Method for tracing producing area of Xinjiang grape wine
By measuring the isotope ratios of δ13C, δ2H and δ18O in wine and combining the discriminant function equations, the accuracy and adaptability of the origin traceability of Xinjiang wine was solved, and efficient and accurate origin traceability was achieved, which was suitable for the three major production areas in Xinjiang.
Patent Information
- Application Number
- CN202510498197.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-21
- Publication Date
- 2025-05-30
AI Technical Summary
The application effect and adaptability of existing wine origin traceability technology in Xinjiang has not been fully verified, especially the chemical analysis methods based on elemental components are affected by the brewing process and are difficult to accurately trace the source, while the application effect of stable isotope technology in specific production areas of Xinjiang still needs further verification.
By measuring the ratio of the three isotopes of δ13C, δ2H and δ18O in wine, and combining the discriminant function equations, the traceability of the three major production areas in Xinjiang is achieved. This method simplifies the inspection process, reduces cost and time, and improves inspection efficiency and accuracy.
It has achieved high accuracy traceability of Xinjiang wine, and the original discrimination accuracy and cross-verification discrimination accuracy both reach 100%. It is suitable for major production areas such as the Yanqi Basin, Tuha Basin and the northern foothills of the Tianshan Mountains, and is highly economical and practical.
Smart Images

Figure CN120064429A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of wine identification, and more particularly, to a method for tracing the origin of Xinjiang wine. Background Art
[0002] The technology of tracing the origin of wine is an important research field that has gradually emerged in recent years with the development of the wine industry. Tracing the origin not only helps to protect the geographical indication and brand value of wine, but also provides authenticity and quality assurance for consumers. By using scientific methods to determine the origin of wine, it is possible to effectively prevent counterfeit and shoddy products in the market and maintain the healthy development of the wine industry. Currently, the technology of tracing the origin mainly involves multiple fields such as chemical analysis, physical detection, and biomarkers. Among them, chemical analysis methods have been widely studied and applied because they can directly reflect the component characteristics of wine.
[0003] In the existing technology of tracing the origin of wine, chemical analysis methods play an important role. One common method is to determine the origin of wine by detecting the elemental composition in wine. This method is based on the influence of soil, water source, and climate conditions in different origins on grape growth and wine composition. However, this method has obvious limitations. The brewing process of wine is complex and diverse. From grape planting, harvesting to fermentation, aging, etc., all these processes may affect the elemental composition in wine. Therefore, it is difficult to accurately determine the origin of wine only by detecting the elemental composition, and the accuracy of its tracing results is greatly limited.
[0004] In addition, as a new tracing method, the stable isotope technique has received extensive attention in recent years. The principle of this technique is based on the differences in the natural environment in different origins, resulting in significant differences in the stable isotope ratios in wine. For example, Raco et al. found that there is a correlation between the hydrogen stable isotope (δ 2 H) and oxygen stable isotope (δ 18 O) in wine and natural factors such as precipitation; the research by Adami et al. also showed that the δ 18 O value of wine water has high selectivity in geographical region differentiation and is sensitive to altitude changes. These studies provide a theoretical basis for the application of the stable isotope technique in tracing the origin of wine.
[0005] However, stable isotope technology also faces some challenges in practical application. Although this technology can provide relatively accurate origin information, its application effect in certain specific production areas still needs further verification. Taking Xinjiang wine as an example, there are currently few studies on the changing trends of different stable isotopes during its fermentation process. The climate conditions in Xinjiang are complex and diverse, and wines from different production areas may show unique isotope change characteristics during the fermentation process. The application effect and adaptability of the existing general traceability methods in the specific production area of Xinjiang wine have not been fully verified.
[0006] In summary, although the existing wine origin traceability technology has made certain progress in theory and practice, there are still some problems that need to be solved. On the one hand, the chemical analysis method based on elemental composition is interfered by factors such as brewing technology, making it difficult to accurately trace the origin; on the other hand, although the stable isotope technology has a high traceability accuracy, its application effect and adaptability in specific production areas such as Xinjiang still need further research. The existence of these problems limits the widespread application and promotion of wine origin traceability technology, and also provides new directions and challenges for research in related fields.
[0007] In view of this, the present invention is proposed. Summary of the invention
[0008] The purpose of the present invention is to provide a method for tracing the origin of Xinjiang wine. The tracing method is to determine the origin of the wine by measuring the δ 13 C.δ 2 H and δ 18 The three isotope ratios of O can realize the traceability of the three major production areas in Xinjiang, with high accuracy, simple detection process, low cost, high efficiency and strong practicality.
