CN111505170A - Method for identifying authenticity of five-grain strong aromatic Chinese spirits - Google Patents
Method for identifying authenticity of five-grain strong aromatic Chinese spirits Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for identifying the authenticity of five-grain strong aromatic Chinese spirits, which relates to the technical field of Chinese spirits identification, and comprises the following steps: (1) measuring the numerical values of ethanol carbon isotopes and ethyl caproate carbon isotopes in a five-grain strong aromatic Chinese spirit true wine sample by using a gas chromatography-combustion-isotope ratio mass spectrometer, and taking the numerical values as true wine sample data; (2) determining the numerical values of the carbon isotopes of ethanol and the carbon isotopes of ethyl caproate in the sample to be detected by using a gas chromatography-combustion-isotope ratio mass spectrometer as the data of the sample to be detected; (3) and calculating the Mahalanobis distance between the sample data to be detected and the real wine sample data, classifying, and judging the truth of the sample to be detected. The method provided by the invention has the advantages of small sample consumption, simple and rapid operation and high accuracy, and the data of false wine measured by the method for identifying the authenticity of the five-grain strong aromatic Chinese spirits provided by the invention is difficult to achieve, so the difficulty of adulteration of the Chinese spirits is obviously improved.
Description
Technical Field
The invention relates to the technical field of liquor identification, in particular to a method for identifying the authenticity of five-grain strong aromatic liquor.
Background
At present, in the domestic white spirit market, the quality of the white spirit prepared by a solid state method is the best, the variety of the white spirit prepared by the solid state method is various, and five-grain strong-flavor white spirit is one of the white spirits prepared by the solid state method.
The solid-state method white spirit takes pure grain brewing, non-additive brewing and the like as main selling points, has the highest consumer acceptance degree, and becomes an 'inferior and good' adulteration heavy disaster area due to higher commodity profit and great identification difficulty of adulteration white spirit. The solid-state method strong aromatic Chinese spirits are adulterated by adding ethanol and ethyl caproate, wherein the added ethanol mainly comes from liquid-state method fermentation products such as corn, rice and the like, and the added ethyl caproate mainly is a chemical synthesis or liquid-state method fermentation product.
The existing method for identifying the authenticity of the five-grain strong aromatic Chinese spirits has the disadvantages of large sample consumption, complex operation, long time consumption and poor accuracy.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for identifying the truth of five-grain strong aromatic Chinese spirits, which comprises the following steps: (1) measuring the numerical values of ethanol carbon isotopes and ethyl caproate carbon isotopes in a five-grain strong aromatic Chinese spirit true wine sample by using a gas chromatography-combustion-isotope ratio mass spectrometer, and taking the numerical values as true wine sample data; (2) determining the numerical values of the carbon isotopes of ethanol and the carbon isotopes of ethyl caproate in the sample to be detected by using a gas chromatography-combustion-isotope ratio mass spectrometer as the data of the sample to be detected; (3) and calculating the Mahalanobis distance between the sample data to be detected and the real wine sample data, classifying, and judging the truth of the sample to be detected.
Preferably, in the step (1), the step of measuring the carbon isotope of ethanol in the five-grain Luzhou-flavor liquor sample comprises the steps of diluting the 200 mu L five-grain Luzhou-flavor liquor sample with 1m L acetone, uniformly mixing, placing the mixture in a 2ml gas chromatography bottle, and carrying out sample injection measurement, and the step of measuring the carbon isotope of ethyl hexanoate in the five-grain Luzhou-flavor liquor sample comprises the step of directly carrying out sample injection measurement.
Preferably, in the step (2), the carbon isotope of ethanol in the sample to be detected is obtained by diluting a 200 mu L sample to be detected with 1m L acetone, mixing uniformly, placing the mixture in a 2ml gas chromatography bottle, and performing sample injection measurement, and the carbon isotope of ethyl hexanoate in the sample to be detected is obtained by performing direct sample injection measurement.
Preferably, in the step (1), the instrument conditions for measuring the ethanol carbon isotope in the five-grain strong aromatic Chinese spirit true spirit sample are that the chromatographic conditions are that the injection port temperature is 180 ℃, the flow rate is 1.0m L/min, the temperature is programmed to be raised to 40 ℃, the initial temperature is kept for 5min, the temperature is raised to 50 ℃ at 1 ℃/min, the temperature is raised to 200 ℃ at 15 ℃/min, the temperature is kept for 2min, the split ratio is 50:1, and the combustion condition is that the combustion temperature is 1000 ℃.
