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Detection method of phenolic acids and/or their esters in wine and/or by-products of brewing

A detection method and by-product technology, applied in the field of chemical analysis, can solve the problems of difficult detection, weak column retention, complex components, etc., and achieve the effects of high sensitivity, extended column retention, and high detection sensitivity

Active Publication Date: 2019-02-15
WULIANGYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, due to the complex composition of wine and winemaking by-products, phenolic acids / esters are only trace substances, making detection difficult
Moreover, phenolic acids themselves contain more -OH and -COOH, which makes them have the characteristics of strong polarity and weak column retention, while phenolic acid esters have relatively weak polarity and strong column retention, so they must be separated and detected at the same time. These two types of compounds are more difficult
[0005] At present, there is no relevant report on the detection of phenolic acids and / or their esters in wine and / or by-products of winemaking. Therefore, it is urgent to provide a detection method with simple operation, high sensitivity and high accuracy.

Method used

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  • Detection method of phenolic acids and/or their esters in wine and/or by-products of brewing
  • Detection method of phenolic acids and/or their esters in wine and/or by-products of brewing
  • Detection method of phenolic acids and/or their esters in wine and/or by-products of brewing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Example 1 Using the method of the present invention to detect phenolic acid / ester compounds in liquor

[0062] LC-QTOF (high performance liquid chromatography quadrupole time-of-flight mass spectrometry instrument) liquid chromatography conditions: mobile phase: A is ultrapure aqueous solution (0.1g / L formic acid), B is methanol, gradient elution: 0 -15 min: 5-100% v / v B (the instrument automatically realizes the gradient change); 15-20 min: 100% v / v B; 20-22 min: 5% v / v B; stop elution.

[0063] The chromatographic column is a ZORBAX Eclipse Plus C18 column with a column length of 100mm, an inner diameter of 2.1mm, a particle size of 1.8μm, a column temperature of 30°C, a flow rate of 0.2mL / min, and an injection volume of 2μL.

[0064] The mass spectrometry conditions of the LC-QTOF coupled instrument are: electrospray ion source, negative mode, drying gas temperature 325°C, drying gas flow rate 10L / min, atomizing gas pressure 40psig, capillary voltage 3500v, capillary...

Embodiment 2

[0076] Example 2 Using the method of the present invention to detect phenolic acid / ester compounds in distiller's grain yellow water

[0077] a. The drawing of the standard curve is the same as in Example 1; the conditions of the liquid chromatography of the LC-QTOF coupled instrument are the same as in Example 1.

[0078] b. Take three samples of distiller's grain yellow water respectively (provided by the Analysis and Research Office of Wuliangye Technology Research Center), each 1ml, two of which are respectively added with phenolic acid standard solution 200ug / L, 2000ug / L, loading HLB, 0.01%w / w rinse with formic acid water, elute with 90% methanol water solution, dry methanol water eluent with nitrogen gas, dissolve in 1ml methanol, and inject LC-QTOF as a test sample. The total ion chromatogram of distiller's grain yellow water sample is shown in image 3 (The abscissa in the figure represents time / min, and the ordinate represents ion intensity).

[0079] c. Analysis o...

Embodiment 3

[0083] Example 3 Using the method of the present invention to detect phenolic acid / ester compounds in distiller's grains

[0084] a. The drawing of the standard curve is the same as in Example 1; the conditions of the liquid chromatography of the LC-QTOF coupled instrument are the same as in Example 1.

[0085] b. Take three samples of distiller's grains (distiller's grains samples are provided by the Analysis and Research Office of Wuliangye Technology Research Center), each 10g, two of which are added to phenolic acid standard solution 200ug / L, 2000ug / L, 50ml methanol extraction, take 10ml Evaporate the extract at 90°C to remove methanol, apply HLB after dilution with water, rinse with 0.01% w / w formic acid water, elute with 90% methanol aqueous solution, dry methanol water eluent with nitrogen, dissolve in 1ml methanol, and use it as a test sample Inject LC-QTOF. The total ion chromatogram of the distiller's grain sample is shown in Figure 4 (The abscissa in the figure r...

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Abstract

The invention discloses a detection method of phenolic acids and / or phenol esters in wine and / or wine by-products, which is detected by combining high performance liquid chromatography with mass spectrum. The high-performance liquid chromatography utilizes reversed-phase chromatography. The aqueous phase of mobile phase contains 0.1 - 1 gram per liter formic acid or acetic acid. The organic phase is methanol or acetonitrile. The mass spectrum utilizes a negative mode to detect. The detection method of phenolic acids and / or phenol esters in wine and / or wine by-products can be utilized to simultaneously separate and detect phenolic acids / esters compounds in alcoholic products such as gallic acid and ferulic acid, has the advantages of high sensitivity and accurate detection results, and is an effective method for detecting the kinds and contents of such substances in wine and wine by-products.

Description

technical field [0001] The invention relates to a detection method of phenolic acid and / or its ester in wine and / or by-products of brewing, and belongs to the technical field of chemical analysis. Background technique [0002] Phenolic acids are a class of organic acids containing phenolic rings, which have antioxidant activity and the effect of scavenging free radicals, and some corresponding phenolic ester compounds also have similar biological activities. For example, both ferulic acid and ethyl ferulate have anti-platelet aggregation, inhibit the release of platelet 5-hydroxytryptamine, inhibit the generation of platelet thromboxane A2 (TXA2), enhance the activity of prostaglandins, relieve pain, relieve vasospasm, and regulate immune function , scavenging and inhibiting oxygen free radicals, can play a role in bodybuilding and protecting the skin in the human body. [0003] There are some phenolic acids / esters in the raw and auxiliary materials of brewing. In addition,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89G01N30/06G01N30/34G01N30/88
CPCG01N30/06G01N30/34G01N30/88G01N30/89G01N2030/062G01N2030/884
Inventor 廖勤俭周韩玲李扬华安明哲练顺才乔宗伟赵东王小琴谢正敏郭艳王芳
Owner WULIANGYE
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