Method for evaluating quality stability of Maotai-flavor round new wine

Abstract

The invention belongs to the technical field of wine brewing, and relates to a method for evaluating the quality stability of Maotai-flavor round new wine. The method is based on a gas chromatography technology, and comprises the following steps: detecting chemical components of new wine and a reference standard sample in each turn, constructing a fingerprint spectrum, and carrying out full-spectrum peak alignment and matching on chromatograms of the sample and the reference standard sample by using a fingerprint spectrum similarity evaluation system, so as to generate a control fingerprint spectrum and calculate the similarity. According to the method, the quality consistency of the new wine in each round can be effectively evaluated, the process stability in the production process is monitored, and a scientific basis is provided for quality control of the new wine.

Description

Technical Field

[0001] The invention belongs to the technical field of wine making and relates to a method for evaluating the quality stability of new Maotai-flavor wine. Background Art

[0002] Fingerprint quality control technology refers to the use of certain analytical methods to obtain a chromatogram or spectrum that can represent the characteristics of the sample after the sample is properly processed. [1] . Fingerprint technology is an important technology for identifying and evaluating sample quality, stability and authenticity. By detecting the characteristics of various chemical components in the sample, a unique "fingerprint" is formed, which is similar to the uniqueness and reproducibility of human fingerprints. At present, the existing technologies for fingerprints mostly use instruments such as gas chromatography (GC), gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), nuclear magnetic resonance spectrometer (NMR) and nuclear magnetic resonance spectrometer (FT-IR). These instruments can be used to separate and identify volatile and non-volatile components in wine. By establishing a standard reference fingerprint map, the sample to be tested can be compared with the standard map to quickly determine whether the sample quality is qualified. At the same time, it can be used to monitor the stability of samples during the production process to ensure the consistency of the quality of each batch of samples.

[0003] In the process of brewing liquor, the fermentation liquor is produced in batches according to different fermentation rounds, and its chemical composition and flavor characteristics may vary between different rounds. The traditional liquor quality evaluation method mainly relies on sensory evaluation and the determination of some physical and chemical indicators. This method has problems such as strong subjectivity and poor stability. In recent years, with the development of chromatography technology, chromatographic fingerprints have been widely used in the quality control of traditional Chinese medicines as a tool for characterizing complex chemical systems. However, there has been no systematic research and patent protection for the application of this technology in the quality control of liquor fermentation.

[0004] The quality and stability of new wines of the Maotai-flavor cycle are the prerequisites for ensuring the high quality of its products. Traditional brewing of liquor usually relies on sensory evaluation to evaluate the quality of new wines. The objective quality stability evaluation method based on instrumental analysis will help promote the optimization and upgrading of the modernization and digitalization of the Maotai-flavor liquor industry. Therefore, how to scientifically, accurately and quickly determine the quality stability of new wines of the Maotai-flavor cycle needs to be solved urgently. The fingerprint spectrum of Maotai-flavor new wines constructed by GC can quickly reflect the distribution of chemical components and contents of new wines of each cycle. It has the advantages of obvious characteristics, strong specificity and good reproducibility, and is easy and fast to operate. It can be used to evaluate the quality stability of new wines of each production cycle, so as to control the quality of wines produced under different environments and different personnel in real time. The fingerprint spectrum is undoubtedly a simple and fast analysis method for multi-component and multi-index analysis and discrimination of Maotai-flavor new wines. Summary of the invention

[0005] The present invention aims to evaluate the stability quality of new wines of Maotai-flavor rounds by using fingerprint technology. First, the consistency of product quality can be ensured. The chemical composition of new wines of different rounds can be monitored to ensure that the new wines of each round are consistent in quality and flavor. Secondly, the stability of the production process is controlled. The stability of each link in the production process is detected by fingerprint, and the unstable factors in the process are discovered and solved in time to ensure the quality of the final product. At the same time, the quality of the raw materials used can be evaluated. The quality stability of the raw materials used for brewing (such as sorghum, wheat, water, etc.) can be tracked by fingerprint technology to ensure that different batches of raw materials will not have a significant impact on the quality of the new wine. And the research and development efficiency of the product can also be improved. The influence of new formulas, new processes or new environments on the quality of new wines of Maotai-flavor rounds can be quickly and accurately analyzed by fingerprint technology, and the production formula or process can be optimized in time to accelerate the research and development process of new products. In short, the quality stability of new wines of Maotai-flavor rounds can be evaluated by fingerprint technology, and the quality of products can be systematically and scientifically monitored and guaranteed, the production process can be optimized, the consistency and authenticity of products can be ensured, and the competitiveness and market recognition of brands can be improved.

[0006] The method of the present invention can efficiently and accurately construct the characteristic chromatographic fingerprint of new Maotai-flavor liquor, and on this basis, scientifically evaluate the stability of liquors from different batches, providing a reliable basis for the quality control of Maotai-flavor liquor.

[0007] In order to make the grade evaluation and acceptance of new liquor in the round of Maotai-flavor liquor more objective, the present invention takes professional and traditional sensory evaluation samples as reference standard samples, and constructs the fingerprint of Maotai-flavor liquor by randomly sampling and testing the new liquor in the round of Maotai-flavor liquor through gas chromatograph, and forms a control fingerprint to monitor whether the new liquor in different rounds is consistent, so as to ensure the stability of the new liquor in each round in quality and flavor, and secondly to control the stability of the production process, detect the stability of each link in the production process through fingerprint, timely discover and solve the unstable factors in the process, ensure the quality of the final product, and provide scientific support for the grading, classification and stability evaluation of new liquor from the digital information level.

[0008] In some embodiments, the present invention provides a method for constructing a liquor fingerprint, characterized in that it comprises the following steps:

[0009] Take the liquor sample to be tested and the reference standard sample of the same round as the liquor sample to be tested, and use gas chromatography to detect them, so as to obtain the chromatograms of the liquor sample to be tested and the reference standard sample respectively; calibrate and match the chromatograms of the liquor sample to be tested and the reference standard sample to obtain the liquor control fingerprint.

[0010] The detection conditions of the gas chromatography method include: the chromatographic column is an Agilent DB-WAX UI chromatographic column; the heating program adopted by the chromatographic column is: the initial temperature is 30-70°C, maintained for 3-20 minutes, increased to 80-120°C at 3-20°C / min, increased to 150-350°C at 5-30°C / min, and maintained for 3-25 minutes; the carrier gas flow rate is 0.5-3mL / min, constant flow.

