# US 10,768,159 B2 · Method for tracing wine origin based on multielements and stable isotopes

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- Number: US 10,768,159 B2
- Document ID: US10768159B2
- Status: Granted
- Kind: B2
- Application number: 15/549,989
- Filed: 2016-09-05
- Published: 2019-02-28
- Granted: 2020-09-08
- Earliest claimed: 2016-06-08
- Assignees: Food Inspection Center of Ciq-Shenzhen; Shenzhen Academy of Inspection and Quarantine
- Applicants: Food Inspection Center of Ciq-Shenzhen; Shenzhen Academy of Inspection and Quarantine
- Inventors: Liqi Xie; Hao Wu; Zhi Yan; Bo Chen; Xiaolei Jin; Baohui Jin; Xuehai Bian; Xu Zhao
- Web page: https://patentgrep.com/patent/US10768159B2

## CPC

- G01N 33/146: {containing alcohol}
- G01N 30/02: Column chromatography
- G01N 30/8675: {Evaluation, i.e. decoding of the signal into analytical information (for analysis of specific compounds see also G01N30/88 and subgroups of G01N33/00; chemical libraries per se C40B)}
- G01N 33/143: {containing sugar}
- G01N 2030/025: {Gas chromatography}
- H01J 49/105: {using high-frequency excitation, e.g. microwave excitation, Inductively Coupled Plasma [ICP]}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)

## Abstract

The present application provides a method for tracing wine origin based on multielements and stable isotopes, comprising the steps of: 1) collecting wine samples from a plurality of origins; 2) filtering the wine samples collected in step 1) and using the filtrate for carbon stable isotope ratio analysis of ethanol and glycerol; using the filtrate for analyzing oxygen stable isotopes in water; performing digestion with HNO3 overnight, and diluting to a constant volume to be tested; 3) performing carbon stable isotope analysis, oxygen stable isotope ratio analysis and elemental analysis; 4) utilizing information of the origins of the wine samples and analytical data of step 3) to perform statistical modeling to obtain a wine origin discrimination model coefficient matrix and a corresponding predicted accuracy rate of the origin discrimination; and 5) determining attributes of the wine origin by using the statistical model.

## Claims

### Claim 1

A method for tracing wine origin based on multielements and stable isotopes, characterized by comprising steps of:
1) sample collection: collecting wine samples from a plurality of origins;
2) sample pre-processing: filtering each of the wine samples collected in Step 1) using a pore size of 0.22 μm aqueous filter membrane, and pouring 1.5 ml of a filtrate into an autosampler vial for carbon stable isotope ratio analysis of ethanol and glycerol; pouring 0.3 ml of the wine sample into a 12 ml glass tube with a stopper for analyzing oxygen stable isotopes in water; and pouring 0.5 ml of the wine sample into a 15 ml centrifuge tube, and adding 0.5 ml of concentrated HNO3, performing digestion overnight, and diluting to a constant volume of 10 ml to be tested;
3) sample analysis: performing carbon stable isotope analysis, oxygen stable isotope ratio analysis and elemental analysis, respectively;
4) statistical modeling: utilizing information of the origins of the wine samples and analytical data of Step 3) to perform statistical modeling to obtain a origin discrimination model coefficient matrix and a corresponding predicted accuracy rate of the origin discrimination; and
5) sample testing: performing origin discrimination by using an unknown sample in the model, and ultimately determining attributes of the origin.

### Claim 2 (depends on 1)

The method for tracing wine origin based on multielements and stable isotopes according to claim 1, characterized in that the carbon stable isotope analysis comprises steps of: switching on a host machine of a stable isotope ratio mass spectrometer and adjusting a reference gas balance, such that a variation of the carbon stable isotope ratios of CO2 reference gases is less than 0.06‰.

### Claim 3 (depends on 1)

The method for tracing wine origin based on multielements and stable isotopes according to claim 1, characterized in that the elemental analysis is performed by utilizing an Inductively Coupled Plasma-Mass Spectrometer.

### Claim 4 (depends on 1)

The method for tracing wine origin based on multielements and stable isotopes according to claim 1, characterized in that the oxygen stable isotope ratio analysis comprises steps of: switching on a Gasbench instrument, setting a chromatographic column temperature to 70° C., inflating helium containing 0.3% of CO2 by utilizing an accessory sample injector of the instrument, equilibrating at 28° C. for over 18 hours, and analyzing the oxygen stable isotope ratio of CO2 in headspace gas as a stable isotope of oxygen in water.

### Claim 5 (depends on 1)

The method for tracing wine origin based on multielements and stable isotopes according to claim 1, characterized in that a model verification step is comprised between Step 4) and Step 5), wherein the model verification step comprises steps of: grouping the data of the wine samples and importing the data into the model obtained in Step 4), providing a predicted grouping information, and calculating a verification precision of the model according to the accuracy rate of the predicted grouping information.