CN114113360B - Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid - Google Patents

Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid Download PDF

Info

Publication number
CN114113360B
CN114113360B CN202111127944.1A CN202111127944A CN114113360B CN 114113360 B CN114113360 B CN 114113360B CN 202111127944 A CN202111127944 A CN 202111127944A CN 114113360 B CN114113360 B CN 114113360B
Authority
CN
China
Prior art keywords
acid
wine
aftertaste
concentration
organic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111127944.1A
Other languages
Chinese (zh)
Other versions
CN114113360A (en
Inventor
胡光源
杨帆
王莉
李永素
陈宗校
杨婧
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kweichow Moutai Co Ltd
Original Assignee
Kweichow Moutai Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kweichow Moutai Co Ltd filed Critical Kweichow Moutai Co Ltd
Priority to CN202111127944.1A priority Critical patent/CN114113360B/en
Publication of CN114113360A publication Critical patent/CN114113360A/en
Application granted granted Critical
Publication of CN114113360B publication Critical patent/CN114113360B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025Gas chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/884Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/30Computing systems specially adapted for manufacturing

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention belongs to the field of food analysis, and relates to a method for distinguishing the aftertaste of Maotai-flavor liquor based on difficult-to-volatilize organic acids. The invention provides a method for distinguishing the aftertaste of white spirit, which is characterized in that the aftertaste of white spirit is distinguished according to the composition of organic acid, wherein the organic acid comprises tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid. The inventor researches the organic acids which are difficult to volatilize in the white spirit, explores the influence of the organic acids on the taste and the mouthfeel of the white spirit, and establishes a discrimination model based on the influence. The innovation point of the invention is to provide a method for rapidly, accurately and highly sensitively measuring the content of the organic acid difficult to volatilize in the Maotai-flavor liquor; the innovation point of the invention is that a soy sauce flavor type white spirit aftertaste discrimination model based on the content of the difficult volatile organic acid is established; the innovation point of the invention is that the quantity of the difficult-to-volatilize organic acids required by modeling is only five, and the invention has important significance for more comprehensively knowing the Maotai-flavor liquor and the quality control of the liquor.

Description

Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid
Technical Field
The invention belongs to the field of biological medicine, and relates to a method for distinguishing the aftertaste of Maotai-flavor liquor based on difficult-to-volatilize organic acid.
Background
The Maotai-flavor liquor is one of the important flavors of Chinese distilled liquor, and adopts the unique brewing process of 'three high and one long', namely high-temperature starter making, high-temperature fermentation, high Wen Liu liquor and long-term storage. The unique brewing process gives the wine a lot of fragrance substances. The high-quality Maotai-flavor liquor has unique style of prominent Maotai-flavor, elegant and fine flavor, mellow liquor body, long aftertaste and lasting fragrance of empty cups. In the past, the research on the flavor of white wine mainly comprises volatile flavor substances, and the research on the substances which are difficult to volatilize, especially the organic acids which are difficult to volatilize, is very difficult. The content of the difficultly volatile organic acid in the white spirit is low, and the substances have high boiling point, relatively large molecular groups and difficultly volatile property and are not easy to detect, and although the substances possibly do not show fragrance, the substances have influence on the taste and the mouthfeel of the white spirit or influence the volatilization of volatile components in the white spirit, and the interaction of the non-volatile substances and fragrance molecules can influence the release of the fragrance. Research shows that higher fatty acid and esters thereof are typical aroma and taste components, so that aroma substances are tightly combined in a system, the aftertaste characteristics of the wine body after entering the mouth are affected, and the aftertaste of the wine body is greatly affected.
At present, few studies on the difficultly volatile compounds in white spirit are reported in a small number of documents, but no document report is made on the basis of the difficultly volatile organic acids to distinguish the aftertaste of white spirit.
Disclosure of Invention
In some embodiments, the invention provides a method for distinguishing the aftertaste of white spirit, which is characterized in that the aftertaste of white spirit is distinguished according to the composition of organic acid, wherein the organic acid comprises tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid.