[0011] In some embodiments, the method comprises:

[0012] An internal standard solution is added to the liquor sample to be tested and the reference standard sample of the same round as the liquor sample to be tested. The preparation steps of the internal standard solution include the following steps: tert-amyl alcohol, n-amyl acetate and 2-ethylbutyric acid are taken respectively, mixed, and an internal standard solution is obtained.

[0013] In some embodiments, a Chinese medicine chromatographic fingerprint similarity evaluation system is used to synthesize a reference fingerprint of the liquor.

[0014] In some embodiments, the chromatograms of the liquor sample to be tested and the reference standard sample are imported into a similarity evaluation system for Chinese medicine chromatographic fingerprints, and the chromatogram of the reference standard sample is used as a reference spectrum to perform full spectrum peak matching and multi-point correction, and a control fingerprint is generated by the average method.

[0015] The method based on the traditional Chinese medicine chromatographic fingerprint similarity evaluation system provided by the present invention can systematically construct the GC chromatographic fingerprint of the new round of Maotai-flavor liquor and accurately evaluate the stability of its quality.

[0016] By using standard reference samples and full-spectrum peak matching common peaks, and generating standard fingerprints using the average method, and tracing the full-spectrum peak fingerprints to analyze the new wines in each round, we can more comprehensively understand the quality and stability of the new sauce-flavored wines.

[0017] In some embodiments, the liquor is a sauce-flavor liquor.

[0018] In some embodiments, the liquor is liquor from rounds 1 to 7.

[0019] In some embodiments, the method further comprises preparing a mixed solution of standard substances, and detecting the mixed solution by chromatography to obtain a chromatogram of the standard substances.

[0020] In some embodiments, the number of liquor samples used to construct the control fingerprint of the liquor is no less than 30.

[0021] In some embodiments, the reference standard samples are obtained by conducting sensory evaluations of liquors from rounds 1 to 7 by national liquor tasters to determine the reference standard samples for each round.

[0022] In some embodiments, the weight ratio of tert-amyl alcohol, n-amyl acetate and 2-ethylbutyric acid in the internal standard solution is 1:(1-3):(1-3).

[0023] In some embodiments, the solvent used for mixing the internal standard solution is ethanol solution.

[0024] In some embodiments, the solvent used for mixing the internal standard solution is 30% to 90% v / v ethanol solution.

[0025] In some embodiments, the solvent used for mixing the internal standard solution is 30% to 70% v / v ethanol solution.

[0026] In some embodiments, the solvent used for mixing the internal standard solution is 30% to 60% v / v ethanol solution.

[0027] In some embodiments, the internal standard solution is sealed and stored at -10°C to 10°C.

[0028] In some embodiments, the internal standard solution is sealed and stored at 0°C to 10°C.

[0029] In some embodiments, the internal standard solution is sealed and stored at 0°C to 4°C.

[0030] In some embodiments, the detection conditions of the gas chromatography method are as follows: the column length of the chromatographic column is 10 to 60 m, the inner diameter is 0.1 to 0.5 mm, and the film thickness is 0.1 to 5 μm; the detector temperature is 150 to 300° C.; the inlet temperature is 150 to 230° C.; the septum purge flow rate is 1 to 20 mL / min, and the tail gas flow rate is 10 to 50 mL / min; the injection volume is 0.1 to 2 μL; the injection method is split injection, and the split ratio is 10:1 to 40:1.

[0031] In some embodiments, the length of the chromatographic column is 10 to 50 m.

[0032] In some embodiments, the length of the chromatographic column is 10 to 40 m.

[0033] In some embodiments, the length of the chromatographic column is 10 to 30 m.

[0034] In some embodiments, the inner diameter of the chromatographic column is 0.1-0.4 mm.

[0035] In some embodiments, the inner diameter of the chromatographic column is 0.1-0.3 mm.

[0036] In some embodiments, the inner diameter of the chromatographic column is 0.2-0.3 mm.

[0037] In some embodiments, the film thickness of the chromatographic column is 0.1-4 μm.

[0038] In some embodiments, the film thickness of the chromatographic column is 0.1-3 μm.

[0039] In some embodiments, the film thickness of the chromatographic column is 0.1-1 μm.

[0040] In some embodiments, the heating program is: initial temperature 30-60°C, maintained for 3-15 min, increased to 80-110°C at 3-15°C / min, increased to 150-300°C at 5-25°C / min, and maintained for 3-20 min.

[0041] In some embodiments, the heating program is: initial temperature 30-50°C, maintained for 3-10 min, increased to 80-100°C at 3-10°C / min, increased to 150-250°C at 5-20°C / min, and maintained for 3-15 min.

[0042] In some embodiments, the temperature rising program is: initial temperature 30-40°C, maintained for 5-10 min, raised to 80-100°C at 5-10°C / min, raised to 200-200°C at 5-15°C / min, maintained for 5-15 min.

[0043] In some embodiments, the detector temperature is 150-250°C.

[0044] In some embodiments, the detector temperature is 180-250°C.

[0045] In some embodiments, the detector temperature is 200-250°C.

[0046] In some embodiments, the injection port temperature is 150-250°C.

[0047] In some embodiments, the injection port temperature is 180-250°C.

[0048] In some embodiments, the injection port temperature is 200-250°C.

[0049] In some embodiments, the carrier gas is nitrogen with a purity of ≥99.999%.

[0050] In some embodiments, the carrier gas flow rate is 0.5 to 2.5 mL / min.

[0051] In some embodiments, the carrier gas flow rate is 0.5-2 mL / min.

[0052] In some embodiments, the carrier gas flow rate is 0.5-1.5 mL / min.

[0053] In some embodiments, the septum purge flow rate is 1 to 15 mL / min.

[0054] In some embodiments, the septum purge flow rate is 1 to 10 mL / min.

[0055] In some embodiments, the septum purge flow rate is 1 to 5 mL / min.

[0056] In some embodiments, the tail gas sweep flow rate is 10 to 40 mL / min.

[0057] In some embodiments, the tail gas sweep flow rate is 10 to 30 mL / min.

[0058] In some embodiments, the tail gas sweep flow rate is 10 to 25 mL / min.

[0059] In some embodiments, the injection volume is 0.1-1.5 μL.

[0060] In some embodiments, the injection volume is 0.1-1 μL.

[0061] In some embodiments, the injection volume is 0.5-1 μL.

[0062] In some embodiments, the split ratio is 20:1 to 40:1.

