Detection method of pyrazine compounds in Jiang-flavour Chinese spirit

A sauce-flavored liquor and detection method technology, applied in the field of liquor detection, can solve problems such as poor selectivity, quantitative influence, and reduced sensitivity

Inactive Publication Date: 2016-02-24
GUIZHOU PROVINCIAL PRODUCT QUALITY SUPERVISION AND INSPECTION INSTITUTE +1
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  • Application Information

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Problems solved by technology

In the experiment, it was found that while detecting pyrazine compounds by means of full scan, it will also be interfered by esters and alcohol compounds, which will affect the quantification
[0006] In 2009, Kweichow Moutai Co., Ltd. used gas chromatography-mass spectrometry-ion scanning to quickly determine 4 pyrazine compounds in liquor (China Brewing, 2009, 204(3), 148-150). According to the same method, it was determined that the four pyrazine compounds with higher content in Moutai liquor were 2-ethyl-6-methylpyrazine, 2,3,5-trimethylpyrazine, 2,3,5,6- Tetramethylpyrazine and 2,3-dimethyl-5-ethylpyrazine, although the pretreatment time of the sample is shortened, but the large amount of water contained in the wine sample will cause great damage to the high vacuum system of the mass spectrometer. In order to reduce the damage to the instrument, the injection volume was reduced to 0.2μL, which also reduced the detection sensitivity. The detection limit of the four compounds was about 0.2mg / L, so this method only determined the relatively low content of Moutai wine. High 4 pyrazine compounds
In addition, the types of extraction fiber heads are limited, the selectivity is poor, there are many affected factors, and the repeatability is relatively poor. The sensitivity, accuracy and precision of this method for the detection of some pyrazines need to be improved.

Method used

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  • Detection method of pyrazine compounds in Jiang-flavour Chinese spirit
  • Detection method of pyrazine compounds in Jiang-flavour Chinese spirit
  • Detection method of pyrazine compounds in Jiang-flavour Chinese spirit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] A detection method for pyrazine compounds in Maotai-flavor liquor, comprising the steps of:

[0108] (1) Accurately weigh 2,3,5-trimethylpyrazine, 2,3,5,6-tetramethylpyrazine, 2,3-dimethyl-5-ethylpyrazine, 2-ethylpyrazine, Base-6-methylpyrazine, 2,6-dimethylpyrazine, 2,3-dimethylpyrazine, 2,5-dimethylpyrazine and 2-methylpyrazine reference substance 100mg each, with methanol Dilute to 10mL, make 10mg / mL standard stock solution, and dilute with pure water into pyrazine mixed reference substance with mass concentration from low to high in order of 20ppb, 50ppb, 100ppb, 200ppb, 500ppb, 1000ppb, 2000ppb, 5000ppb solution. Linear regression was performed on the mass concentration (X, ng / mL) of the peak area (Y) to establish a calibration curve for the eight pyrazine compounds for quantitative calculation by the external standard method.

[0109] (2) Shake the Maotai-flavor liquor sample at 53 degrees, take 2mL and pass it through a 0.22μm filter membrane for analysis by HP...

Embodiment 2

[0113] A detection method for pyrazine compounds in Maotai-flavor liquor, comprising the steps of:

[0114] (1) Accurately weigh 2,3,5-trimethylpyrazine, 2,3,5,6-tetramethylpyrazine, 2,3-dimethyl-5-ethylpyrazine, 2-ethylpyrazine, Base-6-methylpyrazine, 2,6-dimethylpyrazine, 2,3-dimethylpyrazine, 2,5-dimethylpyrazine and 2-methylpyrazine reference substance 100mg each, with methanol Dilute to 10mL, make 10mg / mL standard stock solution, and dilute with pure water into pyrazine mixed reference substance with mass concentration from low to high in order of 20ppb, 50ppb, 100ppb, 200ppb, 500ppb, 1000ppb, 2000ppb, 5000ppb solution. Linear regression was performed on the mass concentration (X, ng / mL) of the peak area (Y) to establish a calibration curve for the eight pyrazine compounds for quantitative calculation by the external standard method.

[0115] (2) Shake the Maotai-flavor liquor sample at 53 degrees, take 2mL and pass it through a 0.22μm filter membrane for analysis by HP...

Embodiment 3

[0119] A detection method for pyrazine compounds in Maotai-flavor liquor, comprising the steps of:

[0120] (1) Accurately weigh 2,3,5-trimethylpyrazine, 2,3,5,6-tetramethylpyrazine, 2,3-dimethyl-5-ethylpyrazine, 2-ethylpyrazine, Base-6-methylpyrazine, 2,6-dimethylpyrazine, 2,3-dimethylpyrazine, 2,5-dimethylpyrazine and 2-methylpyrazine reference substance 100mg each, with methanol Dilute to 10mL, make 10mg / mL standard stock solution, and dilute with pure water into pyrazine mixed reference substance with mass concentration from low to high in order of 20ppb, 50ppb, 100ppb, 200ppb, 500ppb, 1000ppb, 2000ppb, 5000ppb solution. Linear regression was performed on the mass concentration (X, ng / mL) of the peak area (Y) to establish a calibration curve for the eight pyrazine compounds for quantitative calculation by the external standard method.

[0121] (2) Shake the Maotai-flavor liquor sample at 53 degrees, take 2mL and pass it through a 0.22μm filter membrane for analysis by HP...

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Abstract

The present invention discloses a detection method of pyrazine compounds in Jiang-flavour Chinese spirit, according to the method, qualitative and quantitative analysis of the pyrazine compounds in the Jiang-flavour Chinese spirit can be performed by high performance liquid chromatography-tandem mass spectrometry, and eight pyrazine compounds of 2-methyl pyrazine, 2,3-dimethyl pyrazine, 2,5-dimethyl pyrazine, 2,6-dimethyl pyrazine, 2,3, 5-trimethyl pyrazine, 2-ethyl-6-methyl pyrazine, 2,3,5,6-tetramethyl pyrazine, 2,3-dimethyl-5-ethyl-pyrazine in the Jiang-flavour Chinese spirit can be simultaneously detected by the method. A sample directly passes through into a membrane for sample injection, no chiral column or chiral additive is used for isomeride resolution in the chromatography, sample derivatization is not needed, and the method has the advantage of high sensitivity, good accuracy and repeatability, and simple operation.

Description

technical field [0001] The invention relates to a method for detecting pyrazine compounds in Maotai-flavor liquor, belonging to the technical field of liquor detection. Background technique [0002] In recent years, there has been increasing interest in nitrogenous compounds in food. This is mainly due to the fact that these compounds, especially pyrazine compounds, have a unique role in forming the flavor of food. The domestic liquor industry gradually regards this type of compound as one of the important components of the flavor of liquor, because they have a very low It also has an obvious contrast and superposition effect on other aroma substances, which can make the aroma of the liquor more full and make an important contribution to the flavor of the liquor. [0003] For the Chinese liquor industry, after the era of light fragrance and strong fragrance, the world of sauce-flavored liquor has come, and more and more consumers prefer sauce-flavored liquor. At present, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 孙棣冯永渝杨敏赵贵斌田志强寻思颖龙四红黄家岭赵应梅杨波廖妍俨袁荟琳
Owner GUIZHOU PROVINCIAL PRODUCT QUALITY SUPERVISION AND INSPECTION INSTITUTE
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