In some embodiments, the organic acid further comprises at least one of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid.
In some embodiments, the organic acid further comprises a combination of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid.
In some embodiments, the invention provides a method for distinguishing the aftertaste of white spirit, which comprises the following steps: obtaining the content of organic acid in a white spirit sample; inputting the content of the organic acid into a judging model to obtain a judging result of the grade of the aftertaste of the white wine; the judging model is a functional relation between the content of organic acid and the grade of the aftertaste of the white spirit; the organic acid includes tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid.
In some embodiments, the organic acid further comprises at least one of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid.
In some embodiments, the organic acid further comprises a combination of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid.
In some embodiments, the functional relationship is a linear model, where y=k×x+b, K is a functional coefficient, b is a constant, X is an organic acid concentration, and the score Y has a corresponding level of off-flavor of white spirit.
In some embodiments, when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid, the functional relationship comprises y1= -11.018 ×c1+121.191 × c2-0.481 ×c3-1.215×c4-1.786 ×c5-12.907; y2= -25.680 ×c1-7.347 ×c2+0.159×c3+61.705 ×c4+1.837 ×c5-13.576.
In some embodiments, for the alcohol aftertaste classes Y1 and Y2, comprising: when y1=4.831 to 9.595 and y2= 5.161 to 12.915, the wine-like type is three times of low-aftertaste wine; when y1=5.208-12.668 and y2= 3.670-7.955, the wine-like type is three times of long-aftertaste wine; when Y1= -14.462 to-8.972 and Y2= -0.095-4.963, the wine sample type is four times of wine with short aftertaste; when y1= -14.618 to-12.725 and y2= 0.621-2.742, the wine sample type is four times of long-aftertaste wine; when y1=2.501-4.740 and y2= -9.058 to-6.941, the wine sample type is five rounds of wine with short aftertaste; when y1=4.100-4.933 and y2= -9.457 to-7.717, the wine sample type is five rounds of wine with long aftertaste.
In some embodiments, when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid, the functional relationship comprises: y1= -29.099 ×c1+108.74 ×c2-0.554×c3+6.945 ×c4+1.248×c5+0.548×c6+4.114 ×c7-0.454×c8-1.769 ×c9+0.715×c10-2.569 ×c11-1.836×c12-1.13×c13-1.43×c14-14.672, y2= -13.499 ×c1-56.82×c2-0.151×c3+18.102 ×c4+0.991×c5+3.663 ×c6+7.12×c7+1.582×c8-2.398×c9+0.203×c10+0.911×c11-3.713 ×c12+0.665×c13-3.662 ×c14-0.7.
In some embodiments, for the alcohol aftertaste classes Y1 and Y2, comprising: when y1= 13.007-18.384 and y2=1.487-6.067, the wine-like type is three times of short-aftertaste wine; when y1=9.100-15.389 and y2= -1.803-2.460, the wine sample type is three times of long-aftertaste wine; when y1= -12.195 to-7.701 and y2= 8.102 to 12.339, the wine sample type is four times of wine with short aftertaste; when y1= -10.755 to-9.363 and y2= 9.907 to 12.994, the wine sample type is four times of long-aftertaste wine; when Y1 = -7.211 = -4.645 and Y2 = -12.943 = -9.108, the wine sample type is five times of wine with short aftertaste; when Y1 = -5.812-3.788 and Y2 = -13.400-10.773, the wine sample type is five times of long-aftertaste wine.
In some embodiments, the present invention provides a device for discriminating after taste of white spirit, the device comprising: the data acquisition module is used for acquiring the content of the organic acid in the white spirit sample; the judging module is used for inputting the content of the organic acid into a judging model to obtain a white wine aftertaste judging result; the judging model is a functional relation between the content of organic acid and the grade of the aftertaste of the white spirit; the organic acid includes tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid.
In some embodiments, the organic acid further comprises at least one of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid.
In some embodiments, the organic acid further comprises a combination of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid.
