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A kind of synthesis method of stable isotope labeling prohibited pigment

A stable isotope and synthesis method technology, applied in the field of stable isotope-labeled prohibited pigment synthesis, can solve problems such as poor color, reddening when encountering alkali, fading when restored, endangering consumers' health, etc., and achieves good promotion prospects and good economy. and use-value, easy-to-compose effects

Active Publication Date: 2017-09-26
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has good heat resistance, acid resistance, light resistance and salt resistance. It is stable to citric acid and tartaric acid, but its oxidation resistance is poor. In food, beverage, medicine, cosmetics, feed and other industries, but because of its carcinogenicity, it has been banned from being used in meat and its processed products (including offal processed products), fish and its processed products, fruits and their products
[0004] But at present, some unscrupulous manufacturers still add Acid Orange II and Lemon Yellow to food, which seriously endangers the health of consumers.

Method used

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  • A kind of synthesis method of stable isotope labeling prohibited pigment
  • A kind of synthesis method of stable isotope labeling prohibited pigment
  • A kind of synthesis method of stable isotope labeling prohibited pigment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A. Stable isotope labeled aniline-D 5 Synthesis

[0042] Add bromobenzene-D to the flask successively 5 , ammonia water, bromobenzene-D 5 The molar ratio with ammonia water is 1:10, respectively add ferric chloride and ferric oxide (the molar ratio of the two is 1:1), and distilled water with a reaction volume of 20%, stir, heat to 60°C, and react for 18h. After the reaction, extract, wash and dry. The crude yield is 68.5%, and the distillation yield is 42.0%. The HPLC detection purity is 99.4%, and the abundance is 99.2%.

[0043] B. Synthesis of Stable Isotope Labeled Sodium p-Sulfuran

[0044] Add stable isotope-labeled aniline-D to the flask 5 , then sequentially add oleum, aniline-D 5 The molar ratio of oleum to oleum is 1:2, then add ethylene glycol, aniline-D 5 The molar ratio with ethylene glycol is 1:10. The reaction was sealed in vacuum, the reaction temperature was controlled at 120° C., and the reaction was stopped after 4 hours. Let the reactant st...

Embodiment 2

[0048] A. Stable isotope labeled aniline-D 5 Synthesis

[0049] Add bromobenzene-D to the flask successively 5 , ammonia water, bromobenzene-D 5 The molar ratio with ammonia water is 1:15, respectively add ferric chloride and ferric oxide (the molar ratio of the two is 1:1), and distilled water with a reaction volume of 20%, stir, heat to 60°C, and react for 18h. After the reaction, extract, wash and dry. The crude yield is 68.5%, and the distillation yield is 42.0%. The HPLC detection purity is 99.3%, and the abundance is 99.1%.

[0050] B. Synthesis of Stable Isotope Labeled Sodium p-Sulfuran

[0051] Add stable isotope-labeled aniline-D to the flask 5 , then sequentially add oleum, aniline-D 5 The molar ratio with oleum is 1:2.5, then add o-dichlorobenzene, aniline-D 5 The molar ratio to o-dichlorobenzene is 1:8. The reaction was sealed in vacuum, the reaction temperature was controlled at 140° C., and the reaction was stopped after 5 hours. Let the reactant stand ...

Embodiment 3

[0055] A. Stable isotope labeled aniline- 13 C 6 Synthesis

[0056] Add bromobenzene- 13 C 6 , ammonia water, bromobenzene- 13 C 6 The molar ratio with ammonia water is 1:15, respectively add ferric chloride and ferric oxide (the molar ratio of both is 1:1.5), and distilled water with 20% reaction volume, stir, heat to 100°C, and react for 20h. After the reaction, extract, wash and dry. The crude yield was 70.5%. After distillation, the yield was 46.0%. The HPLC detection purity was 99.4%, and the abundance was 99.5%.

[0057] B. Stable isotope labeled sodium p-aminobenzenesulfonate- 13 C 6 Synthesis

[0058] Stable isotope-labeled aniline was added to the flask- 13 C 6 , then sequentially added oleum, aniline- 13 C 6 The molar ratio with oleum is 1:3, then add ethylene glycol, aniline- 13 C 6 The molar ratio with ethylene glycol is 1:12. The reaction was sealed in vacuum, the reaction temperature was controlled at 160° C., and the reaction was stopped after 4 ...

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Abstract

The invention relates to a synthesis method of stable isotope-labeled prohibited pigments. The method uses stable isotope D or 13C-labeled bromobenzene to synthesize stable isotope D- or 13C-labeled intermediate sodium p-aminobenzenesulfonate through ammoniation and sulfonation , or use bromobenzene as a raw material, and ammonate and sulfonate the stable isotope 15N-labeled intermediate sodium p-aminobenzenesulfonate through ammoniation and sulfonation with a stable isotope 15N-labeled ammoniation reagent, and then undergo diazotization and coupling to obtain stable synthesis Prohibited pigments labeled with isotope D or 15N or 13C. Compared with the prior art, the process route of the present invention is simple, easy to synthesize, easy to separate and purify the product, the chemical purity of the product is above 99.0%, and the isotope abundance is above 98.0% atom, which can fully meet the needs of trace detection in the field of food safety. It has good economy and use value.

Description

technical field [0001] The invention belongs to the technical field of isotope labeling, and relates to a synthesis method for stable isotope labeling prohibited pigments. Background technique [0002] Acid orange Ⅱ belongs to chemical dyes, usually golden yellow powder, so commonly known as golden yellow powder, it dissolves in water and turns red light yellow, adding hydrochloric acid produces brownish yellow precipitate, adding sodium hydroxide solution turns dark brown, dissolves in ethanol and turns orange, dissolves in water It is magenta in concentrated sulfuric acid, and produces a brownish-yellow precipitate after dilution. It is mainly used for dyeing wool, silk, nylon and direct printing of fabrics. It has bright color and good level dyeing, but its fastness is poor. It can also be used for leather. , coloring of paper and biological products. At the same time, it is also an indicator, which is commonly used in the staining of tissue sections in medicine. In the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B29/01C09B29/15C09B29/50
Inventor 杨维成王浩然罗勇杨超方超李美华盛立彦潘洁孙雯
Owner SHANGHAI RES INST OF CHEM IND
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