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Method for determining stable hydrogen isotope ratio of ethanol methyl site in beverage wine

A hydrogen isotope and beverage technology, applied in the field of stable isotope technology research, can solve the problems of poor universality, low analysis efficiency, high cost, etc., and achieve the effect of safe experiment, fast analysis and simple operation

Pending Publication Date: 2020-11-27
CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are two major disadvantages in this technology: ① the above-mentioned micro-distillation system needs to be specially customized to meet the requirements of a recovery rate higher than 96.5% and an ethanol concentration in the distillate greater than 95% v / v. This micro-distillation system is a patented product of the French company Eurofins , a single set needs 1.6 million yuan, and the operation process requires high proficiency of the operator, and the time for a single distillation also needs more than 4 hours; The absolute content of deuterium at the methyl site in the sample, because the content of deuterium in the natural state only accounts for 0.02% of hydrogen atoms, so in order to obtain sufficient signal-to-noise ratio and stability, the measurement time of a single sample is as long as 5h or more
It can be seen that the analysis efficiency of this technology is low, the cost is high, and the universality is poor, which seriously hinders some research and application in the field of beverage alcohol in my country

Method used

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  • Method for determining stable hydrogen isotope ratio of ethanol methyl site in beverage wine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Embodiment one The ratio of stable hydrogen isotopes at the methyl site of acetic acid (δ 2 H) and the relationship model between measured values

[0056] 1) Select three acetic acid working standard substances, denoted as 1#, 2#, 3#, and the stable hydrogen isotope ratios of the methyl sites (δ 2 H) are -223.93‰, -61.02‰ and 141.65‰ respectively;

[0057] 2) Take 2 mL of the three acetic acid standard substances in step 1), and prepare aqueous solutions with a volume concentration of 3% acetic acid content with purified water;

[0058] 3) Take 25 mL each of the three acetic acid aqueous solutions obtained in step 2), add 1 g of calcium hydroxide, vortex for 2 h, centrifuge at 8000 rpm for 30 min, and take the supernatant for later use;

[0059] 4) Freeze-dry the supernatant obtained in step 3) to remove moisture in a freeze dryer, and keep the powder for later use;

[0060] 5) Add 15mL sulfuric acid solution (1moL / L) to the powder obtained in step 4), the δ of wate...

Embodiment 2

[0066] Embodiment two Determination of Stable Hydrogen Isotope Ratios at the Methyl Sites of Ethanol in Alcoholic Beverages

[0067] Take wine, whiskey and pure ethanol as research objects, and dilute them with pure water to ethanol volume concentration of 3% respectively;

[0068] Add 50mL of the diluted sample obtained in step 1) to a 500mL reagent bottle, add 2.5mL of Acetobacter culture solution each, fill it with oxygen, seal it, and shake it at 30°C until the fermentation is terminated, and process 5 copies of each sample;

[0069] Take 25 mL of each fermented sample in step 2), add 1 g of calcium hydroxide, vortex and shake for 2 h, then centrifuge at 8000 rpm for 30 min, and take the supernatant and save it for later use;

[0070] Freeze-dry the supernatant obtained in step 3) in a freeze dryer to remove moisture, and keep the powder for later use;

[0071] Add 15mL sulfuric acid solution (1moL / L) to the powder obtained in step 4), wherein, the δ of water in the sul...

Embodiment 3

[0077] Embodiment three Verification of the accuracy of the method for the determination of stable hydrogen isotope ratios of ethanol methyl sites in alcoholic beverages

[0078] The SNIF-NMR technique is currently the official method for the determination of the hydrogen isotope ratio at the methyl site of ethanol recognized by the International Organization of Vine and Wine. In order to verify the accuracy of the method of the present invention, the three samples in Example 2 were measured using SNIF-NMR technology, and the results are shown in Table 3.

[0079] Table 3 SNIF-NMR technology and the measurement result comparison of the method of the present invention (‰)

[0080] sample wine whisky pure ethanol SNIF-NMR measurement results (D / H, ppm) 100.54 97.16 130.75 The inventive method measurement result (δ 2 H value, ‰)

[0081] As can be seen from Table 3, there is a linear positive correlation between the SNIF-NMR measurement results (D...

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Abstract

The invention provides a method for determining a stable hydrogen isotope ratio of an ethanol methyl site in beverage wine, and belongs to the field of stable isotope technology research. The method comprises the following steps: a), converting ethanol in beverage wine to be detected into acetic acid; b), determining the hydrogen isotope ratio of acetic acid in the beverage wine obtained in the step a); and c), correcting the hydrogen isotope ratio of the acetic acid measured in the step b) by using an acetic acid standard substance. The method is mainly used for measuring the stable hydrogenisotope ratio of the ethanol methyl site in the beverage wine and researching and applying in the field of beverage wine adulteration detection, and is simple to operate, safe in experiment, rapid inanalysis and suitable for analysis and test of large-batch samples.

Description

technical field [0001] The invention belongs to the field of stable isotope technology research, in particular to a method for measuring the stable hydrogen isotope ratio of alcohol methyl sites in drinking wine. Background technique [0002] The brewing industry is a traditional industry in my country and an important part of the food industry. As the world's largest producer and consumer of alcoholic beverages, in recent years, the scale of my country's brewing industry has continued to expand, and its economic benefits have increased year by year. Beverage alcohol refers to beverages with an alcohol content above 0.5% vol, including fermented alcohol, distilled alcohol and formulated alcohol. Drinking alcohol has a long history. Special raw material selection, traditional brewing technology and even unique distillation technology have created different types of alcohol and products of different quality, but at the same time it also provides opportunities for criminals to ...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28G01N33/14
CPCG01N27/62G01N33/146G01N1/28
Inventor 钟其顶王道兵
Owner CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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