In some embodiments, the functional relationship is a linear model, where y=k×x+b, K is a functional coefficient, b is a constant, X is an organic acid concentration, and the score Y has a corresponding level of off-flavor of white spirit.
In some embodiments, when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid, the functional relationship comprises y1= -11.018 ×c1+121.191 × c2-0.481 ×c3-1.215×c4-1.786 ×c5-12.907; y2= -25.680 ×c1-7.347 ×c2+0.159×c3+61.705 ×c4+1.837 ×c5-13.576.
In some embodiments, for the alcohol aftertaste classes Y1 and Y2, comprising: when y1=4.831 to 9.595 and y2= 5.161 to 12.915, the wine-like type is three times of low-aftertaste wine; when y1=5.208-12.668 and y2= 3.670-7.955, the wine-like type is three times of long-aftertaste wine; when Y1= -14.462 to-8.972 and Y2= -0.095-4.963, the wine sample type is four times of wine with short aftertaste; when y1= -14.618 to-12.725 and y2= 0.621-2.742, the wine sample type is four times of long-aftertaste wine; when y1=2.501-4.740 and y2= -9.058 to-6.941, the wine sample type is five rounds of wine with short aftertaste; when y1=4.100-4.933 and y2= -9.457 to-7.717, the wine sample type is five rounds of wine with long aftertaste.
In some embodiments, when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid, the functional relationship comprises: y1= -29.099 ×c1+108.74 ×c2-0.554×c3+6.945 ×c4+1.248×c5+0.548×c6+4.114 ×c7-0.454×c8-1.769 ×c9+0.715×c10-2.569 ×c11-1.836×c12-1.13×c13-1.43×c14-14.672, y2= -13.499 ×c1-56.82×c2-0.151×c3+18.102 ×c4+0.991×c5+3.663 ×c6+7.12×c7+1.582×c8-2.398×c9+0.203×c10+0.911×c11-3.713 ×c12+0.665×c13-3.662 ×c14-0.7.
In some embodiments, for the alcohol aftertaste classes Y1 and Y2, comprising: when y1= 13.007-18.384 and y2=1.487-6.067, the wine-like type is three times of short-aftertaste wine; when y1=9.100-15.389 and y2= -1.803-2.460, the wine sample type is three times of long-aftertaste wine; when y1= -12.195 to-7.701 and y2= 8.102 to 12.339, the wine sample type is four times of wine with short aftertaste; when y1= -10.755 to-9.363 and y2= 9.907 to 12.994, the wine sample type is four times of long-aftertaste wine; when Y1 = -7.211 = -4.645 and Y2 = -12.943 = -9.108, the wine sample type is five times of wine with short aftertaste; when Y1 = -5.812-3.788 and Y2 = -13.400-10.773, the wine sample type is five times of long-aftertaste wine.
In some embodiments, the organic acid content is determined using a gas chromatography mass spectrometry method.
In some embodiments, the step of determining the organic acid content comprises: (1) concentrating the wine sample; (2) constant volume and saturation of the concentrated sample; (3) Carrying out liquid-liquid microextraction on the solution in the step (2) by using an organic solvent, and extracting an organic phase to be detected; (4) The organic phase obtained in the step (3) is measured by a gas chromatography-mass spectrometry method.
In some embodiments, the step (1) comprises taking the white spirit and performing vacuum concentration in a vacuum concentration rotary evaporator.
In some embodiments, the vacuum concentration conditions described in step (1) are from 35 to 50 ℃.
In some embodiments, the volume ratio of the original white spirit in the step (1) to the concentrated sample in the step (2) after the volume is fixed is 2-4:1.
In some embodiments, the organic solvent described in step (3) comprises n-hexane, diethyl ether, ethyl acetate, or dichloromethane.
In some embodiments, the organic solvent in step (3) is diethyl ether.
In some embodiments, the ratio of the volume of the diethyl ether to the volume of the sample after the volume is fixed in step (2) is 1 to 3:2 to 5.
