Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive

A technology of dimethyl fumarate and food additives, applied in the field of food additives, can solve problems such as damage to the intestinal tract, visceral allergies, etc., and achieve the effects of easy operation, simple pretreatment, and short time-consuming method

Active Publication Date: 2015-05-13
CHINA TOBACCO JIANGSU INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, excessive intake of dimethyl fumarate can damage the intestines, internal organs and cause allergies

Method used

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  • Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive
  • Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive
  • Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A gas chromatography / mass spectrometry detection method for dimethyl fumarate in a food additive, comprising the following steps:

[0038] 1) Accurately weigh 0.2 g of the food additive sample, place it in a 25 mL Erlenmeyer flask, add 15 mL of dichloromethane extract with an internal standard concentration of 2 μg / mL, and perform ultrasonic extraction at room temperature for 15 min;

[0039] 2) The extract is filtered through an organic phase filter membrane with a pore size of 0.45 μm, and then detected by gas chromatography / mass spectrometry.

[0040] Gas chromatography / mass spectrometry analysis conditions: use DB-5MS (30m×0.25mm×0.25μm) capillary column for separation, inlet temperature: 250°C, injection volume: 1μL, split ratio: 1:10, column flow: 1mL / min, heating program: hold at 80°C for 2min, rise to 200°C at 5°C / min, hold for 2min; mass spectrometry conditions: electron ionization source (EI), ionization voltage: 70eV, ion source temperature: 230°C; quadrupole...

Embodiment 2

[0044] Same as Example 1, except that 0.1 g of the sample was weighed into a 10 mL Erlenmeyer flask, 5 mL of the extract was added and ultrasonicated for 15 min, and the extract was filtered through a 0.22 μm organic phase membrane for measurement. To obtain the content of dimethyl fumarate in the sample, add a standard sample of dimethyl fumarate to a certain food additive sample with known content, and measure the content of dimethyl fumarate in three levels of low, medium and high. Methyl ester content value. Three samples were measured in parallel for each level, and the average value was used to calculate the recovery rate of standard addition. The test results are shown in Table 1:

[0045] The recovery rate result of table 1 method

[0046]

[0047]The results in Table 1 show that the recovery rate of dimethyl fumarate is 95.86%-102.46%, indicating that the recovery rate of the method of the present invention is relatively high and meets the requirements of quantit...

Embodiment 3

[0050] A gas chromatography / mass spectrometry detection method for dimethyl fumarate in a food additive, comprising the following steps:

[0051] According to the sample processing, extraction, and analysis methods in Example 1, weigh 0.3g extract-like food additive sample into a 25mL Erlenmeyer flask, add 15mL extract and sonicate for 15min, and then filter the extract through a 0.45 μm organic phase membrane for determination.

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Abstract

The invention discloses a gas chromatography / mass spectrometry (GC / MS) method for detecting the content of dimethyl fumarate in a food additive. The method comprises the following steps: extracting the food additive by dichloromethane containing an internal standard substance, filtering an extracting solution through a filter membrane, detecting by GC / MS, and selecting an ion mode for monitoring and quantifying. The dimethyl fumarate in the food additive is measured by the GC / MS, the method is simple in pretreatment, easy to operate, low in detection cost, high in repeatability and high in recovery rate, uses few solvents, and can be used for measuring the content of dimethyl fumarate in food additives of various shapes rapidly and accurately in batches.

Description

technical field [0001] The invention relates to the technical field of food additives, in particular to a gas chromatography / mass spectrometry detection method for dimethyl fumarate in food additives. Background technique [0002] Dimethyl fumarate (commonly known as mold killer) is a new type of anti-mold preservative developed in the 1980s, widely used in leather, textiles, food, cosmetics, etc. However, excessive intake of dimethyl fumarate can damage the intestinal tract, internal organs and cause allergies. Directive 2009 / 251 / EC promulgated by the European Union stipulates that from May 1, 2009, all EU member states are prohibited from placing or selling products containing more than 0.1mg / kg of dimethyl fumarate on the market. On May 15, 2012, the European Union promulgated Directive (EU) No412 / 2012, formally approving the addition of DMF to Annex XVII of the REACH Regulation (restrictions on the manufacture, marketing and use of certain hazardous substances, mixtures...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 朱怀远尤晓娟张媛庄亚东盛金曹毅
Owner CHINA TOBACCO JIANGSU INDAL
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