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Stable isotope 13C or 15N-labeled biurea synthesis method

A stable isotope and synthesis method technology, which is applied in the field of synthesis of stable isotope 13C or 15N labeled biurea, can solve the problems of difficult separation and recovery, lower isotope utilization rate, and difficult to meet the synthesis of stable isotope labeled biurea, and achieve the utilization The effect of high efficiency, simple operation, good practical value and economic value

Active Publication Date: 2016-02-03
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis methods of natural abundance biurea mainly include alkali method and acid method. In the existing synthesis technology, the excess of raw material urea or hydrazine hydrate is required to be more than 3 times, and in this reaction system, both the reactant and the product are in the water phase , therefore, the added excess urea or hydrazine hydrate is difficult to separate and recover in small-scale processes, resulting in a decrease in isotope utilization
It can be seen that the acid synthesis technology and alkaline synthesis technology of natural abundance biurea are difficult to meet the synthesis requirements of stable isotope-labeled biurea.

Method used

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  • Stable isotope 13C or 15N-labeled biurea synthesis method
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  • Stable isotope 13C or 15N-labeled biurea synthesis method

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Embodiment 1

[0029] Stable isotope labeled biurea-[ 13 C 2 , 15 N 2 ] The synthetic method, the concrete synthetic process of this method comprises the following steps:

[0030] In the reactor, add 12.5g (0.1mol) of 40wt% hydrazine hydrate N 2 h 4 ·H 2 O solution, be warmed up to 100 ℃, under stirring state, slowly add the sulfuric acid 98g (0.3mol) of the 30wt% freshly prepared dropwise, then add the urea-[ 13 C, 15 N 2 ], heat preservation reaction for 9 hours; after the reaction, cool to room temperature, suction filter, wash the product with warm water at 30°C, then filter with suction, and dry to constant weight in a vacuum oven at 50°C to obtain 8.7g of white powder with a yield of 71.2%, urea -[ 13 C, 15 N 2 ] has an isotope utilization rate of 71.2%, a chemical purity of 99.02%, and an isotope abundance of 99.02atom%. 15 N and 99.05atom% 13 c.

Embodiment 2

[0032] Stable isotope labeled biurea-[ 13 C 2 , 15 N 2 ] The synthetic method, the concrete synthetic process of this method comprises the following steps:

[0033] In the reactor, add 15g (0.15mol) of 50wt% hydrazine hydrate N 2 h 4 ·H 2 O solution, warming up to 120°C, under stirring, slowly add 514.5g (0.525mol) of freshly prepared 10wt% sulfuric acid, and then add 6.3g (0.1mol) of urea-[ 13 C, 15 N 2], heat preservation reaction for 7 hours; after the reaction, cool to room temperature, filter with suction, wash the product with warm water at 35°C, filter with suction again, and dry to constant weight in a vacuum oven at 50°C to obtain 10.7g of white powder with a yield of 87.6%, urea -[ 13 C, 15 N 2 ] has an isotope utilization rate of 87.6%, a chemical purity of 99.6%, and an isotope abundance of 99.35atom%. 15 N and 99.12atom% 13 c.

Embodiment 3

[0035] Stable isotope labeled biurea-[ 13 C 2 , 15 N 2 ] The synthetic method, the concrete synthetic process of this method comprises the following steps:

[0036] In the reactor, add 10g (0.12mol) of 60wt% hydrazine hydrate N 2 h 4 ·H 2 O solution, warming up to 120°C, under stirring, slowly add 47.04g (0.24mol) of freshly prepared 50wt% sulfuric acid, and then add 6.3g (0.1mol) of urea-[ 13 C, 15 N 2 ], heat preservation reaction for 5 hours; after the reaction, cool to room temperature, suction filter, wash the product with warm water at 40°C, then filter with suction, and dry to constant weight in a vacuum oven at 50°C to obtain 10.2g of white powder with a yield of 83.2%, urea -[ 13 C, 15 N 2 ] has an isotope utilization rate of 83.2%, a chemical purity of 99.45%, and an isotope abundance of 99.22atom%. 15 N and 99.15atom% 13 c.

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Abstract

The invention relates to a stable isotope 13C or 15N-labeled biurea synthesis method. Stable isotope-labeled urea and stable isotope-labeled hydrazine hydrate as raw materials undergo a reaction under the acid catalysis action and the product is purified to form the stable isotope-labeled biurea. Compared with the prior art, the synthesis method has mild reaction conditions and a high isotope utilization rate. Through separation purification, the stable isotope 13C or 15N-labeled biurea has chemical purity of 99% or more, isotopic abundance of 99atom% or more and mass number difference of 3 or more, satisfies requirements on an internal standard reagent in isotope dilution mass spectrometry-based detection of biurea residues in a flour product and has a good practical value and a good economic value.

Description

technical field [0001] The invention relates to the field of stable isotope labeling compounds, in particular to a stable isotope used for the detection of biurea residues in flour products 13 C or 15 Synthetic method of N-labeled biurea. Background technique [0002] Natural abundance biurea is an intermediate for the production of ADC foaming agent (azodicarbonamide). Azodicarbonamide is a foaming agent commonly used in industry and can be used in the production of yoga mats, rubber soles, etc. , to increase the elasticity of the product. It can also be used in the food industry to increase the strength and flexibility of dough. After processing, the metabolites of ADC are not safe. While improving the quality of flour, ADC will also produce by-products biurea and semicarbazide under high temperature pyrolysis conditions. Biurea and semicarbazide have strong mutagenic and carcinogenic effects in the human body. The use of azodicarbonamide in food has been banned in the...

Claims

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Application Information

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IPC IPC(8): C07C281/06
Inventor 王伟杜晓宁王雪婷解龙罗勇徐建飞宋明鸣雷雯田小叶侯捷
Owner SHANGHAI RES INST OF CHEM IND
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