In some embodiments, the chromatographic conditions of the gas chromatography mass spectrometry include: a capillary gas chromatographic column is adopted, and the specification of the capillary gas chromatographic column is DB-WAX UI (30 m multiplied by 0.25mm multiplied by 0.25 mu m); setting the ionization mode as EI, setting the temperature of an ion source at 230 ℃ and setting the temperature of a transmission line at 250 ℃; helium is used as carrier gas, and the flow rate is 1.2mL/min; the gas chromatography temperature program was set to an initial temperature of 40℃and was raised to 230℃at a rate of 6℃per minute and maintained for 14 minutes.
In some embodiments, the mass spectrometry conditions of the gas chromatography mass spectrometry comprise: the mass spectrum scanning adopts an ion scanning mode and a full scanning mode, and the scanning range is 35-350 amu.
In some embodiments, constructing a correspondence between the organic acid content and the off-flavor level of the white spirit includes obtaining a standard curve and a correction factor of the organic acid by an external standard method and an internal standard method, and calculating the content of the organic acid in the white spirit sample according to the standard curve and the correction factor of the organic acid; and then according to the organic acid content and the grade of the aftertaste of the white spirit obtained by the sensory evaluation, establishing a corresponding relation between the organic acid content and the grade of the aftertaste of the white spirit, thereby obtaining a distinguishing model of the aftertaste of the white spirit.
The method provided by the invention has the advantages of rapidness, accuracy and higher sensitivity in determining the content of the difficult-to-volatilize organic acid in the Maotai-flavor liquor, and can be used as a method for determining the content of the difficult-to-volatilize organic acid in the Maotai-flavor liquor. In addition, by analyzing the difference of the content of the hard volatile organic acids in the aftertaste liquor samples with different lengths, the Maotai-flavor liquor with different aftertaste lengths is found to have a certain difference in the content of the hard volatile organic acids. Thereby establishing a method for distinguishing the aftertaste of the wine body based on the difference of the content of the difficult volatile organic acids.
In some embodiments, the white spirit is a Maotai-flavor white spirit.
In some embodiments, the white spirit is any one of a round to a seven round of base spirit.
In some embodiments, the invention provides the use of the method in determining the aftertaste of white wine.
In some embodiments, the invention provides the use of the method in determining the aftertaste of white wine.
In some embodiments, the inventor researches the organic acids which are difficult to volatilize in the white spirit, explores the influence of the organic acids on the taste and the mouthfeel of the white spirit, and based on the organic acids, establishes a discrimination model, and has great significance for more comprehensively knowing the Maotai-flavor white spirit and the quality control of the white spirit.
Drawings
FIG. 1 is a box-type diagram of the content of difficultly volatile organic acids in the aftertaste Maotai-flavor liquor samples of different types of liquor bodies.
Fig. 2 is a pattern of identification of Maotai-flavor liquor of different rounds and different classes based on 14 hard volatile organic acid contents.
FIG. 3 is a graph of identification models of Maotai-flavor liquor of different rounds and different classes based on 5 hard volatile organic acid contents.
FIG. 4 shows the results of analysis and detection of 14 hard-to-volatile organic acids in three rounds of wine samples by different pretreatment methods.
FIG. 5 is a graph showing the extraction effect of different concentration volumes on 14 difficultly volatile organic acids in three rounds of wine samples.
FIG. 6 is a graph showing the effect of using different solvents on extraction of 14 poorly volatile organic acids from three rounds of wine samples.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples, which do not represent limitations on the scope of the present invention. Some insubstantial modifications and adaptations of the invention based on the inventive concept by others remain within the scope of the invention.
As used herein, the term "aftertaste" in the term "aftertaste" refers to the long-lasting sensation of the flavor component in the oral cavity after the white spirit has no longer contacted the nerve ending taste organ, such as a mellow aftertaste, etc.
In the following examples herein, 3 as in 3A represents a third round of Maotai-flavor liquor samples; 4 in 4A represents the Maotai-flavor liquor sample of the fourth round; "5" in 5A indicates the Maotai-flavor liquor sample of the fifth round. The other groups and so on.
