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Method for determining ethyl 2-aminobenzoate grape essences in wine with gas chromatography-mass spectrography

A technology of anthranilic acid and gas chromatography, which is applied in the field of determination of anthranilate grape flavor in wine by gas chromatography-mass spectrometry, can solve the problems affecting sample determination, difficult to remove impurities, complexity, etc., and achieve good recovery rate and stability, the effect of simple method

Inactive Publication Date: 2018-01-16
佛山海关综合技术中心(佛山国际旅行卫生保健中心、佛山海关口岸门诊部)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for some samples with complex background, difficult to remove impurities, and obvious matrix effects, the existing methods are easily interfered in the detection, affecting the determination of samples, and have certain limitations for confirmation

Method used

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  • Method for determining ethyl 2-aminobenzoate grape essences in wine with gas chromatography-mass spectrography
  • Method for determining ethyl 2-aminobenzoate grape essences in wine with gas chromatography-mass spectrography
  • Method for determining ethyl 2-aminobenzoate grape essences in wine with gas chromatography-mass spectrography

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Experimental program
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Effect test

Embodiment 1

[0041] The present embodiment provides a method for determining anthranilate grape essence in wine by gas chromatography-mass spectrometry, comprising the following steps:

[0042] S1. Use a pipette to accurately measure 10mL wine sample into a 50mL centrifuge tube (sparkling wine is degassed by ultrasonication at room temperature for 30min before sampling), extract with 10mL n-hexane, vortex for 2min, and then shake in a shaker 10min, fully mixed and centrifuged at 4000r / min for 5min;

[0043]S2. The extract obtained in step S1 is purified by liquid-liquid extraction to obtain the sample liquid to be tested; specifically, absorb the organic layer into another centrifuge tube. If the layering is not obvious, add a small amount of sodium chloride to saturate the lower layer , repeat the extraction once more, combine the supernatant, blow with nitrogen on a nitrogen blower at a water bath temperature of 40°C, concentrate to less than 0.5mL, dissolve the residue with ethanol and ...

Embodiment 2

[0048] The optimization experiment of embodiment 2 detection conditions

[0049] 1. Comparative test of extraction solvent

[0050] Based on the applicant's long-term and large amount of research, the basic components of wine include water, alcohol, sugar, acid, tannin, and polyphenols, and are also rich in amino acids, vitamin C, minerals, and various trace aroma components. The main volume is a polar solvent, and anthranilate grape flavors are weakly polar solutes. Therefore, only non-polar or weakly polar organic solvents can be used for the anthranilate grape flavors in wine samples. extract. It is true that the non-polar and weakly polar organic solvents that general laboratories can choose include methylene chloride, petroleum ether, n-hexane, ethyl acetate, ether, benzene, toluene, etc. However, for the wine samples to be detected in the present invention, it is necessary to solve the problem of determining the solvent in a targeted manner, not only to consider the sa...

Embodiment 3

[0069] Embodiment 3 linear range and method quantitative limit test

[0070] The prepared mixed standard series solutions 0.05, 0.10, 0.20, 0.50, 1.00 mg / L were analyzed by gas chromatography-mass spectrometry, the concentration of each grape flavor in the standard working solution was taken as the abscissa, and the quantitative ion extraction chromatographic peak area was drawn as the ordinate The standard curve, the obtained linear equation is shown in Table 2, and the three anthranilate grape flavors are in the range of 0.05-1.00mg / L, showing a good linear relationship. Add a low-concentration mixed standard working solution to the blank sample, carry out pretreatment according to the method of the present invention, and then carry out on-machine detection, and obtain 3 kinds of anthranilate grape flavors with a quantitative limit of 5 μg / L by 10 times the signal-to-noise ratio .

[0071] Table 2 Linear equation, R 2 Value and method limit of quantitation

[0072]

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Abstract

The invention discloses a method for determining ethyl 2-aminobenzoate grape essences in wine with gas chromatography-mass spectrography. A wine sample is subjected to extraction with n-hexane servingas an extractant, a selected ion monitoring mode of a gas chromatography-mass spectrometer is used for determination after specific liquid-liquid extraction purification treatment is performed, and quantitation is performed with an external standard method. Results show that the three ethyl 2-aminobenzoate grape essences in the wine show a good linear relation in the range of 0.05-1.00 mg / L, correlation coefficient r values are all larger than 0.999, the quantitation limit of the method is 5 mu g / L, the average recovery rate of the sample is 86.2%-102.4%, and the average relative standard deviation is 1.02%-8.75% (n is 6). The method is convenient, quick, accurate and sensitive, has good recovery rate and stability and is applicable to quick determination of ethyl 2-aminobenzoate grape essences in the wine.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a method for determining anthranilate grape essence in wine by gas chromatography-mass spectrometry. Background technique [0002] As a good drink, wine is loved by more and more people. It contains a lot of nutrients and has good effects on anti-oxidation, anti-aging, and prevention of coronary heart disease. However, the quality and safety of wine has always been a concern of people. There are illegal activities such as shoddy wine market and even manufacturing and selling fake wine. The main reasons for poor quality wine are: 1. The raw materials of the grapes are of poor quality; 2. During the fermentation process, the wine is diluted with water in order to save costs, which makes the taste of the wine dull, so individual manufacturers add various additives to the wine, such as: Synthetic coloring agents, sweeteners, grape flavors, etc., complement the taste and aroma of w...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
Inventor 陈丹萍谢应新杨富春曹晓燕陈彩彦原波
Owner 佛山海关综合技术中心(佛山国际旅行卫生保健中心、佛山海关口岸门诊部)
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