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Stable isotope labeled leucomalachite green and synthesis method thereof

A leuco-malachite green and stable isotope technology, applied in the field of stable isotope-labeled leuco-malachite green and its synthesis, can solve the problems of cumbersome methods, only semi-quantitative analysis, low sensitivity and the like, and achieves easy separation and purification , good economy, high atom utilization effect

Inactive Publication Date: 2018-10-09
SHANGHAI ANPEL SCI INSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The detection methods for leuco malachite green residues in aquatic products mainly include high performance liquid chromatography, thin layer chromatography, spectrophotometry, high performance liquid chromatography-mass spectrometry (LC-MS), Raman spectroscopy, etc. However, these methods generally have shortcomings such as low sensitivity, complicated methods, or only semi-quantitative analysis.

Method used

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  • Stable isotope labeled leucomalachite green and synthesis method thereof
  • Stable isotope labeled leucomalachite green and synthesis method thereof
  • Stable isotope labeled leucomalachite green and synthesis method thereof

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Effect test

Embodiment 1

[0024] A kind of synthetic method of the leuco malachite green of stable isotope label, this method specifically comprises the following steps:

[0025] (a) At 0°C, slowly add 4mL of concentrated sulfuric acid to the mixed solution of 80mL acetic acid and 80mL acetic anhydride, the temperature does not exceed 5°C, add 4mL of toluene-D 8 , slowly add 8 g of chromium trioxide solid, the temperature does not exceed 10 ° C, continue to stir for 10 min, pour into ice water, extract with ether, wash the organic phase with water until PH = 7, and remove the solvent under reduced pressure to obtain benzylidene diacetic acid- D. 6 Intermediate, the intermediate was refluxed in a mixed solution of 80mL ethanol and 40mL 1M sulfuric acid for 30min. After the end, the ethanol was removed under reduced pressure, extracted with ether, the organic phase was washed with water until PH=7, separated by column chromatography, and the yield was 38%. Benzaldehyde-D 6 .

[0026] (b) benzaldehyde-...

Embodiment 2

[0028] A kind of synthetic method of the leuco malachite green of stable isotope label, this method specifically comprises the following steps:

[0029] (a) At 0°C, slowly add 4mL of concentrated sulfuric acid to the mixed solution of 80mL acetic acid and 80mL acetic anhydride, the temperature does not exceed 5°C, add 4mL of toluene-D 8 , slowly add 12g of chromium trioxide solid, the temperature does not exceed 10°C, continue to stir for 10min, pour into ice water, extract with ether, wash the organic phase with water until PH = 7, remove the solvent from the organic phase under reduced pressure to obtain benzylidene diacetic acid- D. 6 Intermediate, the intermediate was refluxed in a mixed solution of 80mL ethanol and 40mL 1M sulfuric acid for 30min. After the end, the ethanol was removed under reduced pressure, extracted with ether, the organic phase was washed with water until PH=7, separated by column chromatography, and the yield was 40%. Benzaldehyde-D 6 .

[0030] (...

Embodiment 3

[0032] A kind of synthetic method of the leuco malachite green of stable isotope label, this method specifically comprises the following steps:

[0033] (a) At 0°C, slowly add 4mL of concentrated sulfuric acid to the mixed solution of 80mL acetic acid and 80mL acetic anhydride, the temperature does not exceed 5°C, add 4mL of toluene-D 8 , slowly add 16g of chromium trioxide solid, the temperature does not exceed 10°C, continue to stir for 10min, pour into ice water, extract with ether, wash the organic phase with water until PH = 7, and remove the solvent from the organic phase under reduced pressure to obtain benzylidene diacetic acid- D. 6 Intermediate, the intermediate was refluxed in a mixed solution of 80mL ethanol and 40mL 1M sulfuric acid for 30min. After the end, the ethanol was removed under reduced pressure, extracted with ether, the organic phase was washed with water until PH = 7, separated by column chromatography, and the yield was 32%. Benzaldehyde-D 6 .

[0...

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Abstract

The invention discloses stable isotope labeled leucomalachite green and a synthesis method thereof. The method comprises the following steps: (a), oxidizing stable isotope labeled methylbenzene in a mixed solvent of acetic acid, acetic anhydride and concentrated sulfuric acid through an oxidizing agent, so as to obtain stable isotope labeled a benzal diacetate intermediate, and performing hydrolysis under the action of ethanol and 1M sulfuric acid, so as to obtain stable isotope labeled benzaldehyde; (b), ensuring that the stable isotope labeled benzaldehyde is reacted with N, N dimethylaniline under the action of a catalyst, and performing treatment, separation and purification after reaction is finished, so as to obtain the stable isotope labeled leucomalachite green. The stable isotopelabeled leucomalachite green and the method have the advantages that the utilization of stable isotope atom is high, the synthesis steps are simple, products are easy to separate and purify, the requirement of serving as a standard reagent for the quantitative detection of the leucomalachite green is met, the use value is high, and the stable isotope labeled leucomalachite green has excellent economical efficiency.

Description

technical field [0001] The invention relates to the field of isotope labeling, in particular to a stable isotope-labeled leuco malachite green and a synthesis method thereof. Background technique [0002] Malachite green can inhibit cell division, thereby producing good antibacterial and bactericidal effects, and has been widely used in aquaculture, fresh-keeping and transportation processes. After it enters the human body or animal body through the food chain, it can be metabolized into fat-soluble leuco malachite green through biotransformation. This triphenylmethane substance has the risk of mutagenesis, teratogenicity and carcinogenicity, and can grow in the organism. Time remains, therefore, many countries including our country prohibit the use of malachite green in aquaculture. However, because of its cheap price and good bactericidal effect, it is still used illegally in the process of aquaculture, fresh-keeping and transportation. Therefore, it is necessary to moni...

Claims

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Application Information

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IPC IPC(8): C07C211/50C07C209/78
CPCC07B2200/05C07C45/54C07C209/78C07C211/50C07C47/54
Inventor 郭会陈武炼
Owner SHANGHAI ANPEL SCI INSTR
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