In the examples herein below, a represents a short aftertaste wine-like; b represents a long aftertaste wine-like.
In the examples herein below, the gas chromatography mass spectrometry test conditions were that a capillary gas chromatography column was used, which had a specification of DB-WAX UI (30 m. Times.0.25 mm. Times.0.25 μm); setting the ionization mode as EI, setting the temperature of an ion source at 230 ℃ and setting the temperature of a transmission line at 250 ℃; helium is used as carrier gas, and the flow rate is 1.2mL/min; the temperature of the gas chromatography is raised to be 40 ℃ at the initial temperature, and the temperature is raised to be 230 ℃ at the speed of 6 ℃/min and kept for 14min; the mass spectrum scanning adopts an ion scanning mode and a full scanning mode, and the scanning range is 35-350 amu.
Qualitative properties of the poorly volatile organic acid compounds herein: retention time, standards, parent and secondary fragment ions were used for characterization.
In the examples herein below, the 14 organic acids are tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid; wherein C1-C14 are respectively corresponding to tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid and linolenic acid.
Main reagents and materials:
sample: the round base wine is provided by Maotai wine, inc., guizhou.
Standard substance: oleic acid (purity not less than 99%), linoleic acid (purity not less than 99%), lactic acid (purity not less than 98%), pentadecanoic acid (purity not less than 99%), benzoic acid (purity not less than 99.5%), phenylacetic acid (purity not less than 99%), 3-phenylpropionic acid (purity not less than 99%), palmitoleic acid (purity not less than 98.5%), linolenic acid (purity not less than 99%) Sigma company in America; tetradecanoic acid (purity not less than 98%) Shanghai chemical reagent company of Shanghai medical group; heptadecanoic acid (purity not less than 99%), octadecanoic acid (purity not less than 99%) jingbailing science and technology limited company;
reagent: ethyl acetate (chromatographic purity), diethyl ether (analytical purity), methylene chloride (chromatographic purity), n-hexane (chromatographic purity), pentane (chromatographic purity), propyl acetate (analytical purity), sodium chloride (analytical purity) national pharmaceutical chemicals limited.
The main instrument is as follows:
concentrating Eppendorf by vacuum centrifugation; 7890B/5977B GC-MS combined instrument, HP-5 capillary chromatographic column DB-WAX UI (30 m 0.25mm 0.25 μm) Agilent company, america; MS1602TS electronic balance, mestrehler, switzerland.
In the examples herein below, the gas chromatography mass spectrometry test conditions were that a capillary gas chromatography column was used, which had a specification of DB-WAX UI (30 m. Times.0.25 mm. Times.0.25 μm); setting the ionization mode as EI, setting the temperature of an ion source at 230 ℃ and setting the temperature of a transmission line at 250 ℃; helium is used as carrier gas, and the flow rate is 1.2mL/min; the temperature of the gas chromatography is raised to be 40 ℃ at the initial temperature, and the temperature is raised to be 230 ℃ at the speed of 6 ℃/min and kept for 14min; the mass spectrum scanning adopts an ion scanning mode and a full scanning mode, and the scanning range is 35-350 amu.
Example 1 method for discriminating after-taste of Maotai-flavor liquor based on poorly volatile organic acids
1. Quantification of poorly volatile organic acids
1.1 external Standard method for quantifying organic acids difficult to volatile
And respectively measuring a certain amount of standard substances of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid, adding 99.9% ethanol to prepare standard substance mother liquor solution, so that the concentration of the tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid is 13469.00ppm, 9292.00ppm, 18983.00ppm, 11386.00ppm and 11940.00ppm respectively, then preparing a difficult-to-volatilize organic acid sample with a certain concentration gradient by using analytically pure diethyl ether as a solvent, and measuring by using a gas chromatography mass spectrometry method. And drawing a standard curve by taking the peak area of each standard substance as an ordinate and the concentration of the standard substance as an abscissa. The limit of detection (LOD) of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid under experimental conditions was calculated with a signal to noise ratio equal to 3, and the results are given in table 1 below.