Preferably, in the step (1), the instrument conditions for measuring the carbon isotope of ethyl caproate in the five-grain Luzhou-flavor liquor sample are that an HP-INNOWAx capillary chromatographic column is adopted, carrier gas is high-purity helium, a constant flow mode is adopted, the flow rate is 3ml/min, the sample is injected in a non-split-flow manner, the injection amount is about 0.3u L-2 u L, the initial temperature of a column incubator is 40 ℃, the temperature is kept for 4min, the temperature is increased to 92 ℃ at 5 ℃/min, the temperature is increased to 230 ℃ at 30 ℃/min, the temperature is kept for 5min, the combustion condition is that the injection port temperature is 230 ℃, the oxidation furnace temperature is 960 ℃, the reduction furnace temperature is 640 ℃, the mass spectrum condition is that the ion source is high in pressure of 10.0kV, and the emission current is 1.
More preferably, the filler of the oxidation furnace is CuO, NiO and Pt.
Preferably, in the step (2), the instrument for measuring the ethanol carbon isotope in the sample to be measured is used for measuring the chromatographic condition that the injection port temperature is 180 ℃, the flow rate is 1.0m L/min, the temperature programming is carried out at the initial temperature of 40 ℃, the temperature is kept for 5min, the temperature is raised to 50 ℃ at 1 ℃/min, the temperature is kept for 1min, the temperature is raised to 200 ℃ at 15 ℃/min, the temperature is kept for 2min, the split ratio is 50:1, and the combustion condition is 1000 ℃.
Preferably, in the step (2), the instrument for measuring the carbon isotope of ethyl caproate in the sample to be measured is characterized in that a HP-INNOWAx capillary chromatographic column is adopted as a chromatographic condition, high-purity helium is adopted as carrier gas, the constant-current mode is adopted, the flow rate is 3ml/min, the sample is injected in a non-split-flow mode, the injection amount is about 0.3u L-2 u L, the initial temperature of a column incubator is 40 ℃, the temperature is kept for 4min, the temperature is increased to 92 ℃ at 5 ℃/min, the temperature is increased to 230 ℃ at 30 ℃/min, the temperature is kept for 5min, the combustion condition is that the injection port temperature is 230 ℃, the oxidation furnace temperature is 960 ℃, the reduction furnace temperature is 640 ℃, the mass spectrum condition is that the ion source is high in pressure and 10.0.
More preferably, the filler of the oxidation furnace is CuO, NiO and Pt.
The invention has the beneficial effects that: the method provided by the invention has the advantages of small sample consumption, simple and rapid operation and high accuracy, and the data of false wine measured by the method for identifying the authenticity of the five-grain strong aromatic Chinese spirits provided by the invention is difficult to achieve, so the difficulty of adulteration of the Chinese spirits is obviously improved.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Examples
1. Materials and methods
1.1 Experimental samples
The five-grain strong aromatic white spirit true spirit sample: 5 kinds of five-grain strong aromatic liquor true liquor produced in Yibin areas;
a sample to be tested: 3 five-grain strong-flavor liquor pseudo-liquor
1.2 sample preparation
(1) And (3) measuring the carbon isotope of the ethanol, namely accurately measuring a five-grain strong aromatic Chinese spirit true wine sample or a sample to be measured of 200 mu L, putting the five-grain strong aromatic Chinese spirit true wine sample or the sample to be measured into a 2m L gas chromatography sample injection bottle, adding 1m L acetone, fully and uniformly mixing, measuring to be measured, and measuring by sample injection.
(2) Determination of carbon isotope of ethyl hexanoate: directly injecting sample for determination.
1.3 instruments and reagents
The instrument equipment comprises: gas chromatography-combustion-stable isotope mass spectrometer (GC-C-IRMS);
reagents and consumables: high purity helium (99.999%); two compounds of ethyl caproate and amyl acetate are used as carbon isotope standard samples.
1.4 apparatus conditions
(1) Instrument conditions for measuring carbon isotope of ethanol
Chromatographic conditions, wherein the temperature of a sample inlet is 180 ℃, the flow rate is 1.0m L/min, the temperature is programmed to be 40 ℃ at the initial temperature and kept for 5min, the temperature is raised to 50 ℃ at 1 ℃/min and kept for 1min, the temperature is raised to 200 ℃ at 15 ℃/min and kept for 2min, and the split ratio is 50: 1.
The combustion conditions are as follows: the combustion temperature was 1000 ℃.
