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A method for detecting 3-acetyl-2,5-dimethylthiophene

A technology based on dimethylthiophene and acetyl, which is applied in the field of analytical chemistry, can solve problems such as lack of research, and achieve the effects of high sensitivity, elimination of interference, and easy operation

Active Publication Date: 2020-01-17
CHINA TOBACCO GUANGXI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is no detection method for 3-acetyl-2,5-dimethylthiophene in food additives in my country, and there is also a lack of related research

Method used

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  • A method for detecting 3-acetyl-2,5-dimethylthiophene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Determination of 3-acetyl-2,5-dimethylthiophene in potato essence

[0023] (1) Sample preparation: take 1mL of potato essence, add deionized water to make the volume to 10mL, and obtain the sample solution;

[0024] (2) Sample determination: in the sample liquid of step (1), add 5mg magnetic Fe 3 o 4 Nanoparticles, vortexed for 1min, separated from solid and liquid by an external magnetic field, and took out the supernatant; Added a mixture of 500 μL octanoic acid and 100 μL TMN-6, vortexed for 1 min to form a cloudy solution, added 300 μL of ammonia water, vortexed for 1 min , to form uniform micelles, add 1.5mL of hydrochloric acid, vortex mix for 2min, centrifuge at 4000r / min for 8min, take out the mixture of caprylic acid and non-ionic surfactant TMN-6 in the upper layer, filter it through a 0.45μm organic phase filter membrane and analyze it by HPLC , The HPLC chromatographic conditions are: mobile phase: isocratic methanol-water solution, the ratio of...

Embodiment 2

[0025] Embodiment 2: Determination of 3-acetyl-2,5-dimethylthiophene in grape essence

[0026] (1) Sample preparation: take 2mL of grape essence, add deionized water to make the volume to 10mL, and obtain the sample solution;

[0027] (2) Sample determination: in the sample liquid of step (1), add 6mg magnetic Fe 3 o 4 Nanoparticles, vortexed for 2 minutes, separated from solid and liquid by an external magnetic field, and took out the supernatant; Added a mixture of 500 μL nonanoic acid and 100 μL TMN-6, vortexed and mixed for 2 minutes to form a cloudy solution, added 400 μL ammonia water, vortexed and mixed 1min to form uniform micelles, add 1mL of hydrochloric acid, vortex mix for 1min, centrifuge at 3000r / min for 10min, take out the mixture of nonanoic acid and non-ionic surfactant TMN-6 in the upper layer, filter through a 0.45μm organic phase filter membrane and use HPLC Analysis and chromatographic conditions were the same as in Example 1, and the content of 3-acetyl...

Embodiment 3

[0028] Example 3: Determination of 3-acetyl-2,5-dimethylthiophene in beef essence

[0029] (1) Sample preparation: Weigh 2g of beef essence, add 20g of acetone, ultrasonically extract for 30min, blow with nitrogen to 1mL, dilute to 10mL with deionized water, and set aside;

[0030] (2) sample determination: sample determination: in the sample liquid of step (1), add 8mg magnetic Fe 3 o 4 Nanoparticles, vortexed for 3 minutes, separated from solid and liquid by an external magnetic field, and took out the supernatant; Added a mixture of 500 μL heptanoic acid and 100 μL TMN-6, vortexed and mixed for 2 minutes to form a cloudy solution, added 500 μL ammonia water, vortexed and mixed 2min to form uniform micelles, add 2mL hydrochloric acid, vortex mix for 3min, centrifuge at 5000r / min for 5min, take out the mixture of heptanoic acid and non-ionic surfactant TMN-6 in the upper layer, filter through a 0.45μm organic phase filter membrane and use HPLC Analysis and chromatographic c...

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Abstract

The invention discloses a method for detecting 3-acetyl-2, 5-dimethylthiophene by the aid of acid-alkali induced liquid-liquid micro-extraction and magnetic solid-phase purified high-performance liquid chromatography. According to the method, mixture of fatty acid and non-ionic surface active agents is added into detected solution with the 3-acetyl-2, 5-dimethylthiophene, alkali is added into the mixture of the fatty acid and the non-ionic surface active agents to form homogeneous phase micelles, the 3-acetyl-2, 5-dimethylthiophene is extracted, and an acid-induced phase is added to separate. The 3-acetyl-2, 5-dimethylthiophene and the mixture of the fatty acid and the non-ionic surface active agents have good affinity, extraction rate exceeds 98%, samples are purified by the aid of magnetic Fe3O4 nano particles, the content of the samples is detected by the aid of the high-performance liquid chromatography, fat in the samples can be effectively adsorbed by the magnetic Fe3O4 nano particles, the fat and the 3-acetyl-2, 5-dimethylthiophene coexist in the samples, interference of the fat to detection is removed, extraction technique is performed at the indoor temperature, extraction is finished within 20min, and the method has the advantages of simplicity and convenience in operation, rapidness, high sensitivity and the like, and detection sensitivity of the method reaches 0.5 microgram / kg.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for detecting 3-acetyl-2,5-dimethylthiophene in combination with acid-base induced liquid-liquid microextraction and magnetic solid-phase purification combined with high-performance liquid chromatography. Background technique [0002] 3-Acetyl-2,5-dimethylthiophene is used as a food flavor additive. Its aroma has a musty, vegetable root smell, nutty aroma, slightly roasted aroma, poultry meat aroma. The products can be widely used in sesame, potato, walnut, grape, mushroom, vegetable, ginseng, tropical fruit and meat essence. On June 15, 2013, the European Union issued (EU) No. 545 / 2013 Commission Regulation, amending (EC) No. 1334 / 2008 Food Flavors and Fragrances Regulations, prohibiting 3-acetyl-2,5-dimethylthiophene ( 3-acetyl-2,5-dimethylthiophene, FEMA 3527) is used in food as flavoring. On August 14, 2014, China Flavors, Fragrances and Cosmetics I...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 李小兰孟冬玲周芸陆冰琳朱静唐桂芳许蔼飞韦入丹
Owner CHINA TOBACCO GUANGXI IND