TABLE 1 Standard Curve parameter information Table
Figure BDA0003279319680000061
Figure BDA0003279319680000071
1.2 internal standard method for quantifying organic acids difficult to volatile
The content of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid and linolenic acid in the Maotai-flavor liquor is determined by adopting an internal standard method, and the method comprises the following steps:
concentrating 5mL of Maotai-flavor liquor-like solution at 45 ℃ for 2 hours to a certain amount by using a vacuum concentration rotary evaporator, and fixing the volume by using ultrapure water until the volume ratio of the original sample solution to the concentrated sample is 2.5:1, namely, the volumes after the volume fixing are respectively 2mL, and adding sodium chloride to be saturated; 3 mu L of 3, 4-dimethylphenol which is an internal standard compound with the concentration of 1407.3ppm is added into the solution after the volume fixing and salting-out, then 1.0mL of analytically pure diethyl ether is added for liquid-liquid microextraction, an upper organic phase is collected, and the detection is carried out by using a gas chromatography-mass spectrometry method. Based on the instrument detection results, a correction factor f is calculated,
Figure BDA0003279319680000072
wherein A is s And A r Peak area or peak height, m of the internal standard substance and the reference substance respectively s And m r The amounts of the internal standard and the reference substance are added respectively. Taking the solution of the component to be detected containing the internal standard substance, sampling, recording the chromatogram, and calculating the content (m i ):
Figure BDA0003279319680000073
Wherein A is i And A s Peak areas or peak heights of the object to be detected and the internal standard object, m s In the amount of the added internal standard.
The content of the organic acid which is difficult to volatilize in the Maotai-flavor liquor is m i =A i ×3×10 -3 mL×1407.3ppm/(2mL×A s X 2.5), according to the peak area of each difficultly volatile organic acid of the chromatogram and the correction factor, the content of octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid and linolenic acid in the Maotai-flavor liquor can be calculated respectively. Wherein ppm is mg/L.
2. Recovery measurement
The standard substances of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid are selected, and mixed standard substances with certain concentration are prepared in 53% (V/V) ethanol water solution, so that the concentration of the tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid is 897.93ppm, 619.47ppm, 8858.73ppm, 759.07ppm and 3980.00ppm respectively, and the mixed standard substance solution of the organic acid difficult to volatilize is obtained. Concentrating, extracting and measuring the mixed standard sample solution according to an organic acid content analysis method in the wine sample, analyzing the loss condition of a target object in the process of concentrating and removing ethanol by vacuum centrifugation at 45 ℃, and exploring the blank standard adding recovery rate of the research method.
The method for analyzing the organic acid content of the mixed standard sample comprises the following steps:
concentrating 5mL of the solution at 45 ℃ for 2 hours to a certain amount by using a vacuum concentration rotary evaporator, fixing the volume by using ultrapure water, fixing the volume until the volume ratio of the original mixed standard sample solution to the concentrated sample is 2.5:1, namely, fixing the volume after the volume is 2mL respectively, and adding sodium chloride to be saturated; and respectively adding 1.0mL of analytically pure diethyl ether into the solution after constant volume and salting-out, performing liquid-liquid microextraction, collecting an upper organic phase, and detecting by using a gas chromatography-mass spectrometry method.
As shown in Table 2, the blank standard recovery rate of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid is 83% -101%, which shows that the higher fatty acid has no loss or small loss in the concentration process, and the standard working solution can omit the step of primary concentration when the standard curve is produced in actual work, and is directly prepared into the saturated saline solution for extraction.
TABLE 2 blank mark recovery
Figure BDA0003279319680000081
The results in Table 2 show that the method is accurate and reliable, and can be used for determining the requirements of the difficultly volatile organic acid substances in the Maotai-flavor liquor.
Table 1 shows that the established standard curves all have a good linear relationship (R 2 More than 0.99), can be applied to the quantification of corresponding substances in Maotai-flavor liquor.