(2) Instrument conditions for measuring carbon isotope of ethyl caproate
The chromatographic conditions are that an HP-INNOWAx capillary chromatographic column is adopted, carrier gas is high-purity helium, the constant flow mode is adopted, the flow rate is 3ml/min, the sample is injected in a non-split flow mode, the sample injection amount is about 0.3u L-2 u L, the initial temperature of a column incubator is 40 ℃, the temperature is kept for 4min, the temperature is raised to 92 ℃ at 5 ℃/min, and the temperature is raised to 230 ℃ at 30 ℃/min, and the temperature is kept for 5 min.
The combustion conditions are as follows: the injection inlet temperature is 230 ℃, the temperature of an oxidation furnace (NiO/CuO/Pt) is 960 ℃, and the temperature of a reduction furnace is 640 ℃.
Mass spectrum conditions: the high voltage of the ion source is 10.0kV, and the emission current is 1.5 mA.
2. True and false identification test
2.1 true and false identification test of five-grain Luzhou-flavor liquor
The method comprises the following specific steps:
(1) measuring the numerical values of ethanol carbon isotopes and ethyl caproate carbon isotopes in a five-grain strong aromatic Chinese spirit true wine sample by using a gas chromatography-combustion-isotope ratio mass spectrometer, and taking the numerical values as true wine sample data;
(2) determining the numerical values of the carbon isotopes of ethanol and the carbon isotopes of ethyl caproate in the sample to be detected by using a gas chromatography-combustion-isotope ratio mass spectrometer as the data of the sample to be detected;
(3) and calculating the Mahalanobis distance between the sample data to be detected and the real wine sample data, classifying, and judging the truth of the sample to be detected.
3. Results and analysis
3.1 numerical values of ethanol carbon isotope and ethyl caproate carbon isotope in five-grain Luzhou-flavor liquor true liquor sample and sample to be detected
Specific results are shown in Table 1
TABLE 1
| Categories | Ethanol δ13CV-PDB(‰) | Hexanoic acid ethyl ester δ13CV-PDB(‰) |
| Five-grain strong-flavor liquor sample 1 | -21.01 | -22.12 |
| Five-grain strong-flavor liquor sample 2 | -22.48 | -18.29 |
| Five-grain strong-flavor liquor true liquor sample 3 | -23.15 | -20.21 |
| Five-grain strong-flavor liquor sample 4 | -21.99 | -18.46 |
| Five-grain strong-flavor liquor sample 5 | -22.45 | -18.45 |
| Sample 1 to be tested | -11.15 | -29.13 |
| Sample 2 to be tested | -11.26 | -28.20 |
| Sample to be tested 3 | -10.88 | -33.81 |
3.2 statistics and Classification results
The statistical results are shown in Table 2, and the classification results are shown in Table 3
TABLE 2
TABLE 3
As can be seen from the data in table 3, the method for identifying the true or false five-grain strong aromatic Chinese spirits provided in this embodiment detects the carbon isotopes of ethanol and ethyl caproate by using a carbon isotope determination technique based on the difference between the true or false five-grain strong aromatic Chinese spirits and the carbon isotopes of ethyl caproate, and discriminates and classifies the two carbon isotopes by using a linear discriminant analysis method, and the result shows that: for the test sample of this example, 100.0% of the original grouped observations were correctly classified, and 100.0% of the cross-validated grouped observations were also correctly classified, i.e., true and false discrimination was accurate.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (9)
1. The method for identifying the authenticity of the five-grain strong aromatic Chinese spirits is characterized by comprising the following steps of: the method for identifying the true and the false comprises the following steps: (1) measuring the numerical values of ethanol carbon isotopes and ethyl caproate carbon isotopes in a five-grain strong aromatic Chinese spirit true wine sample by using a gas chromatography-combustion-isotope ratio mass spectrometer, and taking the numerical values as true wine sample data; (2) determining the numerical values of the carbon isotopes of ethanol and the carbon isotopes of ethyl caproate in the sample to be detected by using a gas chromatography-combustion-isotope ratio mass spectrometer as the data of the sample to be detected; (3) and calculating the Mahalanobis distance between the sample data to be detected and the real wine sample data, classifying, and judging the truth of the sample to be detected.
2. The method for identifying the true and false of the five-grain Luzhou-flavor liquor is characterized in that in the step (1), the step of measuring the ethanol carbon isotope in the five-grain Luzhou-flavor liquor sample is that 200 mu L of the five-grain Luzhou-flavor liquor sample is diluted by 1m L of acetone, mixed uniformly, placed in a 2ml gas chromatography bottle and subjected to sample injection measurement, and the step of measuring the ethyl hexanoate carbon isotope in the five-grain Luzhou-flavor liquor sample is directly subjected to sample injection measurement.
