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A method for the determination of 3-acetyl-2,5-dimethylthiophene in edible flavors and fragrances

A technology of dimethyl thiophene and edible flavor, which is applied in the directions of measurement device, material separation, analysis of materials, etc., can solve problems such as lack of research and safety problems, and achieve the effects of good repeatability, short time consumption, and low harm

Active Publication Date: 2017-01-04
CHINA TOBACCO GUANGXI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] On June 4, 2013, the European Food Safety Authority (EFSA) published its opinion on the re-evaluation of 3-acetyl-2,5-dimethylthiophene, which believed that the substance showed mutagenicity in both in vivo and in vitro tests. There are safety problems when used as food spices
[0004] Edible flavors and fragrances are an indispensable part of food production, their safety is an important aspect of food safety, and the source of safety control is the raw materials for production. Literature research shows that: at present, there is no 3-acetyl in flavors and fragrances in my country The detection method of 3-acetyl-2,5-dimethylthiophene is also lack of relevant research. In order to ensure the safety of food additives, it is necessary to establish the determination of 3-acetyl-2,5-dimethylthiophene in food flavors and fragrances. method

Method used

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  • A method for the determination of 3-acetyl-2,5-dimethylthiophene in edible flavors and fragrances
  • A method for the determination of 3-acetyl-2,5-dimethylthiophene in edible flavors and fragrances
  • A method for the determination of 3-acetyl-2,5-dimethylthiophene in edible flavors and fragrances

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Instruments and reagents

[0025] Gas chromatography-mass spectrometry (Thermo TRACE 1300) chromatographic column (Thermo TG-WAXMS, 30m×0.25mm×0.25μm), Millipore Q-pod Element ultrapure water system (Millipore, USA); AB204-S electronic analysis Balance (sensitivity 0.0001g) (Mettler, Switzerland), 0.22 μm microporous filter membrane, ultrasonic cleaner.

[0026] Ultrapure water (18MΩ), ethanol (chromatographically pure, Bailingwei Chemical Reagent Company), 250pmoL / μL, Agilent).

[0027] 2. Solution preparation

[0028] (1) Internal standard solution preparation

[0029] Internal standard stock solution: Accurately weigh 0.0365g (accurate to 0.0001g) of diethyl oxalate in a 50mL volumetric flask, dissolve with absolute ethanol and constant volume to obtain 0.73g / L internal standard mother solution. Store in a cool, dry place to prevent moisture.

[0030] Internal standard extract: pipette 1mL of internal standard stock solution into a 1000mL volumetric flask, dil...

Embodiment 2

[0040] The present embodiment detects the standard addition recovery rate of the present invention, and analysis method is as follows:

[0041] Taking the sample containing 3-acetyl-2,5-dimethylthiophene detected in Example 1 as the object, referring to the method of Example 1, using the method of adding standard at three levels of low, medium and high, adding 3 -Acetyl-2,5-dimethylthiophene standard sample, measure its content after adding standard. Each level was measured in parallel three times, and the average value was taken to calculate the recovery rate of the standard addition. The measurement results are shown in Table 1:

[0042] Table 1 Method spike recovery

[0043]

[0044] It can be seen from Table 1 that the recovery rate of the standard addition of the sample is between 95.91-100.23%, indicating that the recovery rate of this method is better.

Embodiment 3

[0046] The present embodiment detects the precision of the present invention, and analysis method is as follows:

[0047] Taking the sample containing 3-acetyl-2,5-dimethylthiophene detected in Example 1 as the object, referring to the method of Example 1, 6 parallel determinations of 3-acetyl-2,5-dimethylthiophene in the spiked sample The content of dimethylthiophene, calculate relative standard deviation, investigate the precision of method, the result is as shown in table 2,

[0048] The precision of the method in Table 2

[0049]

[0050]It can be seen from Table 2 that the relative standard deviation RSD of this method is less than 3%, indicating that the method has good repeatability and meets the experimental requirements.

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Abstract

The invention relates to a method for measuring 3-acetyl-2, 5-dimethyl thiophene in edible flavor and fragrance. The method comprises the steps of selecting an absolute ethyl alcohol ultrasonic extraction sample containing an internal standard for use in the pretreatment process, enabling extract liquor to directly enter a gas chromatograph-mass spectrometer for measurement after the extract liquor passes through a filtering membrane, detecting in an ion mode, and quantifying by an internal standard method. The method for measuring 3-acetyl-2, 5-dimethyl thiophene in edible flavor and fragrance by the gas chromatograph-mass spectrometer is simple in sample treatment, easy to operate, low in detection cost, good in repeatability and high in recovery rate, and is capable of rapidly and accurately measuring the content of 3-acetyl-2, 5-dimethyl thiophene in flavor and fragrance in batches; furthermore, harmful and toxic chemicals are not used in the experiment process, so that the method is less in harm to an operator and free from pollution to environment.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical testing of food additives, and in particular relates to a method for determining 3-acetyl-2,5-dimethylthiophene in food flavors and fragrances. Background technique [0002] On June 4, 2013, the European Food Safety Authority (EFSA) published its opinion on the re-evaluation of 3-acetyl-2,5-dimethylthiophene, which believed that the substance showed mutagenicity in both in vivo and in vitro tests. There are safety problems when used as food spices. On June 14, 2013, the European Commission passed regulations ( Regulation (EC) No 545 / 2013 ), prohibiting the use of 2,5-dimethyl-3-acetyl-thiophene as a food spice, and deleting it from the list of food spices in Appendix I of the Food Spice Regulations. [0003] Before August 2013, my country allowed the use of 3-acetyl-2,5-dimethylthiophene as a food spice. This substance is included in the "List of Synthetic Spices Allowed for Food ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 徐雪芹田兆福李小兰陈志燕贾海江许蔼飞周肇峰
Owner CHINA TOBACCO GUANGXI IND
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