[0063] In some embodiments, the split ratio is 20:1 to 30:1.

[0064] In some embodiments, the split ratio is 25:1 to 30:1.

[0065] In some embodiments, the detection conditions of the gas chromatography are as follows: chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; the heating program adopted by the chromatographic column is: initial temperature 40°C, maintained for 5min, increased to 100°C at 5.0°C / min, increased to 200°C at 10°C / min, maintained for 10min; detector temperature: 250°C; injection port temperature: 250°C; carrier gas type is nitrogen, carrier gas flow rate: 0.7mL / min, constant flow; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0066] In some embodiments, the present invention provides a method for evaluating the quality of liquor, characterized in that the fingerprint of the liquor is constructed by the method described, and the quality of the liquor is judged based on the fingerprint.

[0067] In some embodiments, the method is used to evaluate the quality stability of liquor.

[0068] In some embodiments, the liquor is a sauce-flavor liquor.

[0069] In some embodiments, the method of application includes:

[0070] (a) constructing the control fingerprints of liquor samples of each round according to the described method;

[0071] (b) using gas chromatography to detect the liquor sample to be tested, and obtaining a spectrum of the sample to be tested;

[0072] (c) using a fingerprint similarity evaluation system to analyze the fingerprint of the liquor sample to be tested and the reference fingerprint of the same round of the liquor sample to be tested, and calculate the similarity.

[0073] In some embodiments, the liquor is a sauce-flavor liquor.

[0074] In some embodiments, the liquor is liquor from rounds 1 to 7.

[0075] In some embodiments, the number of liquor samples used to construct the control fingerprint maps of liquor samples in each round is no less than 30.

[0076] In some embodiments, the fingerprint similarity evaluation system is a traditional Chinese medicine chromatographic fingerprint similarity evaluation system.

[0077] In some embodiments, the Chinese medicine chromatographic fingerprint similarity evaluation system is a Chinese medicine chromatographic fingerprint similarity evaluation system (2012 version).

[0078] In some embodiments, in the application, the similarity is not less than 0.900, and the quality of the sample to be tested is determined to be stable.

[0079] In some embodiments, the similarity is not less than 0.950, and the quality of the sample to be tested is determined to be stable.

[0080] In some embodiments, the similarity is not less than 0.990, and the quality of the sample to be tested is determined to be stable. BRIEF DESCRIPTION OF THE DRAWINGS

[0081] Figure 1 This is the chromatogram of the characteristic standard substance of the new Maotai-flavor liquor.

[0082] Figure 2 This is the fingerprint map of a new round of Maotai-flavor liquor.

[0083] Figure 3 This is the comparison chart R1 of the first round of new wine with sauce aroma.

[0084] Figure 4 This is the fingerprint map of the second round of new Maotai-flavor liquor.

[0085] Figure 5 This is the comparison chart R2 of the second round of new wine with sauce aroma.

[0086] Figure 6 This is the fingerprint map of the third round of new Maotai-flavor liquor.

[0087] Figure 7 This is the comparison chart R3 of the third round of new wines with sauce aroma.

[0088] Figure 8 This is the fingerprint map of the fourth round of new Maotai-flavor liquor.

[0089] Fig. 9 This is the comparison chart R4 of the four rounds of new wines with sauce aroma.

[0090] Fig.10 This is the fingerprint of the fifth round of new Maotai-flavor liquor.

[0091] Fig.11 This is the comparison chart R5 of the fifth round of new wines with sauce aroma.

[0092] Fig.12 This is the fingerprint map of the sixth round of new Maotai-flavor liquor.

[0093] Fig.13 This is the comparison chart R6 of the six rounds of new wines with sauce aroma.

[0094] Fig.14 This is the fingerprint of the seventh round of new wine with Maotai aroma.

[0095] Fig.15 This is the comparison chart R7 of the seven rounds of new wines with sauce aroma.

[0096] Fig.16 This is a comparison of fingerprint maps of new wines from rounds 1 to 7 of the sauce-flavor type.

[0097] Fig.17 This is the fingerprint spectrum used in the stability evaluation of the second-round new Maotai-flavor liquor.

[0098] Fig.18 This is the fingerprint spectrum of the stability evaluation of five rounds of new Maotai-flavor liquor.

[0099] Fig.19 Chromatograms of the same sample measured for seven instrument parameters. DETAILED DESCRIPTION

[0100] The technical solution of the present invention is further described below by specific embodiments, which do not limit the protection scope of the present invention. Some non-essential modifications and adjustments made by others based on the concept of the present invention are still protected by the present invention.

[0101] 1 Materials and methods

[0102] 1.1 Materials, reagents and instruments

[0103] Reagents and standards: Ultrapure water, Millipore, USA. Ethanol (chromatographic grade), acetaldehyde, propionaldehyde, isobutyraldehyde, ethyl formate, diethoxymethane, ethyl acetate, acetal, methanol, isovaleraldehyde, 2-pentanone, sec-butyl alcohol, ethyl butyrate, propanol, n-butyl acetate, isobutyl alcohol, isoamyl acetate, 2-pentanol, ethyl valerate, butanol, isopentanol, ethyl hexanoate, n-pentanol, ethyl heptanoate, ethyl lactate, n-hexanol, butyl hexanoate, butyl octanoate, furfural, benzaldehyde, propionic acid, (RR(+)+SS(-))-2,3 -Butanediol, isobutyric acid, 1,2-propylene glycol, n-butyric acid, isovaleric acid, valeric acid, ethyl phenylacetate, caproic acid, β-phenylethanol, heptanoic acid, octanoic acid, ethyl palmitate, ethyl oleate, ethyl linoleate, tert-amyl alcohol, n-amyl acetate and 2-ethylbutyric acid standards (purity ≥ 98%) were purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., ethyl isovalerate, acetic acid and acetic acid were purchased from Aike Reagents, and 2,3-butanediol (meso) was purchased from Sigma.

[0104] Instrument: 7890B gas chromatograph (Agilent).

[0105] Other instruments or reagents not specifically described are known reagents and instruments commonly used in the art.

[0106] 1.2 Sample preparation and test methods

[0107] Reference standard samples: 10 national-level liquor tasters conducted sensory evaluations on the new liquors from rounds 1 to 7 of the sauce-flavor liquor to determine the reference standard samples for each round.

