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Application and detecting method of 3,2'-diaminobenzidine (DAB) and quinoxaline analogues thereof on diacetyl detection

A technology of diaminobenzidine and analogs, applied in the field of diacetyl detection, can solve the problem of only seeing selenium in application

Active Publication Date: 2016-12-07
NORTHWEST UNIV
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  • Abstract
  • Description
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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

Method used

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  • Application and detecting method of 3,2'-diaminobenzidine (DAB) and quinoxaline analogues thereof on diacetyl detection
  • Application and detecting method of 3,2'-diaminobenzidine (DAB) and quinoxaline analogues thereof on diacetyl detection
  • Application and detecting method of 3,2'-diaminobenzidine (DAB) and quinoxaline analogues thereof on diacetyl detection

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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 invention discloses an application and a detecting method of 3,2'-diaminobenzidine (DAB) and quinoxaline analogues thereof on diacetyl detection and provides a method for detecting content of diacetyl (2,3-butanedione, C4H6O2) in liquid samples by adopting a precolumn derivatization-HPLC (high performance liquid chromatograph) method. The DAB and the quinoxaline analogues thereof are taken as a derivatization reagent to detect the content of the diacetyl in the liquid samples, reaction can be completely performed for 5 minutes at the indoor temperature, and PH (potential of hydrogen) value of the reaction system does not need to be strictly controlled. Compared with an existing precolumn-derivatization-HPLC method, the detecting method has the advantages of moderate derivatization reaction conditions, easiness in operation, rapidness 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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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
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