3. The method for identifying the authenticity of the specimen according to claim 1, wherein in the step (2), the step of diluting the carbon isotope of ethanol in the specimen with 1m L acetone to 200 μ L specimen, mixing uniformly, placing in a 2ml gas chromatography bottle, and injecting a sample to determine, and the step of directly injecting the carbon isotope of ethyl hexanoate in the specimen to determine.
4. The method for identifying the true and false of the five-grain strong aromatic liquor according to claim 1 is characterized in that in the step (1), the instrument conditions for measuring the ethanol carbon isotope in the five-grain strong aromatic liquor sample are that the chromatographic conditions comprise that the injection port temperature is 180 ℃, the flow rate is 1.0m L/min, the temperature programming is carried out on the initial temperature of 40 ℃, the initial temperature of 5min, the temperature is increased to 50 ℃ at the rate of 1 ℃/min, the initial temperature is maintained for 1min, the temperature is increased to 200 ℃ at the rate of 15 ℃/min, the temperature is maintained for 2min, the split ratio is 50:1, and the combustion condition is 1000 ℃.
5. The method for identifying the authenticity as claimed in claim 1, wherein in the step (1), the apparatus for measuring the carbon isotope of ethyl hexanoate in the sample of the five-grain Luzhou-flavor liquor is characterized in that a HP-INNOWAx capillary chromatographic column is adopted as a chromatographic condition, high-purity helium is adopted as a carrier gas, the constant flow mode is adopted, the flow rate is 3ml/min, the sample is injected without split flow, the sample injection amount is about 0.3u L-2 u L, the initial temperature of a column incubator is 40 ℃, the temperature is kept for 4min, the temperature is increased to 92 ℃ at 5 ℃/min, the temperature is increased to 230 ℃ at 30 ℃/min, the temperature is kept for 5min, the combustion condition is that the sample injection port temperature is 230 ℃, the oxidation furnace temperature is 960 ℃, the reduction furnace temperature is 640 ℃, the mass spectrum condition is that the ion source high pressure is 10.0kV, and the.
6. The method of claim 5, wherein: the filler of the oxidation furnace is CuO, NiO and Pt.
7. The method for identifying the authenticity as claimed in claim 1, wherein in the step (2), the instrument conditions for measuring the ethanol carbon isotope in the sample to be measured are that the chromatographic conditions are that the injection port temperature is 180 ℃, the flow rate is 1.0m L/min, the temperature is programmed to be raised to the initial temperature of 40 ℃, the initial temperature is kept for 5min, the temperature is raised to 50 ℃ at 1 ℃/min, the initial temperature is kept for 1min, the temperature is raised to 200 ℃ at 15 ℃/min, the initial temperature is kept for 2min, the split ratio is 50:1, and the combustion condition is 1000 ℃.
8. The method for identifying the authenticity as claimed in claim 1, wherein in the step (2), the apparatus for measuring the carbon isotope of ethyl hexanoate in the sample to be measured is characterized in that the chromatographic conditions are that an HP-INNOWAx capillary chromatographic column is adopted, the carrier gas is high-purity helium, the constant-current mode is adopted, the flow rate is 3ml/min, the sample is injected in a non-split-flow manner, the sample injection amount is about 0.3u L-2 u L, the initial temperature of a column incubator is 40 ℃, the sample is kept for 4min, the temperature is increased to 92 ℃ at 5 ℃/min, the temperature is increased to 230 ℃ at 30 ℃/min, the sample injection amount is kept for 5min, the combustion conditions are that the sample injection port temperature is 230 ℃, the temperature of an oxidation furnace is 960 ℃, the temperature of a reduction furnace is 640 ℃, and the mass spectrum conditions are that the ion source.
9. The method of claim 8, wherein: the filler of the oxidation furnace is CuO, NiO and Pt.
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Cited By (3)
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| CN112415118A (en) * | 2020-12-09 | 2021-02-26 | 劲牌有限公司 | Method for identifying true and false composite finished white spirit |
| CN113917061A (en) * | 2021-10-22 | 2022-01-11 | 贵州大学 | Detection and identification method for volatile substances of Maotai-flavor base liquor |
| CN114062556A (en) * | 2021-11-19 | 2022-02-18 | 泸州老窖集团有限责任公司 | Carbon isotope composition detection method for white spirit flavor substances |
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| CN114062556B (en) * | 2021-11-19 | 2023-10-31 | 泸州老窖集团有限责任公司 | Carbon isotope composition detection method for white spirit flavor substances |
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