and its quinoxaline analogs in the detection of diacetyl

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Experimental program
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Embodiment Construction

[0042] 1. Preparation of DAB analogs II-IV

[0043] 1. Preparation of DAB analog II: The reaction is as follows, taking diacetyl as an example for compound A.

[0044]

[0045]The specific process is: weigh 3,3'-diaminobenzidine tetrahydrochloride (DAB-4HCl) (108mg, 0.3mmol), add it to a 25mL round bottom flask, add 10mL distilled water, and stir gently at room temperature to make DAB fully dissolve. After about 10-20 minutes, add diacetyl (35mg, 0.4mmol), continue stirring at room temperature for half an hour, filter the reaction solution, wash the insoluble matter with distilled water three times (5mL×3), and combine the washing solution with the previous filtrate , extracted with chloroform (20mL×5), combined the 3rd to 5th extracts, anhydrous MgSO 4 After drying for 2 hours, the desiccant was removed by filtration, and the filtrate was concentrated under reduced pressure to obtain a dark red powder (65.2 mg, 82.3%). 1 H-NMR (D 2 O, 400MHz): 7.51 (1H, brs), 7.41 (1H,...

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Abstract

The present invention establishes for the first time the use of 3,3'-diaminobenzidine and its quinoxaline analogues in the detection of diacetyl, and provides a pre-column derivatization-HPLC method for detecting diacetyl (2, 3‑Butanedione, C 4 H 6 O 2 ) content method. DAB and its quinoxaline analogues were used as derivatization reagents to detect diacetyl content in wine samples. The reaction can be completed in 5 minutes at room temperature, and the pH value of the reaction system does not need to be strictly controlled. Compared with the existing pre-column derivatization-HPLC method, the present invention has the advantages of mild derivatization reaction conditions, simple and fast operation, and the like.

Description

technical field [0001] The invention relates to a diacetyl detection method. Background technique [0002] 2,3-Butanedione, also known as diacetyl, is a light yellow to yellow-green liquid at room temperature, with a benzoquinone smell, and a creamy smell in dilute solutions. It exists in fennel oil and cream, is soluble in water, and can be mixed with ethanol, Miscible with ether. [0003] Diacetyl is a degradation product of many components in food such as fatty acids (triglycerides), carbohydrates (sugars), proteins, and nucleic acids. As a natural product in the fermentation process, it exists in fermented dairy products and beverages; An important flavor substance, it is widely used in the production of creamy microwave popcorn, candy, chocolate, baked goods, etc. But when its concentration exceeds a certain range, it will have a negative impact on the flavor of food and has potential hazards to human health. A large number of studies on the negative impact of diacet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06C07D241/12C07D241/46
CPCC07D241/12C07D241/46G01N30/02G01N30/06
Inventor 高文运王继宇李恒惠先甘泉
Owner NORTHWEST UNIV