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Synthesis method for stable isotope labeled malachite green

A stable isotope, malachite green technology, applied in the preparation of imino compounds, organic chemistry, etc., can solve the problems of not being able to detect malachite green and leuco malachite green at the same time, poor accuracy, cumbersome methods, etc., and achieve good economy. and use value, stable isotope atom utilization, simple effect of method and process

Active Publication Date: 2014-11-26
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-performance liquid chromatography has high sensitivity, but the method is cumbersome, so this method is rarely used
Thin-layer chromatography is simple and quick to operate, but it cannot detect malachite green and leuco malachite green at the same time
Spectrophotometry has high detection limits, but low sensitivity and poor accuracy of detection

Method used

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  • Synthesis method for stable isotope labeled malachite green
  • Synthesis method for stable isotope labeled malachite green
  • Synthesis method for stable isotope labeled malachite green

Examples

Experimental program
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Effect test

Embodiment 1

[0026] an isotope 13 The synthetic method of C marking malachite green, this method specifically comprises the following steps:

[0027] the isotope 13 C-labeled N,N-dimethylaniline- 13 C 2 Mix it with benzaldehyde at a molar ratio of 1:1, and with urea at a molar ratio of 2:1, then place it in a mixed solution of acetic acid and acetic anhydride, add dodecyltrimethylammonium chloride, dodecyltrimethylammonium ammonium chloride with 13 The weight ratio of C-labeled leuco malachite green is 0.04:1, the reaction temperature is controlled at 120°C, the reaction is stirred for 4 hours, and then NO and NO are introduced 2 The mixed gas, stirring reaction 8h, get 13 C-marked malachite green is the product, and the obtained product has a chemical purity of 99.0% and an isotopic abundance of 99.0% atom.

Embodiment 2

[0029] an isotope 13 The synthetic method of C marking malachite green, this method specifically comprises the following steps:

[0030] the isotope 13 C-labeled N,N-dimethylaniline- 13 C 2 Mix it with benzaldehyde at a molar ratio of 3:1, and with urea at a molar ratio of 4:1, put it in hydrochloric acid solution, add tetrabutylammonium chloride, tetrabutylammonium chloride and 13 The weight ratio of C-labeled leuco malachite green is 0.1:1, the reaction temperature is controlled at 160°C, the reaction is stirred for 2 hours, and then NO and NO are introduced 2 The mixed gas, stirring reaction 4h, get 13 C-marked malachite green is the product, and the obtained product has a chemical purity of 99.1% and an isotopic abundance of 99.4% atom.

Embodiment 3

[0032] an isotope 15 The synthetic method of N mark malachite green, this method specifically comprises the following steps:

[0033] the isotope 15 N-labeled N,N-dimethylaniline- 15 N and benzaldehyde in a molar ratio of 2:1, mixed with urea in a molar ratio of 3:1, placed in acetonitrile solution, added tetrabutylammonium bromide, tetrabutylammonium bromide and 15 The weight ratio of N-labeled leuco malachite green is 0.06:1, the reaction temperature is controlled at 90°C, the reaction is stirred for 4 hours, and then NO and NO 2 The mixed gas, stirring reaction 6h, get 15 N-labeled malachite green is the product, and the obtained product has a chemical purity of 99.2% and an isotopic abundance of 99.2% atom.

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Abstract

The invention relates to a synthesis method for stable isotope labeled malachite green. The stable isotope labeled malachite green is obtained by the steps of reacting stable isotope labeled N, N-dimethylaniline with a coupling agent and benzaldehyde, introducing mixed gas of NO and NO2, and separating and purifying after the reaction is finished. Compared with the prior art, after the stable isotope labeled malachite green prepared by the method is separated and purified, the chemical purity reaches over 99 percent and the isotope abundance is over 98 percent atom.

Description

technical field [0001] The invention relates to the field of isotope labeling, in particular to a synthesis method for isotope internal standard detection reagent stable isotope labeling malachite green. Background technique [0002] Malachite green has been widely used as a fungicide in the fish farming industry. The chemical functional group triphenylmethane in malachite green can cause cancer. It has been banned in many countries, but it is still used by fishermen to prevent fungal infection in fish, and also used by transporters as a disinfectant to prolong the survival time of fish in long-distance trafficking. . In order to prevent triphenylmethane compounds such as malachite green from entering the food chain, farmers and government monitoring departments need a fast, accurate and sensitive technology to detect it. [0003] The main detection techniques used to detect these triphenylmethane compounds are high performance liquid chromatography, thin layer chromatogra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/30C07C249/02
Inventor 杨超杨维成罗勇李美华
Owner SHANGHAI RES INST OF CHEM IND
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