[0009] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:
[0010] The present invention provides a method for tracing the origin of Xinjiang wine, comprising:
[0011] The wine sample to be tested is tested to obtain an isotope ratio result; the isotope ratio result includes the carbon isotope ratio δ 13 C. Hydrogen isotope ratio δ 2 H and oxygen isotope ratio δ 18 O;
[0012] The origin of the wine sample to be tested is determined according to the isotope ratio result; the origin is any one of the Yanqi Basin, the Tuha Basin and the northern foothills of the Tianshan Mountains.
[0013] In an optional embodiment, determining the origin of the wine sample to be tested according to the isotope ratio result includes:
[0014] Substitute the isotope ratio results into the discriminant function equations corresponding to the 3 production areas, obtain the calculation results, and screen out the maximum value among the 3 calculation results;
[0015] Determine the production area of the wine sample to be tested according to the obtained maximum value.
[0016] In an alternative embodiment, the discriminant function equations include a first discriminant equation, a second discriminant equation, and a third discriminant equation;
[0017] The determining the production area of the wine sample to be tested according to the obtained maximum value includes:
[0018] If the maximum value is calculated by the first discriminant equation, it is determined that the production area of the wine sample to be tested is the Yanqi Basin;
[0019] If the maximum value is calculated by the second discriminant equation, it is determined that the production area of the wine sample to be tested is the Turpan-Hami Basin;
[0020] If the maximum value is calculated by the third discriminant equation, it is determined that the production area of the wine sample to be tested is the northern foot of the Tianshan Mountains.
[0021] In an alternative embodiment, the discriminant function equations include:
[0022] First discriminant equation: Y 第一 =-74.566×δC 13 +0.427×δH 2 +42.523×δO 18 -1597.841;
[0023] Second discriminant equation: Y 第二 =-81.827×δC 13 +0.127×δH 2 +37.184×δO 18 -1675.47;
[0024] Third discriminant equation: Y 第三 =-80.736×δC 13 -0.660×δH 2 +32.950×δO 19 -1572.342.
[0025] In an alternative embodiment, the testing the wine sample to be tested to obtain the isotope ratio results includes:
[0026] Dry the wine sample to be tested to obtain a dried sample to be tested;
[0027] Detect the dry sample to be tested using an isotope mass spectrometer to obtain the abundance ratio of heavy isotopes to light isotopes in the dry sample to be tested;
[0028] Calculate the isotope ratio result based on the abundance ratio of the heavy isotope to the light isotope.
[0029] In an alternative embodiment, the drying treatment is a reduced-pressure drying treatment;
[0030] Preferably, the drying treatment is a freeze-reduced-pressure drying treatment.
[0031] In an alternative embodiment, the detecting the dry sample to be tested using an isotope mass spectrometer to obtain the abundance ratio of heavy isotopes to light isotopes in the dry sample to be tested includes:
[0032] Weigh the corresponding weight of the dry sample to be tested according to the measured isotope;
[0033] Based on the calibration of the reference material, use the isotope mass spectrometer to detect carbon stable isotope, hydrogen stable isotope and oxygen stable isotope respectively.
[0034] In an alternative embodiment, the weighing the corresponding weight of the dry sample to be tested according to the measured isotope includes:
[0035] When detecting carbon stable isotope, the weighing amount of the dry sample to be tested is 0.2 mg to 2 mg;
[0036] When detecting nitrogen stable isotope, the weighing amount of the dry sample to be tested is 2 mg to 10 mg;
[0037] When detecting hydrogen and oxygen stable isotopes, the weighing amount of the dry sample to be tested is 0.2 mg.
[0038] In an alternative embodiment, the reference material includes:
[0039] IAEA-600 reference material for detecting carbon stable isotope;
[0040] USGS 43, USGS 54 and USGS 56 reference materials for detecting hydrogen stable isotope and oxygen stable isotope.
[0041] In an alternative embodiment, the calculation formula of the isotope ratio result is:
[0042]
[0043] where R 样品 represents the abundance ratio of heavy isotopes to light isotopes of the dry sample to be tested; R 标准represents the abundance ratio of the heavy isotope to the light isotope of the reference material; δ represents the isotope ratio.
