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Method of rapidly detecting content of ethyl carbamate in alcoholic drinks

A technology for urethane and alcoholic beverages, applied in the field of rapid detection of urethane content in alcoholic beverages, can solve the problems of poor material reuse rate, high cost, cumbersome process, etc., and achieve good accuracy and precision , the effect of high sensitivity

Inactive Publication Date: 2019-12-31
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the existing standards for the detection of EC in alcoholic beverages include SN / T 0285-2012 "Methods for the Detection of Ethyl Carbamate Residues in Exported Wine", which uses the pretreatment method of solid phase extraction combined with instrumental analysis, and is carried out by the external standard method. Quantitative, but the pretreatment of samples is very complicated in this method, the material reuse rate is poor, the cost is high, and the accuracy and stability of the external standard method need to be improved
Liquid-liquid extraction also has disadvantages such as cumbersome process and long time consumption. The extraction agent is generally a toxic chemical reagent, and improper use will cause certain harm to the operator.

Method used

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  • Method of rapidly detecting content of ethyl carbamate in alcoholic drinks
  • Method of rapidly detecting content of ethyl carbamate in alcoholic drinks
  • Method of rapidly detecting content of ethyl carbamate in alcoholic drinks

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Detection of alcoholic beverages using HS-SPME-Arrow-GC-MS

[0033] Pre-treatment method: Weigh 1.5g of sodium chloride into a 20mL headspace bottle, add 5mL of diluted wine sample with an alcohol content of 10% vol, and add 50μL of EC-D5 (10mg / L) with a micro-injector. standard, sealed with a hollow magnetic metal cap with a PTFE / blue silicone septum, and subjected to headspace SPME via an autosampler system.

[0034] HS-SPME-Arrow solid-phase microextraction technology was used to inject samples, the coating was 2cm 1.1mm / 120μm three-phase extraction head (DVB / CAR / PDMS), the extraction temperature was 60°C, the sample equilibration time was 5min, and the vibration speed was 250rmp. The depth is 22mm, the extraction time is 45min, and the sample injection depth is 38mm. After the extraction is completed, the extraction head is placed in the injection port of the gas chromatograph, desorbed at 250°C for 5min, and then the gas detection analysis is performed. ...

Embodiment 2

[0037] Embodiment 2: Selection of HS-SPME-Arrow extraction head coating

[0038] The selection of the coating fiber of the extraction head is the key to the HS-SPME-Arrow method. For 2cm 1.1mm / 100μm PDMS, 2cm 1.1mm / 100μm PA, 2cm 1.1mm / 120μm DVB / PDMS, 2cm 1.1mm / 120μm CAR / PDMS, 2cm1.1mm / 120μm DVB / CAR / PDMS five types of extraction head coating to choose, other parameters refer to Example 1, the results are as follows figure 1 shown. It can be seen that the amount of EC adsorbed by different extraction heads is different. The three-phase extraction head DVB / CAR / PDMS has the best adsorption effect, followed by CAR / PDMS and PA, and the adsorption effect of PDMS on EC is the worst. This is because the polarity, selectivity, and stability of the coatings of different materials are different. As a polar hydrophilic compound, EC has a good extraction effect with an extraction head with a polar fiber membrane, so this study chose the best adsorption effect. Good DVB / CAR / PDMS three-phas...

Embodiment 3

[0039] Embodiment 3: the selection of HS-SPME-Arrow extraction condition

[0040] When the concentration of ethanol in alcoholic beverages is high, it will significantly inhibit the adsorption of EC, so choose different alcohol dilutions 2%vol, 4%vol, 6%vol, 8%vol, 10%vol, 15%vol to test samples The EC in is detected, after diluting to corresponding alcoholic strength with ultrapure water, carry out HS-SPME-Arrow-GC-MS analysis as described in Example 1, the detected EC peak area is as follows figure 2 shown. It can be seen that with the increase of alcohol content, the EC peak area increases, but the alcohol content continues to increase, ethanol will produce competitive adsorption on the extraction head, reducing the response value of EC, so for distilled wine with high alcohol content, etc., you can The sensitivity of the assay is improved by dilution reducing the competing effect of high alcohol concentrations. Finally, 10% vol is selected as the diluted alcohol content...

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Abstract

The invention discloses a method of a method of rapidly detecting content of ethyl carbamate in alcoholic drinks and belongs to the technical field of food analysis and food safety. The invention discloses a method of rapidly detecting content of EC in alcoholic drinks by using an HS-SPME-Arrow technology. The method combines with an SIM mode of GC-MS, eliminating interference of other substance of high content; with EC-D5 as an internal standard, different pre-treatment manners, extraction head fibers, extraction conditions, detector temperature rising procedure and other methods are comparedso as to develop an economical, sensitive detection method that is widely used and is easy to quantify; the method is evaluated through a labeling recovery experiment, and requirement meeting pollution condition inspection of EC in alcoholic drinks is explained with parameters like detection limit of the method as basis; and an optimized method is used to check content of EC in alcoholic drinks commercially available, so that the method is proved being applicable in distilled wine and fermented wine.

Description

technical field [0001] The invention relates to a method for quickly detecting the content of ethyl carbamate in alcoholic beverages, belonging to the technical fields of food analysis and food safety. Background technique [0002] Alcoholic beverages (white wine, rice wine, beer, wine, etc.) are a very important part of the traditional fermentation industry, and are widely consumed globally. However, some harmful chemical substances may be derived during the fermentation process, endangering the health of consumers . In particular, the concomitant production of a multisite carcinogen called ethyl carbamate (EC) during the fermentation, heating, and storage of alcoholic beverages can cause a variety of cancers in animals and is heritable. [0003] Since EC is a low-molecular-weight substance, its detection is easily affected by the matrix effect, and it is more suitable to rely on instrumental analysis and detection. With the continuous updating of detection instruments, mo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/045G01N2030/062
Inventor 陈双徐岩高梦昕
Owner JIANGNAN UNIV