[0108] Standard substance mixture: Accurately weigh the reference mass of the standard substance into a 100mL volumetric flask (pre-add a portion of 60% ethanol solution to the volumetric flask), and dilute to the mark with 60% ethanol solution. The reference mass of the standard substance is as follows:

[0109] Acetaldehyde 0.04g; n-propanal, isobutyraldehyde, ethyl formate, diethoxymethane, isovaleraldehyde, 2-pentanone, sec-butanol, ethyl butyrate, ethyl isovalerate, n-butyl acetate, isobutanol, isopentyl acetate, 2-pentanol (sec-pentanol), ethyl valerate, butanol, isopentanol, n-pentanol, 2,3-hydroxy 2-butanone (acetaldehyde), ethyl heptanoate, n-hexanol, butyl hexanoate, ethyl octanoate, furfural, benzaldehyde, propionic acid, RR(+)+ SS(-)-2,3-butanediol, isobutyric acid, 2,3-butanediol (meso), 1,2-propylene glycol, n-butyric acid, isovaleric acid, valeric acid, ethyl phenylacetate, caproic acid, β-phenylethanol, heptanoic acid, octanoic acid, ethyl palmitate, ethyl oleate, ethyl linoleate, 0.02g each; n-propanol 0.05g; ethyl caproate, ethyl lactate, acetic acid, 0.20g each; ethyl acetate 0.30g; acetal, methanol 0.03g. Preparation of three internal standard solutions: weigh 2.0g tert-amyl alcohol, 2.0g n-amyl acetate, 2.0g 2-ethylbutyric acid into a 100mL volumetric flask, dilute to 100mL with 60% v / v ethanol solution, mix well, and store in a sealed refrigerator at 0℃~4℃.

[0110] Preparation of samples to be tested: Randomly select 30 samples from each round of Maotai-flavor liquor from rounds 1 to 7, then accurately pipette 10 mL from each of these samples, transfer them to their respective test tubes, accurately add 0.20 mL of three internal standard solutions to each, mix well and set aside.

[0111] Preparation of reference standard samples: Accurately pipette 10.0 mL of the corresponding reference standard samples from rounds 1 to 7, transfer them to their respective test tubes, accurately add 0.20 mL of the three internal standard solutions, mix well and set aside.

[0112] Detection steps: Accurately aspirate 0.5 μL of the sample to be tested or the reference standard sample, inject it into the gas chromatograph, measure, record the chromatogram, and obtain the sample chromatogram of the sample to be tested or the reference standard sample in each round.

[0113] 1.3 Instrument conditions

[0114] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 5min, increase to 100℃ at 5.0℃ / min, increase to 200℃ at 10℃ / min, hold for 10min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas flow rate: 0.7mL / min, constant flow; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0115] 1.4 Fingerprint establishment

[0116] The sample chromatogram was imported into the "Chinese Herbal Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)". Since the ethanol peak (retention time of 7.5min) accounts for a large proportion and will interfere with other chromatographic peaks, the data with a retention time of 8min was removed before the fingerprint similarity analysis. Then the chromatogram of the reference standard sample was selected as the reference spectrum. In order to more comprehensively reflect the characteristics of more substances in each sample, full spectrum peak matching was selected here, and multi-point correction was used to eliminate the time error of each spectrum. After automatic matching, the common peak was obtained, and the reference fingerprint spectrum was generated by the average method, and the similarity was calculated. A high similarity value indicates that the chemical composition between the samples is highly consistent, otherwise the difference is large. At the same time, the reference fingerprint spectrum of each round of new wine is generated for the later evaluation of the quality stability of the wine samples.

[0117] Example 1 Establishment of fingerprint spectrum of new wine of Maotai-flavor type and evaluation of its stability

[0118] Use GC to detect the standard substance mixture according to the optimal instrument conditions in step "1.3 Instrument Conditions" and obtain the corresponding characteristic substance chromatogram. Figure 1 At the same time, the same method was used to detect 30 samples and reference standard samples from rounds one to seven. The chromatograms of each round of samples and reference standard samples were exported in AIA format, and then the full spectrum of each wine sample was imported into the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)" for spectrum analysis. Among them, the reference standard sample chromatogram of round one was S1, and the sample chromatograms were S2~S31; the reference standard sample chromatogram of round two was S32, and the sample chromatograms were S33~S62; the reference standard sample chromatogram of round three was S63, and the sample chromatograms were S64~S93; the reference standard sample chromatogram of round four was S94, and the sample chromatograms were S95~S124; the reference standard sample chromatogram of round five was S94. is S125, and the sample chromatograms are S126-S155; the reference standard sample chromatogram of the sixth round is S156, and the sample chromatograms are S157-S186; the reference standard sample chromatogram of the seventh round is S187, and the sample chromatograms are S188-S217. The operation is performed according to the method described in "1.4 Fingerprint Spectrum Establishment", and each reference standard sample of each round is used as the reference spectrum of each corresponding round, and the time width is set to 0.1s. All common peak retention times are multi-point corrected, and then the full spectrum peak is automatically matched to generate seven rounds of fingerprint spectra and control fingerprint spectra R1-R7 of each round. Finally, the generated control fingerprint spectra are exported to form new control fingerprint spectra (R1-R7) of each round, as shown in Figure 3 , 5 , 7, 9, 11, 13, and 15, and then the similarity of each round is calculated, as shown in Tables 1 to 7.

[0119] Example 2 Establishment of fingerprint spectrum and stability evaluation of the first round of new wine of Maotai-flavor type

[0120] According to the method described in Example 1, the spectrum analysis was performed using the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Edition)". The full spectrum peak fingerprint of a round of new wine samples is shown in Figure 2 The similarity results are shown in Table 1. Compared with the control fingerprint R1 generated by full spectrum peak matching, the similarities of the first-round new wine samples S2 to S31 of the sauce-flavored type are between 0.961 and 0.998, all greater than 0.9, which can indicate that the quality of the 30 randomly selected samples is stable. The control fingerprint R1 generated by full spectrum peak matching can be used as a quality stability judgment for the later samples of the first-round new wine of the sauce-flavored type, that is, Figure 3 The figure shows the reference fingerprint of the first-round new liquor of the sauce-flavor type R1. The reference fingerprint of the first-round new liquor of the sauce-flavor type is applied to the process production of the sauce-flavor liquor to evaluate the quality stability of the first-round new liquor produced by different workshops and teams in the later stage.

