Method for determining pyrazine compound in spirit

A compound, the technology of pyrazine, which is applied in the field of wine flavor research, can solve the problems of large sample consumption, cumbersome steps, and large loss of analytes, and achieve the effects of improved recovery, high sensitivity, and strong specificity

Inactive Publication Date: 2007-08-15
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above methods require a large amount of organic solvents, a large amount of samples, and the steps are too cumbersome, and the loss of analytes is relatively large during the pretreatment process.

Method used

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  • Method for determining pyrazine compound in spirit
  • Method for determining pyrazine compound in spirit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Optimization of solid phase microextraction conditions:

[0029] The effect of extraction temperature on adsorption sampling is two-sided: on the one hand, more analytes will escape from the matrix into the headspace when the temperature rises, which is beneficial to the headspace solid phase microextraction; on the other hand, the temperature Increasing will also reduce the ability of the extraction head to adsorb analysis components, resulting in a decrease in adsorption capacity. The present invention compares the extraction effects at 30°C, 40°C, 50°C and 60°C, and the result shows that the adsorption effect is the best at 50°C.

[0030] The solid phase microextraction process is a process of enrichment and equilibrium of the analyte between the sample matrix and the coating of the extraction head. Once the equilibrium is reached, the concentration of the analyte between the two phases becomes constant. The present invention compares the extraction effects of 10min, 30m...

Embodiment 2

[0033]Evaluation of the method: Using 2-acetylpyridine as the internal standard, the linear correlation coefficient R2 of 9 pyrazine compounds varies from 0.9908 (2,3-dimethylpyrazine) to 0.9999 (2,3,5-tri Between methylpyrazine), the linearity of the obtained standard curve is good, see Figure 2. At the same time, the linear range of the standard curve includes the concentration range of nitrogen compounds in the wine. The detection limit of 9 pyrazine compounds was less than 1μg / L, among which the detection limit of 2,3-DEP was 62.50ng / L. The overall accuracy of this method is good, and the relative standard deviation is mostly within 10%, which can meet the requirements of analysis. The present invention has done the determination of the recovery rate, and the result shows that the recovery rate of this method is all greater than 80%, as shown in Table 1.

[0034] Table 1 Recovery rate of pyrazine compounds in liquor (%, n=3)

[0035] Item

[0036] N.D.: Not detected ...

Embodiment 3

[0038] Determination of actual wine samples:

[0039] The present invention selects Moutai, Langjiu, and Gujing Gongjiu as target wine samples, dilutes the three kinds of liquor to 12% (v / v), adds 500 μL of internal standard, and determines the content of pyrazine compounds in it according to the above method. Attached Table 2 lists the content of pyrazine compounds in the tested wine samples, and Figure 3 shows the GC-FTD chromatogram of Langjiu wine samples.

[0040] Table 2 Contents of various pyrazine derivatives in different liquors (Mean±Stdev, μg / L, n=3)

[0041] Item

[0042] N.D.: Not detected.

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Abstract

This invention relates to one method to test pyrazine compound in alcohol in liquor taste study, which applies top fix phase micro extraction and gas phase spectrum and flame thermal ion test device and uses gas phase spectrum and flare thermal ion test device cross technique in liquor with strong abnormal property of compound with good linear relation for R2>0.99 and compound test limit less than 1 mu g/L; Repeating the test relative standard bias for less than 15 percent and recycle rate larger than 80 percent.

Description

Technical field [0001] A method for determining pyrazine compounds in liquor, specifically relates to a method for detecting pyrazine compounds in liquor by applying headspace solid phase microextraction and gas chromatography-flame thermionic detector technology, which belongs to the field of wine flavor research. Background technique [0002] The nitrogen-containing compounds present in liquor are mainly pyrazine compounds. Pyrazine is a six-membered heterocyclic compound containing nitrogen at the 1,4-position. Its derivatives are widely present in natural and fermented foods because they have extremely low Flavor threshold has an important contribution to the flavor of liquor. In recent years, it has received more and more attention. [0003] The content of pyrazine compounds in liquor is very small, mostly in the range of a few μg / L to hundreds of μg / L, and there are certain difficulties in qualitative and quantitative detection. Wobben et al. used vacuum distillation to rem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08G01N30/86G01N30/68
Inventor 徐岩范文来
Owner JIANGNAN UNIV
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