Dispersive liquid liquid micro-extraction gas chromatography-mass spectrometry for detecting major higher alcohols in fermented wine

A gas chromatography and dispersion liquid-liquid technology, applied in the direction of measuring devices, material separation, analysis of materials, etc., can solve the problems of large amount of organic solvents, harmful to human health and environment, and achieve high sensitivity and easy to use

Inactive Publication Date: 2018-08-31
JIANGNAN UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it cannot be widely used due to the disadvantage that the large amount of organic solvent is harmful to human health and the environment

Method used

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  • Dispersive liquid liquid micro-extraction gas chromatography-mass spectrometry for detecting major higher alcohols in fermented wine
  • Dispersive liquid liquid micro-extraction gas chromatography-mass spectrometry for detecting major higher alcohols in fermented wine
  • Dispersive liquid liquid micro-extraction gas chromatography-mass spectrometry for detecting major higher alcohols in fermented wine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The method of detecting the content of main higher alcohols in rice wine by using dispersion liquid-liquid microextraction gas chromatography is as follows:

[0045] Determination of alcohol content of samples: Ethanol is one of the most abundant components in rice wine. The alcohol content of commercially available rice wine is between 8-17vol%. Considering that ethanol is also a good solvent, it may affect the extraction efficiency of DLLME. Therefore, using simulated wine samples with different ethanol contents, the results are as follows figure 1 As shown, the ethanol content should not exceed 12vol%, and samples with ethanol content higher than 12vol% should be diluted appropriately. Ethanol is also a common dispersant. If the ethanol content of the sample exceeds 12vol%, the DLLME extraction efficiency of the sample will decrease, which will affect the enrichment of the extractant.

[0046] Determination of sample pH: The pH value of the sample determines the de...

Embodiment 2

[0069] The method for detecting the content of main higher alcohols in wine by using dispersion liquid-liquid microextraction gas chromatography is as follows:

[0070] Wine is a typical representative of fermented wine, and DLLME is used to determine the main higher alcohols in wine. Since the extractant is quickly dispersed into the sample to form an emulsion in the DLLME extraction, the extraction can be completed in a short time. This is also an advantage of DLLME. Therefore, when optimizing the experimental conditions for the extraction of higher alcohols in wine by DLLME, the extraction time was no longer optimized, and the extraction time was set at 1 min. Alcohol content, sample pH, extractant and its volume, dispersant and its volume, sample volume and ionic strength were optimized in this experiment.

[0071] Determination of Alcohol in Samples: Ethanol is one of the most abundant components in wine. The alcohol content of commercially available wine is between 7-...

Embodiment 3

[0092] The method for detecting the content of main higher alcohols in beer by using dispersion liquid-liquid microextraction gas chromatography is as follows:

[0093] Beer and rice wine belong to the same kind of grain fermented wine. Based on the beer sample matrix, explore the method of using DLLME to determine the main higher alcohols in beer, and further promote the sample pretreatment method of the DLLME method for the determination of higher alcohols.

[0094] The difference between beer and rice wine and wine is that it contains a lot of carbon dioxide, so beer samples need to be defoamed before DLLME extraction. No chromatographic peak of 2,3-butanediol was found in the preliminary experiment of using DLLME to enrich higher alcohols in beer, which may be due to the low content of 2,3-butanediol in beer. On the other hand, after the emulsion was centrifuged for 5 minutes in the preliminary experiment stage, there was still a layer of turbid phase visible to the naked...

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Abstract

The invention discloses a dispersive liquid liquid micro-extraction gas chromatography-mass spectrometry for detecting major higher alcohols in fermented wine and belongs to the technical field of analytical chemistry. The method comprises the following steps: selecting appropriate extraction agents and dispersing agents, mixing a certain amount of extraction agents and dispersing agents with internal standard substances, rapidly injecting the mixture into a wine sample to form emulsion so as to be extracted, centrifugally collecting the extraction phase, performing gas chromatography-mass spectrometry, and quantifying through an external standard method, thereby obtaining analytical results of higher alcohols in the fermented wine. The DLLME (Dispersive Liquid Liquid Microextraction) method used for performing sample pretreatment has the advantages that the dose of an organic solvent is small, the operation is rapid, simple and convenient, the usage amount of the organic solvent is small, the detection result accuracy is high, and the recovery is satisfactory. By considering the advantages of low cost and environment friendliness, the method is easily used in practice, is particularly suitable for analysis of a large batch of samples, and can be applied to detecting the major higher alcohols in multiple kinds of fermented wine.

Description

technical field [0001] The invention relates to detection of main higher alcohols in fermented wine by dispersive liquid-liquid micro-extraction gas chromatography and belongs to the technical field of analytical chemistry. Background technique [0002] The formation of flavor in alcoholic beverages mainly depends on various flavor compounds. Flavor is one of the most important factors affecting the quality of alcoholic beverages. Higher alcohols (HAs) are one of the important flavor contributors in fermented alcoholic beverages. Higher alcohols in alcoholic beverages mainly include n-propanol, 2-methyl-1-propanol (isobutanol), 3-methyl-1-butanol (isoamyl alcohol) and β-phenylethanol, accounting for higher alcohols 70%-80% of the total amount. Although, higher alcohols have an important influence on the aroma and taste of alcoholic beverages. However, high concentrations of higher alcohols can produce an unpleasant smell similar to fusel oil, affecting the quality of alc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047G01N2030/062
Inventor 毛健张偲余永建朱胜虎周志磊倪伟
Owner JIANGNAN UNIV
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