[0121] Table 1 Similarity of fingerprint spectra of the first round of new wines with sauce aroma

[0122]

[0123]

[0124] Example 3 Establishment of fingerprint spectrum and stability evaluation of second-round new wine of Maotai-flavor type

[0125] According to the method described in Example 1, the spectrum analysis was performed by the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)". As shown in Table 2, compared with the control fingerprint spectrum R2 generated after full spectrum peak matching, the similarities of the second-round Maotai-flavor new wine samples S33 to S62 were between 0.928 and 1.000, all greater than 0.9, which can indicate that the quality of the 30 randomly selected samples is stable, and the control fingerprint spectrum R2 generated after full spectrum peak matching can be used as a sample quality stability judgment for the later period of the second-round Maotai-flavor new wine, that is, Figure 5 Shown is the reference fingerprint map R2 of the second round of new Maotai-flavor liquor.

[0126] Table 2 Similarity of fingerprint spectra of the second round of new wines with Maotai aroma

[0127]

[0128]

[0129] Example 4 Establishment of fingerprint spectrum and stability evaluation of three rounds of new wine of Maotai-flavor type

[0130] According to the method described in Example 1, the spectrum analysis was performed by the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)". As shown in Table 3, compared with the control fingerprint spectrum R3 generated after full spectrum peak matching, the similarities of the three-round new wine samples S64 to S93 of the sauce-flavored type were between 0.900 and 1.000, all greater than 0.9, which can indicate that the quality of the 30 randomly selected samples is stable, and the control fingerprint spectrum R3 generated after full spectrum peak matching can be used as a sample quality stability judgment for the late stage of the three-round new wine of the sauce-flavored type, that is, Figure 7 Shown is the reference fingerprint map R3 of the third round of new Maotai-flavor liquor.

[0131] Table 3 Similarity of fingerprint spectra of three rounds of new wines with sauce aroma

[0132]

[0133]

[0134] Example 5 Establishment of fingerprint spectrum and stability evaluation of four-round new wine of Maotai-flavor type

[0135] According to the method described in Example 1, the spectrum analysis was performed by the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)". As shown in Table 4, compared with the control fingerprint spectrum R4 generated after full spectrum peak matching, the similarities of the four-round sauce-flavor new wine samples S95-S124 were between 0.926 and 1.000, all greater than 0.9, which can indicate that the quality of the 30 randomly selected samples is stable, and the control fingerprint spectrum R4 generated after full spectrum peak matching can be used as a sample quality stability judgment for the late stage of the four-round sauce-flavor new wine, that is, Fig. 9 Shown is the reference fingerprint spectrum R4 of the fourth round of new wine of Maotai-flavor type.

[0136] Table 4 Similarity of fingerprint spectra of four rounds of new wines with Maotai aroma

[0137]

[0138]

[0139] Example 6 Establishment of fingerprint spectrum and stability evaluation of five-round new wine of Maotai-flavor type

[0140] According to the method described in Example 1, the spectrum analysis was performed by the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)". As shown in Table 5, compared with the control fingerprint spectrum R5 generated after full spectrum peak matching, the similarities of the five-round new wine samples S126 to S155 of the sauce-flavored type were between 0.923 and 1.000, all greater than 0.9, which can indicate that the quality of the 30 randomly selected samples is stable, and the control fingerprint spectrum R5 generated after full spectrum peak matching can be used as a sample quality stability judgment for the late stage of the five-round new wine of the sauce-flavored type, that is, Fig.11 Shown is the reference fingerprint map R5 of the fifth round of new Maotai-flavor liquor.

[0141] Table 5 Similarity of fingerprint spectra of five rounds of new wines with Maotai aroma

[0142]

[0143]

[0144] Example 7 Establishment of fingerprint spectrum and stability evaluation of six-round new liquor of Maotai-flavor type

[0145] According to the method described in Example 1, the spectrum analysis was performed using the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)". As shown in Table 6, compared with the control fingerprint R6 generated after full spectrum peak matching, the similarities of the six-round Maotai-flavor new wine samples S157 to S186 were between 0.931 and 1.000, all greater than 0.9, which can indicate that the quality of the 30 randomly selected samples is stable, and the control fingerprint R6 generated after full spectrum peak matching can be used as a sample quality stability judgment for the later period of the six-round Maotai-flavor new wine, that is, Fig.13 Shown is the reference fingerprint spectrum R6 of the sixth round of new Maotai-flavor liquor.

[0146] Table 6 Similarity of fingerprint spectra of six rounds of new Maotai-flavor liquor

[0147]

[0148]

[0149] Example 8 Establishment of fingerprint spectrum and stability evaluation of seven-round new wine of Maotai-flavor type

[0150] According to the method described in Example 1, the spectrum analysis was performed by the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)". As shown in Table 7, compared with the control fingerprint spectrum R7 generated after full spectrum peak matching, the similarities of the seven-round Maotai-flavor new wine samples S188-S217 were between 0.943 and 1.000, all greater than 0.9, which can indicate that the quality of the 30 randomly selected samples is stable, and the control fingerprint spectrum R7 generated after full spectrum peak matching can be used as a sample quality stability judgment for the late Maotai-flavor seven-round new wine, that is, Fig.15 Shown is the reference fingerprint spectrum R7 of the seventh round of new wine of Maotai-flavor type.

[0151] Table 7 Similarity of fingerprint spectra of seven rounds of new wines with Maotai aroma

[0152]

[0153]

[0154] Example 9 Similarity evaluation of new liquors of each round in sauce-flavored style

[0155] The first to seventh rounds of reference standard samples S1, S32, S63, S94, S125, S156, and S187 were tested, and the chromatograms of the seven rounds of reference standard samples were exported in AIA format. All data were then imported into the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (2012 Version)" for spectrum analysis. The operation was performed according to the method described in "1.4 Fingerprint Spectrum Establishment". The first round of reference standard sample S1 was selected as the reference spectrum, the time width was set to 0.1s, and all common peak retention times were multi-point corrected. Then, the full spectrum peak was automatically matched, and the similarity of the seven rounds of reference standard samples was calculated. As shown in Table 8 and Fig.16 As shown in the figure, each round of Maotai-flavor new wine has its own style characteristics. Taking the first round reference standard sample S1 as the reference, the similarities of the other six rounds are between 0.225 and 0.888, which are obviously different. Therefore, establishing the similarity of fingerprint spectra of each round can well judge the quality stability of each round of new wine and distinguish it from other rounds of new wine.