[0044] The origin tracing method for Xinjiang wine provided by the present invention determines the origin by measuring the carbon isotope ratio (δ 13 C), hydrogen isotope ratio (δ 2 H), and oxygen isotope ratio (δ 18 O) in the wine. The original discrimination accuracy rate and the cross-validation discrimination accuracy rate both reach 100%, showing extremely high accuracy and reliability. This is of great significance for protecting the geographical indication and brand value of Xinjiang wine and preventing counterfeit and shoddy products from entering the market. This method only needs to measure three key isotope ratios, without complex sample pretreatment and the combination of multiple detection means, greatly simplifying the detection process, reducing the detection cost and time. Compared with other existing tracing methods, it significantly improves the detection efficiency while ensuring high accuracy, and has high economy and practicability. This method is specifically aimed at the origin tracing problem of Xinjiang wine and is particularly applicable to the three main production areas of the Yanqi Basin, Turpan-Hami Basin, and the northern foot of the Tianshan Mountains. The climate conditions in Xinjiang are complex and diverse, and wines from different production areas will show unique isotope variation characteristics during the fermentation process. This method fully considers these characteristics and can effectively distinguish wines from different production areas, with strong pertinence and adaptability. In addition, this method is based on stable isotope technology and combines a discrimination analysis model, with a solid scientific theoretical basis. The change of the stable isotope ratio is closely related to the natural environment (such as climate, soil, water source, etc.) of the origin, which can provide a reliable basis for wine origin tracing. At the same time, this method has been verified by experiments, proving its effectiveness in practical applications, and has strong practicability and operability. BRIEF DESCRIPTION OF THE DRAWINGS
[0045] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for the description of the specific embodiments or the prior art. Obviously, the following drawings are some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.
[0046] Figure 1 is a schematic flow chart of the origin tracing method for Xinjiang wine in the embodiment of the present application;
[0047] Figure 2 is a scatter plot result diagram for analyzing and classifying the discrimination function equation in the embodiment of the present application. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0048] The embodiments of the present invention will be described in detail below in conjunction with examples. However, those skilled in the art will understand that the following examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention. For those not specified in the examples, the conventional conditions or the conditions recommended by the manufacturer are followed. For the reagents or instruments not specified by the manufacturer, they are all conventional products that can be obtained through commercial purchase.
[0049] Reference Figure 1 , in the embodiments of the present application, a method for tracing the origin of Xinjiang wine is provided, including:
[0050] Step S1, testing the wine sample to be measured to obtain the isotope ratio result; the isotope ratio result includes the carbon isotope ratio δ 13 C, the hydrogen isotope ratio δ 2 H, and the oxygen isotope ratio δ 18 O.
[0051] The wine sample to be measured refers to the wine sample used for origin tracing analysis. The origin information of these samples is unknown or needs to be verified, and their specific origin is determined by detecting their chemical components (such as stable isotope ratios).
[0052] In this step, the wine sample for which the specific origin in Xinjiang needs to be determined is detected to obtain its carbon isotope ratio (δ 13 C), hydrogen isotope ratio (δ 2 H), and oxygen isotope ratio (δ 18 O).
[0053] The mass spectrometry coupling technology can accurately measure the isotope ratio, providing a reliable data basis for subsequent origin tracing. It can detect tiny isotope ratio differences, which helps to distinguish the subtle characteristics of wines from different origins.
[0054] Step S2, determining the origin corresponding to the wine sample to be measured according to the isotope ratio result; the origin is any one of the Yanqi Basin, the Turpan-Hami Basin, and the northern foot of the Tianshan Mountains.
[0055] Using the obtained isotope ratio data, it is judged whether the wine sample comes from the Yanqi Basin, the Turpan-Hami Basin, or the northern foot of the Tianshan Mountains. The original discrimination accuracy rate and the cross-validation discrimination accuracy rate of the method both reach 100%, and it can accurately judge the origin of the wine.
[0056] This method is specifically aimed at the three main production areas of Xinjiang wine, fully considering the unique climate conditions and fermentation characteristics in the Xinjiang region, and has strong adaptability.
[0057] In some embodiments, in step S2, determining the origin corresponding to the wine sample to be measured according to the isotope ratio result includes:
[0058] Step S21: Substitute the isotope ratio result into the discriminant function equations corresponding to the three production areas, obtain the calculation results, and screen out the maximum value among the three calculation results.
