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Method for simultaneously measuring 10 volatile phenol compounds in white spirit

A technology of phenolic compounds and volatility, applied in the field of simultaneous determination of 10 volatile phenolic compounds in liquor

Inactive Publication Date: 2012-07-18
GUIZHOU PROVINCIAL PRODUCT QUALITY SUPERVISION AND INSPECTION INSTITUTE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on the application of dispersion liquid-liquid microextraction to the determination of volatile phenolic substances in Chinese liquor

Method used

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  • Method for simultaneously measuring 10 volatile phenol compounds in white spirit
  • Method for simultaneously measuring 10 volatile phenol compounds in white spirit
  • Method for simultaneously measuring 10 volatile phenol compounds in white spirit

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Embodiment 2

[0162] Embodiment 2 of the present invention. A method for simultaneously measuring 10 kinds of volatile phenolic compounds in liquor, comprising the following steps,

[0163] After the wine sample was diluted with wine / water (1:1), 5 mL of the diluted wine sample was taken, and 1.5 mL of a mixed solvent composed of a dispersant and an extractant (THF: CH 2 Cl 2 =7:3, V / V) After ultrasonication for 20min, centrifuge at 3000r / min for 5min to separate the precipitated organic phase from the wine phase, carefully transfer the lower organic phase into a 25mL pear-shaped bottle, add 0.2mL, 0.075MPa at 35°C Concentrate by rotary evaporation, and finally dilute to 1.3 mL with 1% glacial acetic acid aqueous solution, pass through a 0.45 μm filter membrane for HPLC analysis.

[0164] HPLC detection Chromatographic conditions: Chromatographic column: Synergi 4u Hydro-RP 80A, 150×4.6mm; mobile phase consists of mobile phase A and mobile phase B, mobile phase A: glacial acetic acid / β-cy...

Embodiment 3

[0168] Embodiment 3 of the present invention. A method for simultaneously measuring 10 kinds of volatile phenolic compounds in liquor, comprising the following steps,

[0169] After the wine sample was diluted with wine / water (1:1), 5 mL of the diluted wine sample was taken, and 2.0 mL of a mixed solvent (THF: CH 2 Cl 2 =7:3, V / V) After ultrasonication for 20min, centrifuge at 3000r / min for 5min to separate the precipitated organic phase from the wine phase, carefully transfer the lower organic phase into a 25mL pear-shaped bottle, add 0.2mL of 1% glacial acetic acid aqueous solution, Concentrate by rotary evaporation at 35°C and 0.075MPa, and finally dilute to 1.5mL with 1% glacial acetic acid aqueous solution, pass through a 0.45μm filter membrane for HPLC analysis.

[0170] HPLC detection Chromatographic conditions: Chromatographic column: Synergi 4u Hydro-RP 80A, 150×4.6mm; mobile phase consists of mobile phase A and mobile phase B, mobile phase A: glacial acetic acid / β-...

Embodiment 4

[0174] Embodiment 4 of the present invention. A method for simultaneously measuring 10 kinds of volatile phenolic compounds in liquor, comprising the following steps,

[0175] After the wine sample was diluted with wine / water (1:1), 5 mL of the diluted wine sample was taken, and 2.0 mL of a mixed solvent (THF: CH 2 Cl 2 =6:4, V / V) After ultrasonication for 20min, centrifuge at 3000r / min for 5min to separate the organic phase precipitate from the wine phase, carefully transfer the lower organic phase into a 25mL pear-shaped bottle, add 0.2mL of 1% glacial acetic acid aqueous solution, Concentrate by rotary evaporation at 35°C and 0.075MPa, and finally dilute to 1.5mL with 1% glacial acetic acid aqueous solution, pass through a 0.45μm filter membrane for HPLC analysis.

[0176] HPLC detection Chromatographic conditions: Chromatographic column: Synergi 4u Hydro-RP 80A, 150×4.6mm; mobile phase consists of mobile phase A and mobile phase B, mobile phase A: glacial acetic acid / β-c...

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Abstract

The invention discloses a method for simultaneously measuring 10 volatile phenol compounds in white spirit and establishes a method for measuring volatile phenol in the white spirit through dispersing liquid-liquid microextraction-FLD-HPLC. When a dispersant is tetrahydrofuran, aether, ethanol, propanol, isopropanol, acetone or a mixture thereof, an extracting agent is dichloromethane or chloroform, the mixing ratio of the dispersant to the extracting agent is 7:3, 6:4 and 5:5, and the total volume using amount is 1.5 and 2ml, 5ml of diluted white spirit sample is extracted and the 10 volatile phenol compounds are measured, wherein the labeling recovery rate is 81.0 to 103.4 percent; the RSD value is 0.9 to 3.1 percent; and the detection limit is 0.0025 to 0.0506 ug / mL. Compared with the traditional liquid-liquid extraction method, the method has the advantages of small using amount of the sample, small using amount of the organic solvent, short pretreatment time and, the like.

Description

technical field [0001] The invention relates to a method for simultaneously measuring 10 kinds of volatile phenolic compounds in liquor, belonging to the technical field of liquor detection. Background technique [0002] Beverage alcohol usually contains some phenolic substances. They have been found in beer, wine and distilled spirits. Volatile phenolic compounds are important aroma components of drinking wine. Since this type of component plays an important role in the smell, taste and stability of wine, it has attracted the attention of many researchers. [0003] In 1978, the Food Fermentation Research Institute of the Ministry of Light Industry of China took Moutai as the main research object. In the analysis and research of volatile phenolic compounds in liquor by chemical derivation method combined with GC-FID / GC-MS, the pre-treatment is cumbersome and requires derivation and the addition recovery of 4-methylguaiacol and 4-ethylguaiacol is only about 40%. [0004] I...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 寻思颖杨敏冯永渝彭黔荣耿平兰张倩孙棣董睿黄卫红吴力菊
Owner GUIZHOU PROVINCIAL PRODUCT QUALITY SUPERVISION AND INSPECTION INSTITUTE
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