[0156] Table 8 Similarity comparison of reference standard samples of sauce-flavored flavors from rounds 1 to 7

[0157] Round Name S1 S1 1.000 S32 0.729 S63 0.599 S94 0.225 S125 0.396 S156 0.888 S187 0.666

[0158] Test Example 1 Evaluation of the stability of the second-round new wine of Maotai-flavor

[0159] Second-round new wine samples produced by different workshops and different teams were randomly selected for GC detection (the sample number consists of three groups of numbers, the middle number is the second round, and the two sides are marked according to the sampling workshop and sequence) and analyzed according to the fingerprint construction method described in "1.4 Fingerprint Establishment". The second-round control fingerprint map R2 constructed by the present invention was used as a reference for similarity evaluation, so as to judge the quality stability of the production batch of wine samples.

[0160] From Table 9 and Fig.17 It can be seen that compared with the second round of control fingerprint spectrum R2, except for the 13-2-1 sample with a similarity lower than 0.900, the similarities of the other samples are between 0.942 and 0.999, indicating that the similarity of these nine samples is high and the wine quality is relatively stable, while the wine similarity of 13-2-1 is 0.882, which is quite different from the other samples in quality. The study found that this sample was produced in a newly commissioned workshop, and its brewing environment and microbial community conditions are slightly different from those of the old workshop, so there is a certain difference in the quality of the new wine produced and that of other workshops and teams. It can be seen that by comparing the fingerprint spectrum, the stability of the wine quality under different production conditions can be quickly grasped, so as to timely adjust and improve the brewing process of Maotai-flavor liquor and ensure the consistency of the high quality of the wine.

[0161] Table 9 Similarity of the second round of new wines with Maotai aroma

[0162] sample Second round of comparison 2-2-2. 2-2-1. 3-2-1. 4-2-1. 5-2-1. 6-2-1. 9-2-2. 10-2-2. 11-2-1. 13-2-1. Second round of comparison 1 0.987 0.943 0.942 0.986 0.945 0.999 0.998 0.996 0.981 0.882 2-2-2. 0.987 1 0.984 0.974 0.994 0.976 0.98 0.976 0.989 0.978 0.921 2-2-1. 0.943 0.984 1 0.979 0.974 0.979 0.929 0.923 0.951 0.946 0.935 3-2-1. 0.942 0.974 0.979 1 0.984 0.999 0.925 0.918 0.941 0.966 0.965 4-2-1. 0.986 0.994 0.974 0.984 1 0.984 0.977 0.973 0.983 0.987 0.936 5-2-1. 0.945 0.976 0.979 0.999 0.984 1 0.93 0.922 0.944 0.969 0.965 6-2-1. 0.999 0.98 0.929 0.925 0.977 0.93 1 1 0.995 0.973 0.861 9-2-2. 0.998 0.976 0.923 0.918 0.973 0.922 1 1 0.995 0.969 0.85 10-2-2. 0.996 0.989 0.951 0.941 0.983 0.944 0.995 0.995 1 0.968 0.866 11-2-1. 0.981 0.978 0.946 0.966 0.987 0.969 0.973 0.969 0.968 1 0.947 13-2-1. 0.882 0.921 0.935 0.965 0.936 0.965 0.861 0.85 0.866 0.947 1

[0163] Test Example 2 Evaluation of the stability of five-cycle new wine of Maotai-flavor

[0164] Five rounds of new wine samples produced by different workshops and different teams were randomly selected for GC detection (the numbering is the same as above, consisting of three groups of numbers, the middle number is five rounds, and the two sides are marked according to the sampling workshop and sequence). According to the fingerprint construction method described in "1.4 Fingerprint Spectrum Establishment", the similarity evaluation was performed using the five-round control fingerprint spectrum R5 constructed by the present invention as a reference, so as to judge the quality stability of the production batch wine samples. From Table 10 and Fig.18 It can be seen that compared with the five-round control fingerprint map R5, the similarities of the ten randomly selected five-round new wine samples are between 0.963 and 0.996, all above 0.960, and the brewing production process fluctuates little, indicating that the quality differences of these ten samples are small and the batch stability is high.

[0165] Table 10 Similarity of five rounds of new wines with Maotai aroma

[0166] sample Five rounds of comparison 1-5-29. 1-5-43. 1-5-49. 2-5-3. 3-5-17. 4-5-37. 5-5-57. 6-5-97. 10-5-69. 13-5-23. Five rounds of comparison 1 0.981 0.975 0.988 0.963 0.966 0.974 0.996 0.996 0.967 0.978 1-5-29. 0.981 1 0.999 0.998 0.897 0.991 0.916 0.992 0.962 0.992 0.927 1-5-43. 0.975 0.999 1 0.997 0.884 0.994 0.902 0.988 0.954 0.996 0.913 1-5-49. 0.988 0.998 0.997 1 0.916 0.989 0.931 0.993 0.973 0.989 0.941 2-5-3. 0.963 0.897 0.884 0.916 1 0.867 0.997 0.936 0.982 0.864 0.995 3-5-17. 0.966 0.991 0.994 0.989 0.867 1 0.884 0.979 0.943 0.997 0.894 4-5-37. 0.974 0.916 0.902 0.931 0.997 0.884 1 0.951 0.987 0.883 0.998 5-5-57. 0.996 0.992 0.988 0.993 0.936 0.979 0.951 1 0.983 0.983 0.957 6-5-97. 0.996 0.962 0.954 0.973 0.982 0.943 0.987 0.983 1 0.942 0.989 10-5-69. 0.967 0.992 0.996 0.989 0.864 0.997 0.883 0.983 0.942 1 0.892 13-5-23. 0.978 0.927 0.913 0.941 0.995 0.894 0.998 0.957 0.989 0.892 1

[0167] The present invention uses the fingerprint spectrum of new liquor of Maotai-flavor rounds to construct a new liquor quality stability evaluation method, which can more objectively, accurately and comprehensively monitor samples in real time, scientifically monitor and ensure product quality, optimize production processes, and ensure product stability and authenticity. The method is simple to operate, has high analysis efficiency, is suitable for quality control of large-scale samples, and helps to improve the quality consistency and market competitiveness of liquor production.

[0168] Through the application of the present invention, quality problems caused by process fluctuations in the liquor production process can be greatly reduced, ensuring the long-term stability of the product in the market.

[0169] The fingerprint map of new liquors of Maotai-flavor liquor cycles constructed by the present invention is beneficial to optimizing the data mining technology of Maotai-flavor base liquors, realizing the classification and identification of Maotai-flavor new liquors and the stability judgment, and plays an important role in supplementing and improving the scientific and effective evaluation of the quality of base liquors.