[0059] Step S22: Determine the production area of the wine sample to be tested according to the obtained maximum value.
[0060] In this step, it is further clarified how to determine the production area of wine by using the isotope ratio result. A specific mathematical model and calculation method are provided, and accurate discrimination of the production area is achieved through the discriminant function equation. This method not only improves the scientificity and accuracy of traceability but also provides clear guidance for actual operation.
[0061] In some embodiments, the discriminant function equations include a first discriminant equation, a second discriminant equation, and a third discriminant equation;
[0062] Determining the production area of the wine sample to be tested according to the obtained maximum value includes:
[0063] If the maximum value is calculated by the first discriminant equation, it is determined that the production area of the wine sample to be tested is the Yanqi Basin;
[0064] If the maximum value is calculated by the second discriminant equation, it is determined that the production area of the wine sample to be tested is the Turpan-Hami Basin;
[0065] If the maximum value is calculated by the third discriminant equation, it is determined that the production area of the wine sample to be tested is the northern foot of the Tianshan Mountains.
[0066] In some embodiments, the discriminant function equations include:
[0067] (1) First discriminant equation: Y 第一 = -74.566×δC 13 + 0.427×δH 2 + 42.523×δO 18 - 1597.841;
[0068] (2) Second discriminant equation: Y 第二 = -81.827×δC 13 + 0.127×δH 2 + 37.184×δO 18 - 1675.47;
[0069] (3) Third discriminant equation: Y 第三 = -80.736×δC 13 - 0.660×δH 2 + 32.950×δO 18-1572.342。
[0070] In some embodiments, step S1 of testing the wine sample to be tested to obtain the isotope ratio result includes:
[0071] Step S11 of drying the wine sample to be tested to obtain a dried sample to be tested.
[0072] In this step, the wine sample is dried to remove moisture and fix the chemical composition of the sample, facilitating subsequent detection.
[0073] In some embodiments, the drying treatment is vacuum drying treatment;
[0074] In some preferred embodiments, the drying treatment is freeze-vacuum drying treatment.
[0075] For example, the wine sample can be freeze-dried at -70°C and 0.01 mbar until the sample reaches a constant weight. This drying method can effectively remove the moisture in the sample while keeping the chemical composition of the sample unchanged.
[0076] Then the sample is stored. The dried sample can be put into a vial and stored in a desiccator to prevent the sample from being affected by the external environment before detection.
[0077] Step S12 of detecting the dried sample to be tested using an isotope mass spectrometer to obtain the abundance ratio of heavy isotopes to light isotopes in the dried sample to be tested.
[0078] The dried sample is detected using an isotope mass spectrometer to obtain the abundance ratio of heavy isotopes to light isotopes in the sample.
[0079] Step S13 of calculating the isotope ratio result based on the abundance ratio of heavy isotopes to light isotopes.
[0080] Based on the detected abundance ratio of heavy isotopes to light isotopes, the isotope ratio (δ value) is calculated.
[0081] In this step, a method for obtaining the isotope ratio result from the wine sample to be tested is provided. The core lies in freeze-drying the sample, precisely detecting it using an advanced isotope mass spectrometer, and calibrating it with internationally recognized reference materials, thereby ensuring the consistency of sample processing and the reliability of the detection results. This process not only achieves high-precision measurement of the isotope ratio, providing solid data support for origin tracing, but also ensures the repeatability of the detection due to its clear steps and methods, facilitating result comparison and verification between different laboratories.
[0082] In terms of implementation, a suitable device such as a DELTAV Plus or Isoprime precision isotope mass spectrometer is selected and combined with professional data processing software (such as IBM SPSS Statistics) to calculate and analyze isotope ratios, further improving the detection efficiency and accuracy.
[0083] In some embodiments, detecting the dry sample to be measured using an isotope mass spectrometer to obtain the abundance ratio of heavy isotopes to light isotopes in the dry sample to be measured includes:
[0084] Weighing the corresponding weight of the dry sample to be measured according to the measured isotope;
[0085] Based on the calibration of reference materials, using the isotope mass spectrometer to detect carbon stable isotopes, hydrogen stable isotopes, and oxygen stable isotopes respectively.
[0086] In some embodiments, weighing the corresponding weight of the dry sample to be measured according to the measured isotope includes:
[0087] (1) When detecting carbon stable isotopes, the weighing amount of the dry sample to be measured is 0.2 mg to 2 mg; for example, it can be 0.2 mg, 0.5 mg, 1 mg, 1.5 mg, 2 mg, etc.
[0088] (2) When detecting nitrogen stable isotopes, the weighing amount of the dry sample to be measured is 2 mg to 10 mg; for example, it can be 2 mg, 3 mg, 5 mg, 8 mg, 10 mg, etc.
[0089] (3) When detecting hydrogen and oxygen stable isotopes, the weighing amount of the dry sample to be measured is 0.2 mg.
[0090] In some embodiments, the reference materials include:
[0091] The IAEA-600 reference material for detecting carbon stable isotopes;
[0092] The USGS 43, USGS 54, and USGS 56 reference materials for detecting hydrogen stable isotopes and oxygen stable isotopes.
[0093] It should be noted that during the long-term operation of precision instruments such as isotope mass spectrometers, drift phenomena may occur, resulting in deviations in measurement results. The isotope ratios of reference materials are known and precise. By regularly calibrating with reference materials, the measurement parameters of the instrument can be adjusted to ensure the accuracy and stability of the instrument. The isotope ratios of reference materials are strictly determined and certified, with high accuracy and traceability. During the detection process, by comparing the measurement results of unknown samples with the known ratios of reference materials, quantitative analysis of the isotope ratios of unknown samples can be achieved.
[0094] In some embodiments, the calculation formula for the isotope ratio result is as follows:
[0095]
[0096] where R 样品 represents the abundance ratio of the heavy isotope to the light isotope of the dry sample to be measured; R 标准 represents the abundance ratio of the heavy isotope to the light isotope of the reference material; δ represents the isotope ratio.
[0097] The present invention will be further illustrated by specific examples below. However, it should be understood that these examples are only for more detailed illustration and should not be construed as limiting the present invention in any way.
[0098] Experimental Example 1: Establishment of discriminant function equation
[0099] In this experimental example, a discriminant function equation was established.
[0100] 1. Experimental method:
[0101] In this embodiment, the element analysis-stable isotope ratio mass spectrometry (EA-IRMS) was used to measure the stable isotope ratios of carbon (δ 13 C), nitrogen (δ 15 N), hydrogen (δ 2 H), and oxygen (δ 18 O) in Xinjiang wine.
[0102] (1) Materials and reagents: The carbon and nitrogen isotope reference materials in wine were IAEA-600 caffeine (δ 13 CV-PDB = 27.771 ± 0.07‰, δ 15 Nair = 1.0 ± 0.2‰), from the International Atomic Energy Agency; the hydrogen and oxygen stable isotope reference materials were USGS 43 (δ 2 HV-SMOW = -50.3‰, δ 18 OV-SMOW = +14.11‰), USGS 54 (δ 2HV-SMOW=-150.4‰、δ 18 OV-SMOW=+17.79‰), USGS56(δ 2 HV-SMOW=-44‰、δ 18 OV-SMOW = +27.23‰, provided by the United States Geological Survey. Xinjiang wine samples come from Xiangdu Winery (Yanqi Basin, 3 batches), Shanshan Loulan Winery (Xinjiang Tuha Basin, 3 batches), Zhongfei Winery (Yanqi Basin, 3 batches), Niya Winery (Northern Foothills of Tianshan Mountains, 6 batches), and the grape varieties include Cabernet Sauvignon, Riesling, Marselan, Merlot, Cabernet Franc, Cabernet Gernischt, Syrah, Chardonnay, and Sauvignon Blanc.
[0103] (2) Instruments and equipment: We used DELTA V Plus stable isotope mass spectrometer (with Flash 2000 Organic elemental analyzer) produced by Thermo Fisher, USA; Isoprime precision stable isotope ratio mass spectrometer (with vario ISOTOPE select elemental analyzer) produced by Elementar, Germany; Milli-Q ultrapure water system produced by Millpore, USA; EPSILON 2-4LSC freeze dryer produced by Marin Christ, Germany; and XP-6 ppm electronic balance produced by Mettler-Toledo, Switzerland.
[0104] (3) Detection method:
[0105] 1) Sample preparation and processing: The wine was freeze-dried to constant weight at -70°C and 0.01 mbar, and then placed in vials and stored in a desiccator until testing.
[0106] 2) Stable isotope analysis: For carbon and nitrogen stable isotope analysis, weigh 0.2-2 mg of the sample to be tested for carbon measurement and 2-10 mg of the sample to be tested for nitrogen measurement, respectively, put them into a tin foil cup (4mm×4mm×11mm), wrap them, and put them into the solid sample automatic sampling tray of the vario ISOTOPEselect elemental analyzer. The carbon in the sample is converted into CO after burning at 950℃, and the nitrogen is burned at 600℃ and reduced to N by reducing copper, and then sent to the stable isotope ratio mass spectrometer for analysis. During the analysis, the carbon stable isotope is calibrated with IAEA-600 standard materials.
[0107] 3) For hydrogen and oxygen stable isotope analysis, weigh about 0.2 mg of the sample to be tested and place it in a silver cup. The package sample was dried in a desiccator for 24 h after being placed in the sample tray, and then put into the automatic solid sample injection tray of the Flash 2000 Organic elemental analyzer. The hydrogen and oxygen elements in the sample were respectively converted into H and CO after pyrolysis at a high temperature of 1350 °C and then entered the stable isotope ratio mass spectrometer for detection. During the detection, USGS 43, USGS 54, and USGS 56 were used as reference materials to correct the test results.
[0108] 4) Calculation of stable isotope ratio: The formula was used for calculation, where R sample is the abundance ratio of the heavy isotope to the light isotope in the measured sample, and R standard is the abundance ratio of the heavy isotope to the light isotope in the reference sample.
[0109] 5) Data processing: Discriminant analysis was carried out using the IBM SPSS Statistics 26 program.
[0110] (4) Establishment of discriminant model:
[0111] Discriminant analysis (DA) is a multivariate statistical analysis method for determining the type attribution of a research object based on various eigenvalue conditions under the condition of known classification. Its basic principle is to establish one or more discriminant functions according to certain discriminant criteria, determine the undetermined coefficients in the discriminant function using a large amount of data of the research object, and calculate the discriminant index. Based on this, it can be determined which category a certain sample belongs to. In this experimental example, discriminant analysis was used for the carbon, nitrogen, hydrogen, and oxygen stable isotopes of 15 batches of Xinjiang wines. It can be seen from the eigenvalues of the canonical discriminant function (Table 1) that 100% of the total variation can be achieved through two linear functions.
[0112] Table 1. Eigenvalues of canonical discriminant function
[0113]
[0114] The classification function coefficients of the Fisher linear discriminant function method are shown in Table 2. Only three indicators of carbon, hydrogen, and oxygen stable isotopes are required to establish the model.
[0115] Table 2. Classification function coefficients of Fisher linear discriminant analysis
[0116]
[0117] Accordingly, the corresponding discriminant function equations can be obtained as follows:
[0118] Table 3. Discriminant function equations
[0119] Production area Discriminant function equation Equation Yanqi Basin First discriminant equation <![CDATA[Y 第 One = -74.566×δC 13 +0.427×δH 2 +42.523×δO 18 -1597.841]]> Turpan-Hami Basin Second discriminant equation <![CDATA[Y 第二 = -81.827×δC 13 + 0.127×δH 2 + 37.184×δO 18 - 1675.47]]> Northern foot of Tianshan Mountains Third discriminant equation <![CDATA[Y 第三 = -80.736 × δC 13 - 0.660 × δH 2 + 32.950 × δO 18 - 1572.342]]>
[0120] The discriminant function equations were analyzed and classified, and the analysis and classification results are shown in Figure 2 and Table 4.
[0121] Table 4, Classification Results of Discriminant Analysis
[0122]
[0123] As can be seen from the classification results, the original discriminant accuracy of the established model is 100%, and the cross-validation discriminant accuracy is 100%. It can be seen that this model (discriminant function equation) has a good traceability effect on Xinjiang wines.
[0124] Experimental Example 2
[0125] In this experimental example, Xinjiang wines of different batches were tested to determine the origin.
[0126] 1. Experimental Method:
[0127] In this experimental example, the testing method used is the same as that in Experimental Example 1.
[0128] In this embodiment, element analysis-stable isotope ratio mass spectrometry (EA-IRMS) was used to measure the stable isotope ratios of carbon (δ 13 C), nitrogen (δ 15 N), hydrogen (δ 2 H), and oxygen (δ 18 O) in Xinjiang wines.
[0129] (1) Materials and Reagents: The carbon and nitrogen isotope reference materials for wine were IAEA-600 caffeine (δ 13 CV-PDB = 27.771 ± 0.07‰, δ 15 Nair = 1.0 ± 0.2‰), from the International Atomic Energy Agency; the hydrogen and oxygen stable isotope reference materials were USGS 43 (δ 2 HV-SMOW = -50.3‰, δ 18 OV-SMOW = +14.11‰), USGS 54 (δ 2 HV-SMOW = -150.4‰, δ 18 OV-SMOW = +17.79‰), USGS56 (δ 2 HV-SMOW = -44‰, δ 18 OV-SMOW = +27.23‰), provided by the United States Geological Survey.
[0130] (2) Instruments and equipment: DELTA V Plus stable isotope mass spectrometer (equipped with Flash 2000 Organic elemental analyzer), produced by Thermo Fisher Company in the United States; Isoprime precision stable isotope ratio mass spectrometer (equipped with vario ISOTOPE select elemental analyzer), produced by Elementar Company in Germany; Milli-Q ultrapure water system of Millpore Company in the United States, EPSILON 2-4LSC freeze dryer of Marin Christ Company in Germany, and XP-6 one-millionth electronic balance of Mettler Toledo Company in Switzerland.
[0131] (3) Detection methods:
[0132] 1) Sample preparation and treatment: The wine is freeze-dried to constant weight at -70 °C and 0.01 mbar, filled into vials and stored in a desiccator for future measurement.
[0133] 2) Stable isotope analysis: For carbon and nitrogen stable isotope analysis, 0.2 - 2 mg of the sample to be measured is weighed for carbon measurement and 2 - 10 mg for nitrogen measurement. After being wrapped in a tin foil cup (4 mm × 4 mm × 11 mm), it is placed into the solid sample automatic injection tray of the vario ISOTOPE select elemental analyzer. The carbon in the sample is converted into CO after high-temperature combustion at 950 °C, and the nitrogen is converted into N after high-temperature combustion at 600 °C and reduction by reducing copper, and then sent to the stable isotope ratio mass spectrometer for analysis. During the analysis process, the carbon stable isotope is calibrated with the IAEA-600 reference material.
[0134] 3) For hydrogen and oxygen stable isotope analysis, about 0.2 mg of the sample to be measured is weighed and placed into a silver cup for sample wrapping. After being placed in the sample tray, it is dried in a desiccator for 24 h, and then placed into the automatic solid sample injection tray of the Flash 2000 Organic elemental analyzer. The hydrogen and oxygen elements in the sample are respectively converted into H and CO after high-temperature pyrolysis at 1350 °C and enter the stable isotope ratio mass spectrometer for detection. During the detection, USGS 43, USGS 54, and USGS 56 are used as reference materials to calibrate the test results.
[0135] 4) Calculation of stable isotope ratio: Calculated using the formula where R_sample is the abundance ratio of the heavy isotope to the light isotope in the measured sample, and R_reference is the abundance ratio of the heavy isotope to the light isotope in the reference sample.
[0136] 2. Test results:
[0137] Table 5. Results of different verification samples
[0138] Sample <![CDATA[δC 13 > <![CDATA[δH 2 > <![CDATA[δO 18 > Sample 1 (Northern foot of Tianshan Mountains) -28.65 -55.23 23.2 Sample 2 (Yanqi Basin) -26.52 -30.88 27.06 Sample 3 (Turpan-Hami Basin) -29.05 -36.5 25.58
[0139] Calculate using the established discriminant function equation:
[0140] (1) Sample 1:
[0141] Table 6, Calculation Process and Results of Sample 1
[0142]
[0143] According to the results in Table 6, the Y of Sample 1 第三 is 1540.7462, the maximum value among the three calculation results. Therefore, this sample is the wine from the northern foot of Tianshan Mountains corresponding to Y 第三 .
[0144] (2) Sample 2:
[0145] Table 7, Calculation Process and Results of Sample 2
[0146]
[0147] According to the results in Table 7, the Y of Sample 2 第一 is 1507.13594, the maximum value among the three calculation results. Therefore, this sample is the wine from Yanqi Basin corresponding to Y 第一 .
[0148] (3) Sample 3:
[0149] Table 8, Calculation Process and Results of Sample 3
[0150]
[0151] According to the results in Table 8, the Y of Sample 3 第二 is 1646.13557, the maximum value among the three calculation results. Therefore, this sample is the wine from Turpan-Hami Basin corresponding to Y 第二 .
