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Detection method for detecting bad smell of 2,4,6-trichloroanisole (TCA) in port wine

A wine and detector technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of complicated operation, poor repeatability, poor sensitivity, etc., and achieve the effect of simplified operation steps, low cost and high sensitivity

Inactive Publication Date: 2011-11-16
CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Generally speaking, the TCA analysis and detection methods in the prior art generally have the disadvantages of cumbersome operation, poor sensitivity, poor repeatability, and high cost, because the content of TCA in wine is an ultra-trace compound substance, and the content range is generally 0.2-41.0ng Between / L, there are more than 1,000 trace components in wine, which need to be extracted and enriched in such a complex matrix, and it is obviously difficult to separate and measure ultra-trace components

Method used

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  • Detection method for detecting bad smell of 2,4,6-trichloroanisole (TCA) in port wine
  • Detection method for detecting bad smell of 2,4,6-trichloroanisole (TCA) in port wine
  • Detection method for detecting bad smell of 2,4,6-trichloroanisole (TCA) in port wine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Column Selection and TCA Qualitative Analysis

[0039] There are many flavor components in wine, and ultra-trace TCA components are also easily interfered by other impurities when they are separated by chromatographic columns. Two chromatographic columns with different specifications and properties are selected, combined with GC chromatographic conditions optimization, to achieve TCA composition in wine.

[0040] Chromatographic column 1: DB-WAX capillary column (30m×0.25mm×0.25μm, film thickness 0.25μm, agilent technical)

[0041] Chromatographic column 2: DB-5 capillary column (30m×320μm×0.25μm, film thickness 0.25μm)

[0042] Chromatographic conditions:

[0043]Injection port temperature: 270°C, detector temperature: 330°C, nitrogen flow rate: 1ml / min, heating program: initial temperature 70°C, hold for 3min, rise to 180°C at a rate of 5°C / min, and then increase at a rate of 10°C / min Rise to 270°C and keep for 3min.

[0044] By configuring standard samples, the r...

Embodiment 2

[0047] Method evaluation:

[0048] With DCA as the internal standard, the linear correlation coefficient R2 of the TCA compound is greater than 0.997, and the detection limit of TCA is 0.5ng / L, wherein the relative standard deviation is less than 15%, which can meet the requirements of ultra-trace TCA analysis in wine. The present invention has made the recovery rate The results show that the recovery rate of the method is more than 90%, which meets the requirements of trace analysis, as shown in the table. According to the principle of the standard addition method, adding 60ng / L, 120ng / L and 240ng / L of TCA to the same wine respectively, a good linear curve was obtained, indicating that the determination of TCA in wine has a very good linear range. For details, see image 3 .

[0049] Table 1 Wine Sample Recovery Determination

[0050]

Embodiment 3

[0052] Determination of actual wine samples

[0053] This invention selects wines of major brands in my country as the target wine samples, and measures them according to the following conditions:

[0054] Sample preparation:

[0055] Take 5mL of wine sample into a 25mL headspace bottle, add 2gNaCl, then add 50μg / L DCA (internal standard) solution, and press the cap. Place in the sample tray and wait for the sample to be injected.

[0056] ITEX conditions:

[0057] Balance temperature: 60°C, balance time: 30min, balance speed: 500rpm;

[0058] Injection needle temperature: 40℃, extraction volume: 1000μl, extraction times: 30; injection volume: 700μl; extraction speed: 100μl / s; ITEX pyrolysis temperature: 200℃; pyrolysis speed: 100μl / s; ITEX cleaning temperature : 200℃, cleaning time: 10:00min

[0059] Chromatographic conditions:

[0060] Inlet temperature: 270°C Detector temperature: 330°C

[0061] Nitrogen flow rate: 1ml / min

[0062] Heating program: the initial tempe...

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Abstract

The invention provides a detection method for detecting bad smell of 2,4,6-trichloroanisole (TCA) in port wine, which belongs to the field of the quality analysis of port wine products. The TCA (2,4,6-trichloroanisole) is the main source (the TCA contamination accounts for about 80 percent of cork stopper contamination) of the cork stopper contamination. ITEX (intraductal adsorption trap) is the latest full-automatic dynamic trapping module at present, which can analyze and detect volatile or semi-volatile compounds to a great extent. The test adopts ITEX-GC-ECD to analyze and detect a trace substance TCA in the port wine, and the result shows that the ITEX can be applied to analyzing and detecting the TCA in the port wine. The method has excellent linearity and recovery rate of standard addition, and the detection sensitivity can reach 1 ng / L.

Description

technical field [0001] The invention discloses a method for analyzing and detecting ultra-trace TCA compounds in wine, specifically relating to a method for detecting TCA compounds in wine by combining adsorption and trapping in a tube with a gas chromatography-microelectronic capture detector, and belongs to the field of wine product quality analysis. Background technique [0002] The problem of cork taint is a very serious problem for the wine and cork industry. There have been frequent reports of incidents that have impacted the cork industry due to cork contamination resulting in a decline in the quality of wine. In 2002, research by people in the Burgundy wine industry showed that in each batch of wine, "problem wines that could not be marketed due to cork odors accounted for 3-5%. Further research found that the main cause of cork pollution is from 2 , 4,6-trichloroanisole (abbreviation: TCA), TCA (Cl 3 C 6 h 2 OCH 3 ) has a very low threshold. It is currently fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08G01N30/02
Inventor 钟其顶熊正河田亚琼雷安亮
Owner CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD