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Method for measuring hydrogen isotope ratio of ethanol in grape wine

A technology of isotope ratio and hydrogen isotope, which is applied in the field of research and daily inspection, can solve the problems of inaccurate measurement of ethanol hydrogen isotope, long pretreatment time, and high requirements for operators, so as to avoid isotope fractionation, small sample consumption and long analysis time short effect

Inactive Publication Date: 2016-08-17
CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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  • Abstract
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Problems solved by technology

The method of purifying ethanol using headspace-solid phase microextraction has been reported ("Determination of hydrogen, carbon and eoxygenisotope ratios of ethanol in aqueous solution at millimole levls" and "An improved method for the measurement of the isotope ratio of ethanol in various samples, including alcoholic and non-alcoholic beverages"), but this technology is prone to lead to inaccurate ethanol hydrogen isotope fractionation in the pretreatment process, and the pretreatment time is longer (75min after improvement), and manual injection is required , Higher requirements for operators

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  • Method for measuring hydrogen isotope ratio of ethanol in grape wine
  • Method for measuring hydrogen isotope ratio of ethanol in grape wine

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Experimental program
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Effect test

Embodiment 1

[0034]Embodiment one: installation packing is the capillary chromatographic column of bonded styrene-divinylbenzene porous polymer (embodiment two and embodiment three also adopt same capillary chromatographic column), determine ethanol retention time:

[0035] a) Using absolute ethanol, water, acetone and methanol as experimental materials, take each pure reagent and put them into 2mL sample bottles and mix them in equal proportions, put them into 2mL sample bottles, and put them in the sample tray for determination;

[0036] b) Set GC condition parameters: injection volume 0.1uL; injection port temperature: 200°C; constant flow mode: 1.2mL / min; split injection mode: 100:1; / 160℃ / 4min / / 15 / / 210℃ / 1min;

[0037] c) Confirm that the working environment, airtightness, and vacuum degree of the ion chamber of the stable isotope ratio mass spectrometer meet the requirements, and then test the instrument to measure H 2 The precision and stability of δD in the medium, adjust the ion s...

Embodiment 2

[0044] a) 5 wine samples and 1 beet alcohol sample were diluted 100 times with acetone,

[0045] Put it into a 2mL sample bottle, put it in the sample tray and wait for the determination;

[0046] b) Set GC condition parameters: injection volume 1uL; injection port temperature: 200°C; constant flow mode: 1.0mL / min; split injection mode: 20:1; 78℃ / 1min / / 15 / / 200℃ / 10min;

[0047] c) Confirm that the working environment, airtightness, and vacuum degree of the ion chamber of the stable isotope ratio mass spectrometer meet the requirements, and then test the instrument to measure H 2 The precision and stability of δD in the medium, adjust the ion source parameter value if necessary;

[0048] d) Set cracking tube parameters: cracking tube temperature is 1420°C;

[0049] e) Optimizing the reaction conditions of the pyrolysis tube: after the temperature of the pyrolysis tube reaches 1420°C, a certain volume of CH is introduced 4 The gas is coated with a layer of C inside the cracki...

Embodiment 3

[0057] a) Choose wine sample 5# and edible alcohol from sugar beet as experimental objects, according to the ethanol content in the wine: beet alcohol = 1: 3 (referred to as "simulated sample-1"), 1: 1 (referred to as "simulated sample-1") 2") and 3:1 (referred to as "simulated sample-3"), add beet alcohol to the wine to prepare a simulated sample, dilute it with acetone 100 times, put it into a 2mL sample bottle, put it in the sample tray and wait Determination;

[0058] b) Set GC condition parameters: injection volume 1uL; injection port temperature: 200°C; constant flow mode: 1.0mL / min; split injection mode: 20:1; 78℃ / 1min / / 15 / / 200℃ / 10min;

[0059] c) Confirm that the working environment, airtightness, and vacuum degree of the ion chamber of the stable isotope ratio mass spectrometer meet the requirements, and then test the instrument to measure H 2 The precision and stability of δD in the medium, adjust the ion source parameter value if necessary;

[0060] d) Set cracki...

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Abstract

The invention relates to a method for measuring the hydrogen isotope ratio of ethanol in grape wine and belongs to the technical field of stable isotope analysis. The method comprises the steps that (1) hydrogen isotope is used for forming a known to-be-tested water treatment sample; (2) acetone is used for diluting a fermentation ethanol sample treated by water, and the mixture is mixed for use; (3) a liquid sample injection needle is used for sample injection, and gas chromatography equipped with a molecular sieve capillary chromatographic column is used for separating ethanol, acetone, water and other hydrogen compounds; (4) an on-line cracking device is used for converting ethanol into hydrogen; (5) CF-IMRS is used for measuring the hydrogen delta D produced by the ethanol; (6) correction computation of delta DSMOW of sample ethanol is performed according to the delta D measured value of an ethanol isotopic reference material. According to the method for measuring the hydrogen isotope ratio of ethanol in grape wine, GC-TC-IRMS is used for measuring the hydrogen isotopic compositions of the fermentation ethanol, and the technical difficulty of series of pretreatment of ethanol purification before measurement of fermentation ethanol hydrogen isotope in the past is solved; advance of the ethanol hydrogen isotope measurement technology can be promoted, and a technical method is provided for source identification of fermentation ethanol, sugar mixing detection of a plant source product and study of metabolic pathways in future.

Description

Technical field: [0001] The invention relates to a method for measuring the hydrogen isotope ratio of ethanol in ethanol-containing solution (for example, wine) by using online technology, belongs to the technical field of stable isotope analysis, and can be used for research and daily inspection in the field of food authenticity identification. Background technique: [0002] Since the reform and opening up, wine has gradually been recognized by Chinese consumers for its healthy and fashionable cultural connotation, and has become the wine with the most development space and potential consumption market in the wine industry. At present, my country has become the fifth largest wine consumer and the No. Top six wine producing countries. [0003] As the saying goes, "Seven points to raw materials, three points to craftsmanship", the quality of wine grapes plays a decisive role in the quality of wine, and the factors that affect the quality of wine grapes are not only the choice ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/025G01N2030/8868
Inventor 钟其顶王道兵
Owner CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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