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Method for measuring 2-furfural in beer by using high performance liquid chromatography

A high-performance liquid chromatography and beer technology, applied in the field of beer, can solve the problems of low efficiency of enrichment methods and low content of 2-furfural, and achieve the effect of overcoming insufficient retention, high sensitivity and good retention performance

Active Publication Date: 2010-06-30
TSINGTAO BREWERY
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to overcome the shortcoming that the content of 2-furfural in beer is too low and the efficiency of commonly used enrichment methods is low, and provide a kind of high performance liquid chromatography (High Performance Liquid Chromatography, be called for short HPLC) method that detects 2-furfural in beer rapidly and accurately , it is meaningful to evaluate the freshness of beer

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  • Method for measuring 2-furfural in beer by using high performance liquid chromatography
  • Method for measuring 2-furfural in beer by using high performance liquid chromatography
  • Method for measuring 2-furfural in beer by using high performance liquid chromatography

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Embodiment Construction

[0034] (1) Standard sample preparation

[0035] Standard stock solution: Accurately weigh 100 mg of 2-furfural (99%) with a balance, and make it to 100 ml with acetonitrile to obtain 2-furfural stock

[0036] The concentration of liquid is 990mg / L. This solution is stored in the dark at 0-5°C and has a stable period of 3 months.

[0037] Standard working solution: dilute the standard stock solution with acetonitrile to an appropriate ratio, so that the concentration of the 2-furfural standard working solution is 1-2mg / L

[0038] between. This solution is stored in the dark at 0-5°C and is stable for 7 days.

[0039] (2) Pretreatment of beer to be tested

[0040]First pass through the PEP-SPE small column with 5ml acetonitrile, the PEP-SPE solid-phase extraction small column (500mg, 6ml) that Agela Company (Aijieer) (China) provides for the purification and concentration of the beer to be tested adopts, and then use 5ml ultrapure Water is passed through the cartridge to ac...

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Abstract

The invention provides a method for measuring 2-furfural in beer by using a high performance liquid chromatography. The method comprises the steps of: sample preparation, pre-treating program for the beer to be measured, gradient elution program, and comparison detecting program of beer and sample spectrogram. In the pre-treating program for the beer to be measured,the solid-phase extraction column PEP-SPE is adopted to maintain the beer 2-furfural. In the gradient elution program, a mobile phase A is 0.01% of trifluoroacetic acid aqueous solution, the mobile phase C is ultrapure water, the mobile phase D is acetonitrile, wherein the ratio of the mobile phase A is kept 95% and the ratio of the mobile phase D is kept 5% in 0 to 16 minutes; the mobile phase C is 40% and the mobile phase D is 60% in 16 to 16.5 minutes; the ratio is maintained for three minutes to thoroughly wash a chromatographic column; the ratio of the mobile phase A is recovered to 95% and the ratio of the mobile phase D is recovered to 5% in 19.5 to 20.0 minutes; the ratio is kept for 8 minutes; the whole gradient elution program is finished at the 28th minutes. The flow speed in each step is 1.0 ml per min and the ratio conversion of the mobile phase is performed in gradient linear mode. The method of the invention can efficiently purify beer and collect the 2-furfuralon the Waters Alantis C18 (250mm*46mm) chromatographic column, 0.01% of trifluoroacetic acid and acetonitrile are treated with gradient elution program, and the 2-furfural in beer can be measured with a wavelength of 280nm. The recycling ratio of the method is 99.8% to 100.2%, the repeatability RSD (n equals to 6) is equal to or less than 2.2% and the minimum detection limit is 5 ug / l.

Description

technical field [0001] The invention relates to the technical field of beer, in particular to a method for determining the content of 2-furfural in beer by using high performance liquid chromatography. Background technique [0002] 2-furfural is a symbolic substance that reflects the degree of beer aging. The higher the content of 2-furfural, the more serious the aging degree of beer. Accurate quantitative detection of it has always been an urgent need for beer production enterprises. The content of 2-furfural in fresh beer is usually less than 50ug / L, so it must be enriched, concentrated or even derivatized. [0003] Steam distillation and liquid-liquid extraction are the earliest methods of enrichment and purification. The recovery rate of liquid-liquid extraction is very low, and it is also exposed to a large amount of toxic organic solvents, which cannot be applied to routine detection. After the beer is steam distilled, the distillate needs to be derivatized with toxi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 李梅杨朝霞郝俊光杨梅单连菊董建军
Owner TSINGTAO BREWERY
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