Deuterated marker and application of the deuterated marker in detection of edible essence 3-acetyl-2, 5-dimethylthiophene

A technology of dimethyl thiophene and food flavor, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unreported, unavailable, mutagenicity, etc., achieve simple pre-treatment, reliable results, and improve accuracy sexual effect

Inactive Publication Date: 2019-12-13
ZHEJIANG INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

3-Acetyl-2,5-dimethylthiophene is a synthetic spice with a roasted and nutty smell. It is allowed to be used as a food in my country's national standard GB 2760-2014 "National Food Safety Standard Food Additive Use Standard" Synthetic spices are used, but in June 2013, the European Food Safety Authority assessed that it showed mutagenicity in both in vivo and in vitro tests, and there were safety problems in using it as a food spice
However, since the detection of 3-acetyl-2,5-dimethylthiophene is still rare in China, its isotope-labeled internal standard has not been reported, nor can it be purchased in the market.

Method used

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  • Deuterated marker and application of the deuterated marker in detection of edible essence 3-acetyl-2, 5-dimethylthiophene
  • Deuterated marker and application of the deuterated marker in detection of edible essence 3-acetyl-2, 5-dimethylthiophene
  • Deuterated marker and application of the deuterated marker in detection of edible essence 3-acetyl-2, 5-dimethylthiophene

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Embodiment 1

[0036] 1. 3-Acetyl-2,5-dimethylthiophene-D 3 Synthesis

[0037] 1.D 3 -Synthesis of deuterated acetyl chloride

[0038]

[0039] Under reflux conditions, slowly drop 4.5mL of deuterated acetic acid (excessive) into 5mL of thionyl chloride, the reaction ends when no gas is produced, and the mixture is distilled to obtain 4.5g of colorless oily deuterated acetyl chloride (1). With, based on thionyl chloride yield 80%.

[0040]

[0041] 2. 3-Acetyl-2,5-dimethylthiophene-D 3 Synthesis

[0042] Under the condition of -15°C ice-salt bath cooling, the CS 2 (20mL) was added dropwise deuterated acetyl chloride (1) (0.89g, 11.0mmol) into the solution, and under stirring, anhydrous aluminum chloride (1.63g, 12.0 mmol), slowly warming up to room temperature, and continue stirring until TLC (thin-layer chromatography, developer is petroleum ether / ethyl acetate with a volume ratio of 10:1) detects that the reaction is complete, and the resulting mixture is poured into 0 ° C, 30m...

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Abstract

The invention discloses a deuterated marker and the application of the deuterated marker in edible essence 3-acetyl-2, 5-dimethylthiophene. According to the invention, an isotope internal standard-ultra-high performance liquid chromatography-triple quadrupole mass spectrometry method is adopted for the first time to determine 3-acetyl-2, 5-dimethylthiophene in an edible essence, a deuterated isotope label of a target is adopted as an internal standard, possible differences of a matrix effect and an extraction effect of different essences can be well corrected, meanwhile, a system error can bereduced, the quantification accuracy and the stability of the method are improved, and the application is wide. An ultra-high performance liquid chromatography-triple quadrupole mass spectrometer is adopted for determination, and the detection means of the 3-acetyl-2, 5-dimethylthiophene is expanded. The method has the advantages of simple pretreatment, good repeatability and reliable result, andthe quantification limit of the method is 1 mg / kg when a sample amount is 0.1 g and a constant volume is 10 mL.

Description

[0001] (1) Technical field [0002] The invention relates to the technical field of food additive detection, in particular to a method for determining 3-acetyl-2,5-dimethylthiophene in food flavors by means of isotope internal standard-ultra-high performance liquid chromatography-triple quadrupole mass spectrometry. [0003] (2) Background technology [0004] Edible flavors and fragrances are indispensable food additives in the modern food industry, often composed of several or even dozens or hundreds of natural or synthetic spices. 3-Acetyl-2,5-dimethylthiophene is a synthetic spice with a roasted and nutty smell. It is allowed to be used as a food in my country's national standard GB 2760-2014 "National Food Safety Standard Food Additive Use Standard" Synthetic spices are used, but in June 2013, the European Food Safety Authority assessed that it showed mutagenicity in both in vivo and in vitro tests, and there was a safety problem when used as a food spice. In June of the sa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/04G01N30/06G01N30/14G01N30/90G01N30/94G01N30/88
CPCG01N30/02G01N30/72G01N30/04G01N30/06G01N30/14G01N30/90G01N30/94G01N30/88G01N2030/045G01N2030/062G01N2030/146G01N2030/067G01N2030/884
Inventor 茅佩卿王峰陈碧莲刘柱梁晶晶金绍强
Owner ZHEJIANG INST FOR FOOD & DRUG CONTROL
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