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Method for determining unsaturated fatty aldehyde in white spirit and method for discriminating grease smell in white spirit

A determination method and unsaturated technology, which is applied in the field of oil smell discrimination in liquor and the determination of unsaturated fatty aldehydes in liquor, can solve the problems of difficult control conditions, separation interference of analytes, and increase in operational complexity, so as to improve the quality of liquor. The effect of improving quality, improving detection efficiency, and reducing sample pretreatment time

Active Publication Date: 2022-05-10
KWEICHOW MOUTAI COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the derivatization process is more complicated, the conditions are not easy to control, and new impurities may be introduced, which not only increases the complexity of the operation, but also produces derivation by-products that interfere with the separation of the analyte.

Method used

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  • Method for determining unsaturated fatty aldehyde in white spirit and method for discriminating grease smell in white spirit
  • Method for determining unsaturated fatty aldehyde in white spirit and method for discriminating grease smell in white spirit
  • Method for determining unsaturated fatty aldehyde in white spirit and method for discriminating grease smell in white spirit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1 Comparison of the influence of different wine sample volumes on the analysis signal

[0055] In this example, in the sample pretreatment step, the influence of five liquor sample volumes of 0.5mL, 1mL, 1.5mL, 2mL, and 2.5mL on the analysis signal of the unsaturated fatty aldehyde compound to be measured is investigated. The analysis signal here Refers to the total peak area of ​​the gas chromatographic peak of the unsaturated fatty aldehyde compound to be tested. The larger the total peak area, the stronger the analysis signal, which is more conducive to the detection and analysis of the unsaturated fatty aldehyde compound to be tested.

[0056] The histograms of signal volume analysis of five kinds of liquor samples are as follows: figure 1 shown. from figure 1 It can be seen that when the sample volume of liquor is 0.5-2.5mL, the analysis signal of the unsaturated fatty aldehyde compound to be tested increases first and then decreases. When the sample volu...

Embodiment 2

[0057] Example 2 Comparison of different solid-phase microextraction heads on the effect of adsorption

[0058] The amount of liquor sample selected in the sample pretreatment step of this example is 1mL, and in the headspace solid-phase microextraction step, 85μm Carboxen / PDMS, 50 / 30μm DVB / CAR / PDMS, 65μm PDMS / DVB, 85μm Polyacrylate, 65 / 10μm PDMS / DVB-OC Five different types of solid-phase microextraction heads affect the adsorption effect of the unsaturated fatty aldehyde compound to be tested. The adsorption effect here refers to the total peak area of ​​the gas chromatographic peak of the unsaturated fatty aldehyde compound to be tested , the larger the total peak area, the better the adsorption effect, which is more conducive to the detection and analysis of the unsaturated fatty aldehyde compound to be tested.

[0059] The histogram of the adsorption effect of five different types of SPME heads is as follows: figure 2 shown. from figure 2 It can be seen that the total...

Embodiment 3

[0060] Embodiment 3 Comparison of the influence of different heating temperatures on the analysis signal

[0061] The liquor sample volume selected in the sample pretreatment step of this example is 1mL, and the 85μm Carboxen / PDMS solid phase microextraction head is selected in the headspace solid phase microextraction step for adsorption treatment of the unsaturated fatty aldehyde compound to be tested, and the tested When the sample heating temperature is 40°C, 50°C, 60°C, and 70°C, the influence of the analysis signal of the unsaturated fatty aldehyde compound to be measured, the analysis signal here refers to the total peak area of ​​the gas chromatographic peak of the unsaturated fatty aldehyde compound to be measured, the total The larger the peak area, the stronger the analysis signal, which is more conducive to the detection and analysis of the unsaturated fatty aldehyde compound to be tested.

[0062] The histograms of the analysis signals at four different heating te...

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Abstract

The invention relates to a method for determining unsaturated fatty aldehyde in white spirit, which comprises the following steps: (1) sample pretreatment: measuring a white spirit sample, diluting the white spirit sample with a solvent to obtain a diluted sample, and adding an internal standard substance into the diluted sample to obtain a sample to be detected; (2) headspace solid-phase microextraction: directly heating the to-be-detected sample obtained in the sample pretreatment step, and adsorbing unsaturated fatty aldehyde volatilized into a gas phase from the to-be-detected sample by adopting a solid-phase microextraction head; and (3) sample injection detection: inserting the solid-phase microextraction head after adsorbing the unsaturated fatty aldehyde into a sample injection port, and detecting and analyzing the unsaturated fatty aldehyde by adopting gas chromatography-mass spectrometry. According to the determination method provided by the invention, the detection efficiency of the unsaturated fatty aldehyde in the Baijiu can be improved, and meanwhile, impurity interference in detection is reduced. The invention further provides a method for discriminating the grease smell in the white spirit, the grease smell in the white spirit can be rapidly and accurately discriminated, and the method has important significance for formulating a more scientific and perfect quality control standard of the white spirit.

Description

technical field [0001] The application relates to the field of liquor flavor research, in particular to a method for determining unsaturated fatty aldehydes in liquor and a method for distinguishing oily smell in liquor. Background technique [0002] Unsaturated fatty aldehyde is an important aroma substance of rice, edible oil, fried food, etc. Studies have shown that trans, trans-2,4-decadienal and trans-2-octenal contained in vegetable oil or fried shallot oil Compounds such as phospholipids can provide a comfortable "fried flavor" in the appropriate range, but when the content is too high, it will show greasy, oily and other odors. Existing studies have shown that unsaturated fatty aldehydes have an important contribution to the aroma of liquor. The research by Xu Yan's team from Jiangnan University showed that trans-2-nonenal and trans-2-octenal are the main aroma substances of soy-flavored liquor. The team also detected 14 kinds of trans-2-ene Aldehydes and dienaldeh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/86
CPCG01N30/02G01N30/06G01N30/30G01N30/8675G01N2030/045G01N2030/062
Inventor 杨帆曹念王莉倪德让
Owner KWEICHOW MOUTAI COMPANY