[0170] Comparative Example 1 Comparison of instrument chromatographic parameter optimization

[0171] 1. Instrument conditions

[0172] 1.1 Method 1 (optimal instrument conditions of the present invention)

[0173] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 5min, increase to 100℃ at 5.0℃ / min, increase to 200℃ at 10℃ / min, hold for 10min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas flow rate: 0.7mL / min, constant flow; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0174] 1.2 Method 2

[0175] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 5min, increase to 100℃ at 5.0℃ / min, increase to 200℃ at 10℃ / min, hold for 10min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas flow rate: 1mL / min, constant flow; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0176] 1.3 Method 3

[0177] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 5min, increase to 100℃ at 10.0℃ / min, increase to 150℃ at 15℃ / min, hold for 15min, increase to 200℃ at 20℃ / min, hold for 15min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas flow rate: 0.7mL / min, constant flow; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0178] 1.4 Method 4

[0179] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 5min, increase to 100℃ at 5.0℃ / min, increase to 200℃ at 10℃ / min, hold for 10min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas pressure: 7psi, constant pressure; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0180] 1.5 Method 5

[0181] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 5min, increase to 100℃ at 5.0℃ / min, increase to 200℃ at 10℃ / min, hold for 10min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas flow rate: 1.5mL / min, constant flow; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0182] 1.6 Method 6

[0183] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 5min, increase to 100℃ at 10.0℃ / min, increase to 200℃ at 10℃ / min, hold for 10min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas flow rate: 0.7mL / min, constant flow; septum purge nitrogen flow rate: 3mL / min, tail gas nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0184] 1.7 Method 7

[0185] Chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; chromatographic column temperature: initial temperature 40℃, hold for 10min, increase to 100℃ at 5.0℃ / min, increase to 200℃ at 10℃ / min, hold for 10min; detector temperature: 250℃; injection port temperature: 250℃; carrier gas type is nitrogen, purity ≥99.999%; carrier gas flow rate: 0.7mL / min, constant flow; septum purge flow nitrogen flow rate: 3mL / min, tail gas flow nitrogen flow rate: 25mL / min; injection volume: 0.5μL; split ratio: 30:1.

[0186] 2. Instrument parameter optimization results

[0187] The same sample (four rounds of new wine sample S95) was tested by changing the instrument testing conditions, and other conditions remained unchanged. The sample was prepared according to the method of the present invention. The results obtained after the above 7 instrument parameter conditions were as follows: Fig.19 As shown in the chromatogram, it can be seen that method 1 is the optimal detection parameter condition of the present invention. Compared with the other 6 detection condition parameters, the optimal method can detect the most complete characteristic peaks and better reflect the overall characteristics of the sample.

[0188] 3. Validation of detection methodology

[0189] 3.1 Linear equation and detection and quantification limits of the method

[0190] Under the optimized conditions (method 1), a series of mixed standard solutions of 48 characteristic substances were prepared, and the standard curve was drawn with the peak area (Y) as the ordinate and the mass concentration (X) as the abscissa to obtain the linear regression equation and correlation coefficient (R 2 The results are shown in Table 11. The correlation coefficients of 48 characteristic substances (R 2) is between 0.9909 and 0.9999. Accurately draw a certain amount of four rounds of new wine samples S95, add characteristic standard compound solutions of different concentrations to prepare spiked samples, and process and detect and analyze according to the sample processing steps described in the optimal method (method one) of the present invention. Each added sample is parallelized for 7 times, and the sample background value is detected at the same time. Finally, the average recovery rate and relative standard deviation (RSD) are calculated. As shown in Table 11, the spiked recovery rate of each substance is between 93.38% and 107.06%, and the RSD is between 0.04% and 5.25%, which has good recovery rate and precision, and the detection method meets the requirements.

[0191] Table 11 Linear equation, spike recovery and precision of characteristic substances

[0192]

[0193]

[0194] The above-mentioned implementation modes are only preferred implementation modes of the present application and cannot be used to limit the scope of protection of the present application. Any non-substantial changes and substitutions made by technicians in this field on the basis of the present application shall fall within the scope of protection required by the present application.

[0195] References

[0196] [1] Zheng Yan, Tang Qingli, Wu Tianxiang, et al. Study on the establishment of fingerprint spectrum of Kweichow Moutai by GC-MS[J]. China Brewing, 2008, (09): 74-6+91.

Claims

1. A method for constructing a liquor fingerprint, characterized in that: The following steps are involved: Take the liquor sample to be tested and the reference standard sample of the same round as the liquor sample to be tested, and use gas chromatography to detect, and obtain the chromatograms of the liquor sample to be tested and the reference standard sample respectively; calibrate and match the chromatograms of the liquor sample to be tested and the reference standard sample to obtain the control fingerprint spectrum of the liquor. The detection conditions of the gas chromatography method include: the chromatographic column is an Agilent DB-WAX UI chromatographic column; the heating program adopted by the chromatographic column is: the initial temperature is 30-70°C, maintained for 3-20 minutes, increased to 80-120°C at 3-20°C / min, increased to 150-350°C at 5-30°C / min, and maintained for 3-25 minutes; the carrier gas flow rate is 0.5-3mL / min, constant flow.

2. The method according to claim 1, characterized in that include: An internal standard solution is added to the liquor sample to be tested and the reference standard sample of the same round as the liquor sample to be tested, and the preparation step of the internal standard solution comprises the following steps: tert-amyl alcohol, n-amyl acetate and 2-ethylbutyric acid are respectively taken and mixed to obtain an internal standard solution; Preferably, a Chinese medicine chromatographic fingerprint similarity evaluation system is used to synthesize the reference fingerprint of the liquor; Preferably, the chromatograms of the liquor sample to be tested and the reference standard sample are introduced into a similarity evaluation system for Chinese medicine chromatographic fingerprints, the chromatogram of the reference standard sample is used as a reference spectrum, all common peak retention times are subjected to multi-point correction and full-spectrum peak matching, and a control fingerprint spectrum is generated by an average method; Preferably, the liquor is a Maotai-flavor liquor; Preferably, the liquor is liquor from rounds 1 to 7; Preferably, the method further comprises preparing a mixed solution of standard substances, and detecting by chromatography to obtain a chromatogram of the standard substances; Preferably, the number of liquor samples used to construct the control fingerprint of the liquor is no less than 30.

3. The method according to claim 1, characterized in that The reference standard samples are determined by national-level liquor tasters through sensory evaluation of liquors from rounds 1 to 7 to determine the reference standard samples for each round.