[0152] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for tracing the origin of Xinjiang wine, characterized in that: include: The wine sample to be tested is tested to obtain an isotope ratio result; the isotope ratio result includes the carbon isotope ratio δ 13 C. Hydrogen isotope ratio δ 2 H and oxygen isotope ratio δ 18 O; The origin of the wine sample to be tested is determined according to the isotope ratio result; the origin is any one of the Yanqi Basin, the Tuha Basin and the northern foothills of the Tianshan Mountains.
2. The method for tracing the origin of Xinjiang wine according to claim 1, characterized in that: Determining the origin of the wine sample to be tested according to the isotope ratio result includes: Substituting the isotope ratio results into the discriminant function equations corresponding to the three origins to obtain a calculation result, and screening to obtain the maximum value of the three calculation results; The origin of the wine sample to be tested is determined according to the maximum value obtained.
3. The method for tracing the origin of Xinjiang wine as claimed in claim 2, characterized in that: The discriminant function equation includes a first discriminant equation, a second discriminant equation and a third discriminant equation; Determining the origin of the wine sample to be tested based on the obtained maximum value includes: If the maximum value is calculated by the first discriminant equation, it is determined that the origin of the wine sample to be tested is the Yanqi Basin; If the maximum value is calculated by the second discriminant equation, it is determined that the origin of the wine sample to be tested is the Tuha Basin; If the maximum value is calculated by the third discriminant equation, it is determined that the origin of the wine sample to be tested is the northern foothills of Tianshan Mountain.
4. The method for tracing the origin of Xinjiang wine as claimed in claim 3, characterized in that: The discriminant function equation includes: First discriminant equation: Y 第一 =-74.566×δC 13 +0.427×δH 2 +42.523×δO 18 -1597.841; Second discriminant equation: Y 第二 =-81.827×δC 13 +0.127×δH 2 +37.184×δO 18 -1675.47; The third discriminant equation: Y 第三 =-80.736×δC 13 -0.660×δH 2 +32.950×δO 18 -1572.
342.
5. The method for tracing the origin of Xinjiang wine according to claim 1, characterized in that: The isotope ratio results obtained by testing the wine sample include: Drying the wine sample to be tested to obtain a dry sample to be tested; The dry sample to be tested is detected by using an isotope mass spectrometer to obtain the abundance ratio of the heavy isotope to the light isotope in the dry sample to be tested; The isotope ratio result is calculated based on the abundance ratio of the heavy isotope to the light isotope.
6. The method for tracing the origin of Xinjiang wine as claimed in claim 5, characterized in that: The drying process is a reduced pressure drying process; Preferably, the drying process is a freeze-dried reduced-pressure drying process.
7. The method for tracing the origin of Xinjiang wine as claimed in claim 5, characterized in that: The method of detecting the dry sample to be tested by using an isotope mass spectrometer to obtain the abundance ratio of the heavy isotope to the light isotope in the dry sample to be tested comprises: According to the isotope to be measured, weigh the corresponding weight of the dry sample to be measured; Based on the calibration of the standard substance, the isotope mass spectrometer is used to detect the carbon stable isotope, the hydrogen stable isotope and the oxygen stable isotope respectively.
8. The method for tracing the origin of Xinjiang wine as claimed in claim 7, characterized in that: The step of weighing the dry sample to be tested by a corresponding weight according to the isotope to be tested comprises: When the carbon stable isotope is detected, the amount of the dry sample to be tested is 0.2 mg to 2 mg; When performing the detection of nitrogen stable isotopes, the amount of the dry sample to be tested is 2 mg to 10 mg; When the stable isotopes of hydrogen and oxygen are detected, the weighed amount of the dry sample to be detected is 0.2 mg.
9. The method for tracing the origin of Xinjiang wine as claimed in claim 7, characterized in that: The standard substances include: IAEA-600 reference materials for carbon stable isotope detection; USGS 43, USGS 54 and USGS 56 reference materials for hydrogen and oxygen stable isotope determinations.
10. The method for tracing the origin of Xinjiang wine as claimed in claim 7, characterized in that: The calculation formula of the isotope ratio result is: Among them, R 样品 represents the abundance ratio of the heavy isotope to the light isotope of the dry sample to be tested; R 标准 represents the abundance ratio of the heavy isotope to the light isotope of the standard substance; δ represents the isotope ratio.