Method for determining acetic acid delta 13C value in fruit vinegar beverage

A fruit vinegar beverage and a technology for measuring values, which are applied in the field of determining the stable carbon isotope ratio of acetic acid in fruit vinegar beverages, can solve the problems of inability to separate acetic acid, inaccurate measurement results, time-consuming and the like, and achieve the effect of high-precision analysis and measurement

Inactive Publication Date: 2016-12-07
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

Li Xin et al. (Preliminary study on the application of stable isotope ratio technology to the identification of authenticity of vinegar) installed a reversed-phase C18 chromatographic column on liquid chromatography-stable isotope ratio mass spectrometry to achieve acetic acid δ 13 C analysis, but because the reversed-phase C18 chromatographic column lacks effective separation effect on complex components (other organic substances except acetic acid) in vinegar, it cannot be separated from acetic acid, so the method of digestion was used to remove the vinegar sample at 80 °C However, it should be noted that this process is operated under non-airtight conditions, and acetic acid is a very volatile substance. During this process, carbon isotope fractionation will occur due to the escape of part of the acetic acid, resulting in inaccurate measurement results, and The digestion step takes time to process the sample, which increases the difficulty of sample analysis

Method used

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  • Method for determining acetic acid delta 13C value in fruit vinegar beverage
  • Method for determining acetic acid delta 13C value in fruit vinegar beverage

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1.1 Instrument

[0025] Liquid chromatography-stable isotope ratio mass spectrometer (LC-IRMS, equipped with oxidation interface Isolink), the above instruments were purchased from Thermo Fisher Scientific (China) Co., Ltd.;

[0026] 1.2 Materials and reagents

[0027] Carbon isotope reference material: sucrose (IAEA-CH-6, δ 13 C PDB =-10.45‰); ultrapure water (prepared by Milli-Q system); orthophosphoric acid (purity≥99%) and sodium peroxodisulfate (purity≥99%); helium gas (purity≥99.999%); 0.22μm filter membrane (water system); sulfuric acid (purity ≥ 99%); acetic acid (purity ≥ 99%).

[0028] 1.3 Chromatographic conditions

[0029] HyperRez XP Carbohydrate H+ column (7.7×300mm / 8μm); mobile phase is 0.0005mol / L sulfuric acid solution, flow rate is 0.30mL / min; column temperature is 35°C.

[0030] 1.4 Working conditions of oxidation interface

[0031] The oxidation interface (IsoLink) uses phosphoric acid and sodium peroxodisulfate solution as reaction aids, and s...

Embodiment 2

[0044] 2.1 Instrument

[0045] Liquid chromatography-stable isotope ratio mass spectrometer (LC-IRMS, equipped with oxidation interface Isolink), the above instruments were purchased from Thermo Fisher Scientific (China) Co., Ltd.;

[0046] 2.2 Materials and reagents

[0047] Carbon isotope reference material: sucrose (IAEA-CH-6, δ 13 C PDB =-10.45‰); ultrapure water (prepared by Milli-Q system); orthophosphoric acid (purity≥99%) and sodium peroxodisulfate (purity≥99%); helium gas (purity≥99.999%); 0.22μm filter membrane (water system); sulfuric acid (purity ≥ 99%); acetic acid (purity ≥ 99%); commercially available apple cider vinegar and aged vinegar.

[0048] 2.3 Chromatographic conditions

[0049] HyperRez XP Carbohydrate H+ column (7.7×300mm / 8μm); mobile phase is 0.0005mol / L sulfuric acid solution, flow rate is 0.30mL / min; column temperature is 35°C.

[0050] 2.4 Working conditions of oxidation interface

[0051] The oxidation interface (IsoLink) uses phosphoric aci...

Embodiment 3

[0065] 3 material method

[0066] 3.1 Instrument

[0067] Liquid chromatography-stable isotope ratio mass spectrometer (LC-IRMS, equipped with oxidation interface Isolink).

[0068] 3.2 Materials and reagents

[0069] Carbon isotope reference material: sucrose (IAEA-CH-6, δ 13 C PDB =-10.45‰); ultrapure water (prepared by Milli-Q system); orthophosphoric acid (purity≥99%) and sodium peroxodisulfate (purity≥99%); helium gas (purity≥99.999%); 0.22μm filter membrane (water system); sulfuric acid (purity ≥ 99%); ethanol (HPLC grade); apple cider vinegar drink (4 in total) and apple cider vinegar (1).

[0070] 3.3 Working conditions of LC-IRMS

[0071] HyperRez XP Carbohydrate H+ column (7.7×300mm / 8μm); mobile phase is 0.0005mol / L sulfuric acid solution, flow rate is 0.30mL / min; column temperature is 35°C; oxidation interface (IsoLink) uses phosphoric acid and peroxodisulfuric acid Sodium solution is a reaction aid, and the ion current signal intensity of m / z=32, 33 and 34 is...

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Abstract

The invention discloses a method for determining acetic acid delta 13C value in a fruit vinegar beverage by using liquid chromatography-stable isotope ratio mass spectrometry, which belongs to the technical field of stable isotope analysis. The method comprises the following steps: 1) preparing an acidic mobile phase for a liquid chromatogram component; 2) adjusting the liquid chromatography-stable isotope ratio mass spectrometry to a work state; 3) determining the delta 13C value of the acetic acid in a known substance and a sample under the same condition; and 4) obtaining the delta 13C value of the acetic acid in the sample according to the systematic deviation of an apparatus. The method has the characteristics of simple operation, convenient calculation, and stable and accurate determination (the determination standard deviation is only 0.01%), and provides the assistance for promoting a stable isotope technology in adulteration detection of a fruit vinegar beverage product and is good for safety of food in our country.

Description

Technical field: [0001] The invention relates to the determination of the stable carbon isotope ratio of acetic acid in fruit vinegar beverages (denoted as δ 13 The method of C) belongs to the technical field of stable isotope analysis. Background technique: [0002] Stable isotope technology has an important role and application value in the adulteration test of food ingredients. It has been applied in the authenticity identification of foreign fruit vinegar drinks, and some achievements have been made. According to the national standard (GB30884-2014), fruit vinegar for beverages is a liquid product made from fruit or concentrated fruit juice through alcoholic fermentation and acetic acid fermentation, while fruit vinegar beverages need to use fruit vinegar for beverages as the basic raw material. Beverages prepared by adding sugar and (or) sweeteners, fruit juices, etc., are not allowed to use non-fruit fermented or artificially synthesized acetic acid such as grains. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 钟其顶王道兵
Owner CHINA NAT RES INST OF FOOD & FERMENTATION IND CO LTD
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