A method for determining trace amount of ethyl carbamate in fermented food

A technology of urethane and fermented food, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., and can solve problems such as difficult to achieve accurate determination of urethane, insufficient repeatability and accuracy, and difficulty in batch determination of samples , achieve the effect of strong innovation, good repeatability and recovery rate, and reduce errors

Active Publication Date: 2017-07-14
CHINA TOBACCO JIANGSU INDAL
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

Gas chromatography / mass spectrometry generally uses two or more different types of solid phase extraction cartridges or a combination of solid phase extraction and matrix dispersion extraction to purify the sample, and then uses a large amount of solvent to elute the amino groups in the extract. For ethyl formate, the eluent is concentrated and then measured. A large amount of organic solvents are used in the experiment. The analysis cost is high, and it is time-consuming and cumbersome. It is difficult to achieve batch determination of a large number of samples.
When the liquid chromatography-fluorescence detector method is used, the sample needs to undergo a derivatization process, and the reaction is required to be carried out under acidic and light-proof conditions. More importantly, the repeatability and accuracy of this method are not high enough, and it can be used It is suitable for the screening of samples, but it is difficult to realize the accurate determination of ethyl carbamate in samples

Method used

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  • A method for determining trace amount of ethyl carbamate in fermented food
  • A method for determining trace amount of ethyl carbamate in fermented food
  • A method for determining trace amount of ethyl carbamate in fermented food

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0051] (1) Preparation of internal standard solution: D5-ethyl carbamate (hereinafter referred to as D5-EC) was used as internal standard substance and acetonitrile was used as solvent to prepare internal standard solution.

[0052] (2) Preparation of standard working solution: take urethane (hereinafter referred to as EC) standard substance as target, use acetonitrile as solvent, prepare standard stock solution through stepwise dilution, and then add a certain amount of internal standard solution respectively , prepared as a standard working solution.

[0053] (3) Preparation of sample solution: Accurately weigh a food sample of a certain quality, add a certain volume of water for ultrasonic extraction to obtain an extract; then use a C18 solid-phase extraction column to purify to obtain a purified solution; then use dichloromethane as Solvent, using a diatomaceous earth solid phase extraction column to back-extract the purified solution to obtain a eluent; finally, concentra...

Embodiment 1

[0074] The present embodiment is as follows to the detection method of trace urethane in fermented food (the flow chart of described detection method is as follows figure 1 shown):

[0075] (1) Preparation of internal standard solution

[0076] ①Internal standard stock solution: Accurately weigh 0.5200g of D5-EC, dissolve it in acetonitrile in a 100mL volumetric flask and bring the volume up to the mark. ②Internal standard solution: Accurately pipette 0.1mL internal standard stock solution, dilute it with acetonitrile in a 100mL volumetric flask, and adjust the volume to the mark. The concentration of D5-EC is 5.2μg / mL.

[0077] (2) Preparation of standard working solution

[0078] ① Primary standard stock solution: Accurately weigh 0.5000g EC, dissolve it in acetonitrile in a 100mL volumetric flask, and dilute to the mark. ②Secondary standard stock solution: Accurately pipette 0.1mL primary standard stock solution into a 100mL volumetric flask, dilute with acetonitrile and...

Embodiment 2

[0104] The present embodiment is as follows to the detection method of the precision of the present invention and the standard addition recovery rate:

[0105] Taking the yoghurt sample used in Example 1 as the analysis object, the intraday precision experiment was carried out respectively. The intraday precision experiment was that the same sample was measured in parallel 6 times under the same conditions (same batch processing), and the results of 6 parallel measurements were calculated respectively. The relative standard deviation (RSD) of the measurement results are shown in the table below. The results in the table show that the intraday repeatability RSD of this experimental method is less than 10%, which indicates that the method has good precision for the quantitative analysis of trace substances.

[0106] The precision results of the method

[0107]

[0108]

[0109] Taking the yogurt sample used in the repeatability test as the analysis object, it was processe...

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Abstract

The invention discloses a method for determining trace ethyl carbamate (EC) in fermented food, and particularly relates to a method for determining trace ethyl carbamate in fermented food on the basis of a gas chromatography-tandem mass spectrometer. The method comprises the steps of preparation of an internal standard solution, a standard work solution and a sample solution, analysis of the gas chromatography-tandem mass spectrometer, calculation of a determined result and the like. According to the method, quantification is performed by taking a deuterated substance of a target substance as an internal standard substance, the optimized detection method is sensitive in response and accurate in quantitative analysis, interference brought due to the fact that a sample matrix is complex is effectively reduced, the target substance has the better signal response and the better linear dependence through the adopted analysis instrument conditions, the detection limit is 0.0259 ng / g, the repeatability (RSD) is 9.10%, the adding standard recovery rate ranges from 84.87% to 105.43%, and therefore the method is high in sensitivity and better in repeatability and recovery rate and suitable for quantitative analysis of trace ethyl carbamate in the fermented food.

Description

technical field [0001] The invention discloses a method for measuring trace amount of ethyl carbamate (EC) in fermented food, in particular to a method for measuring trace amount of ethyl carbamate in fermented food based on gas chromatography-tandem mass spectrometer The method belongs to the technical field of food physical and chemical index detection. Background technique [0002] Urethane, also known as urethane, is widely found in various fermented foods and is a potential carcinogen that can cause various diseases such as lung cancer, lymphoma, liver cancer and skin cancer, according to the International Agency for Research on Cancer of the World Health Organization (IARC) classified it as a 2A carcinogen. The 64th meeting of the United Nations Food and Agriculture Organization / World Health Organization (FAO / WHO) Joint Expert Committee on Food Additives (JECFA) suggested that in order to protect human health, fermented beverages should be reduced as much as possible. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025G01N2030/045G01N2030/062
Inventor 廖惠云庄亚东王晨辉刘献军熊晓敏石怀王珂清李朝建张媛韩开冬尤晓娟张华
Owner CHINA TOBACCO JIANGSU INDAL
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