4. The method according to claim 1, characterized in that The weight ratio of tert-amyl alcohol, n-amyl acetate and 2-ethylbutyric acid in the internal standard solution is 1:(1-3):(1-3); Preferably, the solvent used for mixing the internal standard solution is an ethanol solution; Preferably, the solvent used for mixing the internal standard solution is 30% to 90% v / v ethanol solution; Preferably, the solvent used for mixing the internal standard solution is 30% to 70% v / v ethanol solution; Preferably, the solvent used for mixing the internal standard solution is 30% to 60% v / v ethanol solution; Preferably, the internal standard solution is sealed and stored at -10°C to 10°C; Preferably, the internal standard solution is sealed and stored at 0°C to 10°C; Preferably, the internal standard solution is sealed and stored at 0°C to 4°C.

5. The method according to claim 1, characterized in that The detection conditions of the gas chromatography method also include: the column length of the chromatographic column is 10 to 60 m, the inner diameter is 0.1 to 0.5 mm, and the film thickness is 0.1 to 5 μm; the detector temperature is 150 to 300° C.; the injection port temperature is 150 to 230° C.; the septum purge flow rate is 1 to 20 mL / min, the tail gas flow rate is 10 to 50 mL / min; the injection volume is 0.1 to 2 μL; the injection method is split injection, and the split ratio is 10:1 to 40:1; Preferably, the column length of the chromatographic column is 10 to 50 m; Preferably, the column length of the chromatographic column is 10 to 40 m; Preferably, the column length of the chromatographic column is 10 to 30 m; Preferably, the inner diameter of the chromatographic column is 0.1 to 0.4 mm; Preferably, the inner diameter of the chromatographic column is 0.1 to 0.3 mm; Preferably, the inner diameter of the chromatographic column is 0.2-0.3 mm; Preferably, the membrane thickness of the chromatographic column is 0.1 to 4 μm; Preferably, the membrane thickness of the chromatographic column is 0.1 to 3 μm; Preferably, the film thickness of the chromatographic column is 0.1 to 1 μm; Preferably, the heating program is: initial temperature 30-60°C, maintained for 3-15 minutes, increased to 80-110°C at 3-15°C / min, increased to 150-300°C at 5-25°C / min, maintained for 3-20 minutes; Preferably, the heating program is: initial temperature 30-50°C, maintained for 3-10 minutes, increased to 80-100°C at 3-10°C / min, increased to 150-250°C at 5-20°C / min, maintained for 3-15 minutes; Preferably, the heating program is: initial temperature 30-40°C, maintained for 5-10 min, increased to 80-100°C at 5-10°C / min, increased to 200-200°C at 5-15°C / min, maintained for 5-15 min; Preferably, the detector temperature is 150-250°C; Preferably, the detector temperature is 180-250°C; Preferably, the detector temperature is 200-250°C; Preferably, the injection port temperature is 150-250°C; Preferably, the injection port temperature is 180-250°C; Preferably, the injection port temperature is 200-250°C; Preferably, the carrier gas is nitrogen with a purity of ≥99.999%; Preferably, the carrier gas flow rate is 0.5 to 2.5 mL / min; Preferably, the carrier gas flow rate is 0.5 to 2 mL / min; Preferably, the carrier gas flow rate is 0.5 to 1.5 mL / min; Preferably, the septum purge flow rate is 1 to 15 mL / min; Preferably, the septum purge flow rate is 1 to 10 mL / min; Preferably, the septum purge flow rate is 1 to 5 mL / min; Preferably, the tail gas sweep flow rate is 10 to 40 mL / min; Preferably, the tail gas sweep flow rate is 10 to 30 mL / min; Preferably, the tail gas sweep flow rate is 10 to 25 mL / min; Preferably, the injection volume is 0.1 to 1.5 μL; Preferably, the injection volume is 0.1 to 1 μL; Preferably, the injection volume is 0.5 to 1 μL; Preferably, the split ratio is 20:1 to 40:1; Preferably, the split ratio is 20:1 to 30:1; Preferably, the split ratio is 25:1 to 30:

1.

6. The method according to claim 5, characterized in that The detection conditions of the gas chromatography method are as follows: chromatographic column: Agilent DB-WAX UI chromatographic column, column length 30m, inner diameter 0.25mm, film thickness 0.25μm; the temperature program adopted by the chromatographic column is: initial temperature 40°C, maintained for 5min, increased to 100°C at 5.0°C / min, increased to 200°C at 10°C / min, maintained for 10min; detector temperature: 250°C; injection port temperature: 250°C; carrier gas type is nitrogen, purity is 99.999%; Carrier gas flow rate: 0.7 mL / min, constant flow; septum purge nitrogen flow rate: 3 mL / min, tail gas nitrogen flow rate: 25 mL / min; Injection volume: 0.5 μL; split ratio: 30:

1.

7. A method for evaluating liquor quality, characterized in that: The method described in any one of claims 1 to 6 is used to construct a fingerprint of liquor, and the quality of the liquor is judged based on the fingerprint.

8. Application of the method according to any one of claims 1 to 6 or the evaluation method according to claim 7 in evaluating the quality stability of liquor; Preferably, the liquor is a sauce-flavor liquor.

9. The use according to claim 8, characterized in that: The method of application includes: (a) constructing a control fingerprint of each round of liquor samples according to any one of the methods described in claims 1 to 6; (b) using gas chromatography to detect the liquor sample to be tested, and obtaining a spectrum of the sample to be tested; (c) using a fingerprint similarity evaluation system to analyze the fingerprint of the liquor sample to be tested and the reference fingerprint of the same round of the liquor sample to be tested, and calculate the similarity; Preferably, the liquor is a Maotai-flavor liquor; Preferably, the liquor is liquor from rounds 1 to 7; Preferably, the number of liquor samples used to construct the reference fingerprints of liquor samples in each round is not less than 30; Preferably, the fingerprint similarity evaluation system is a traditional Chinese medicine chromatographic fingerprint similarity evaluation system; Preferably, the Chinese medicine chromatographic fingerprint similarity evaluation system is a Chinese medicine chromatographic fingerprint similarity evaluation system (2012 version).

10. The use according to claim 9, characterized in that: The similarity is not less than 0.900, which indicates that the quality of the sample to be tested is stable; Preferably, the similarity is not less than 0.950, and the quality of the sample to be tested is determined to be stable; Preferably, the similarity is not less than 0.990, and the quality of the sample to be tested is determined to be stable.

Images