Method for rapidly measuring ethyl carbamate content in distilled liquor

A medium-carbamate, rapid determination technology, applied in the field of analysis and detection, can solve the problems of unfavorable health of analysts, cumbersome, uneconomical and environmental protection, etc., and achieve the effect of automatic extraction and sample injection, fast and efficient, and fast and simple detection.

Active Publication Date: 2012-03-28
JIANGNAN UNIV
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Problems solved by technology

In the traditional determination method, the pretreatment method adopts the operation of liquid-liquid extraction (LLE) and solid-phase extraction (SPE), which is cumbersome, time-consuming and labor-intensive, and the process requires the use of certain harmful organic solvents, which is not conducive to the health of analysts. Healthy, but not economical and environmentally friendly

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  • Method for rapidly measuring ethyl carbamate content in distilled liquor
  • Method for rapidly measuring ethyl carbamate content in distilled liquor
  • Method for rapidly measuring ethyl carbamate content in distilled liquor

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Experimental program
Comparison scheme
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Embodiment 1

[0024] The optimization of embodiment 1 solid-phase microextraction condition:

[0025] Sample preparation is required prior to HS-SPME extraction. If the direct dilution of the sample was used to obtain the appropriate alcohol content in previous reports, the EC concentration would be too low to be detected. Considering the water solubility and boiling point of EC, it is determined to remove most of the alcohol and some low-boiling point interferences in the wine by rotary evaporation. After rotary evaporation, the alcohol content of the sample is basically around 10%vol. When the alcohol content was 10%-15%, the adsorption effect of PA head on EC was similar, that is, the EC peak area did not change much.

[0026] Extraction temperature is an important factor affecting extraction speed and efficiency. Although as the temperature increases, more analytes will escape from the matrix into the headspace, which is beneficial for headspace adsorption. However, when the tem...

Embodiment 2

[0029] The rapid determination of EC in the embodiment 2 distilled spirits

[0030] Measure 20 mL of wine sample, rotary evaporate to 10 mL, wash the rotary evaporation bottle with ultrapure water three times, dilute to the original volume, draw 8 mL into a 20 mL headspace bottle, add 5 μL PC internal standard solution (150 mg / L), then add 3 g of sodium chloride, tighten the bottle cap, insert the PA extraction head for headspace solid-phase microextraction and gas chromatography-mass spectrometry to detect EC content. The measured EC content is shown in Table 3.

[0031] The invention is suitable for quantitative detection of EC in distilled liquor with high alcohol content.

[0032] Table 1 Linearity and detection limit of EC quantification method

[0033] R 2 n Linear range (μg / L) linear equation LOD (μg / L) 0.9986 8 7.81~1000 y = 2.6985x + 0.1117 1.16

[0034] Table 2 Method precision (n = 3) and recovery

[0035] sample...

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Abstract

The invention discloses a method for rapidly measuring ethyl carbamate content in distilled liquor, belonging to the technical field of analysis measurement. In the invention, the impurities are removed by adopting rotary evaporation, the ethyl carbamate in a liquor sample is enriched by adopting headspace-solid phase microextraction technology, then gas chromatography-mass spectrum technology is adopted for conducting quantitative measurement, and the EC content in the liquor sample is calculated according to a standard curve. According to the method established in the invention, the ethyl carbamate in the distilled liquor can be detected rapidly and quantified accurately, the detection limit can be lowered to be 1.16mug / L, the linear correlation coefficient is more than 0.99, the recovery rate is 89%-119%, and the relative standard deviation is 1.26%-12.51%. In the method, a plurality of defects of in the original measuring method is overcome, the complicated pretreatment process and organic solvent are not needed, and the method is used for detection and quantitative analysis on the ethyl carbamate in the various distilled liquor with higher alcoholic strength.

Description

technical field [0001] A method for rapidly determining the content of ethyl carbamate in distilled wine relates to a method for detecting ethyl carbamate in distilled wine by applying headspace solid-phase microextraction and gas chromatography-mass spectrometry. The invention belongs to the technical field of analysis and detection. Background technique [0002] The content of ethyl carbamate (EC) in distilled liquor is very small, mostly in tens of μg / L to hundreds of μg / L. In the traditional determination method, the pretreatment method adopts the operation of liquid-liquid extraction (LLE) and solid-phase extraction (SPE), which is cumbersome, time-consuming and labor-intensive, and the process requires the use of certain harmful organic solvents, which is not conducive to the health of analysts. Healthy, but also not economical and environmentally friendly. Contents of the invention [0003] The purpose of the present invention is to provide a simple and fast metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/12
Inventor 范文来徐岩
Owner JIANGNAN UNIV
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