Example 2 method for discriminating after-taste of Maotai-flavor liquor based on fourteen difficultly volatile organic acids
1. Construction of white wine aftertaste discrimination model
The method is adopted to analyze and test 149 liquor samples of a certain plant in three, four and five rounds, firstly, the sensory evaluation group scores the aftertaste length of the liquor samples, and the samples are classified into two grades of A class (short aftertaste) and B class (long aftertaste) according to the scoring result.
And then further detecting and analyzing 113 Maotai-flavor liquor samples, respectively taking 5mL of liquor samples, concentrating in a vacuum concentration rotary evaporator at 45 ℃ for 2 hours, adopting ultrapure water to fix the volume to 2mL, adding 1.8g of sodium chloride to saturation, adding 1.0mL of diethyl ether for liquid-liquid micro extraction, and sucking an upper organic phase to be detected, wherein the testing method is a gas chromatography-mass spectrometry combination method.
The quantitative analysis substances are tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, and linolenic acid. 14 poorly volatile organic acid compounds, designated as: c1 to C14.
And according to the measuring result of the instrument, the concentration of the corresponding organic acid in the wine sample is calculated by combining an external standard method and an internal standard method.
Taking the detection result of each difficultly volatile organic acid in three rounds of base wine samples as an example, as shown in fig. 1, the analysis result shows that the content of the difficultly volatile organic acid compound in the class A samples is obviously higher than that in the class B samples in the rounds.
Analytical modeling was performed based on 14 hard-to-volatilize organic acid species content: and according to the measuring result of the instrument, the concentration of the corresponding organic acid in the wine sample is calculated by combining an external standard method and an internal standard method. And then according to the concentration of the organic acid and the grade of the aftertaste of the white spirit obtained by the sensory evaluation, establishing a corresponding relation between the content of the organic acid and the grade of the aftertaste of the white spirit, thereby obtaining a judgment model of the aftertaste of the white spirit, wherein the judgment function is as follows:
F1=-29.099×C1+108.74×C2-0.554×C3+6.945×C4+1.248×C5+0.548×C6+4.114×C7-0.454×C8-1.769×C9+0.715×C10-2.569×C11-1.836×C12-1.13×C13-1.43×C14-14.672
F2=-13.499×C1-56.82×C2-0.151×C3+18.102×C4+0.991×C5+3.663×C6+7.12×C7+1.582×C8-2.398×C9+0.203×C10+0.911×C11-3.713×C12+0.665×C13-3.662×C14-0.7
note that: c1 to C14 refer to the content of the corresponding organic acid which is difficult to volatilize respectively.
The wine sample type is 3A when the calculation result f1= 13.007-18.384 and f2=1.487-6.067;
when the calculated result f1=9.100-15.389, f2= -1.803-2.460, the wine sample type is 3B;
when the calculated result F1= -12.195-7.701 and F2= 8.102-12.339, the wine sample type is 4A;
when the calculated result f1= -10.755 to-9.363 and f2= 9.907 to 12.994, the wine sample type is 4B;
when the calculation result F1= -7.211 to-4.645 and F2= -12.943 to-9.108, the wine sample type is 5A;
when the calculated result F1= -5.812 to-3.788 and F2= -13.400 to-10.773, the wine sample type is 5B.
As a result, as shown in FIG. 2, the content of the hard volatile organic acid in 113 liquor samples with different rounds and different liquor aftertastes is subjected to discriminant analysis, in the model, the base liquor with different rounds can be well distinguished, the distribution of the base liquor with different liquor aftertastes in the same round also shows a certain regularity, and the A class and the B class of the Maotai-flavor liquor samples with different content of the hard volatile organic acid liquor can be well separated.
2. Verification of discriminant model
The result of discriminant analysis of the data of the content of the difficult volatile organic acids of 113 wine samples shows that the cross-validation accuracy of 113 training samples in all three rounds is about 90% (the result is shown in table 3). In conclusion, the distribution difference of the content of the difficultly volatile organic acid substances in the sample can cause the Maotai-flavor liquor to present different aftertaste length characteristics.
TABLE 3 training sample Cross-validation results
from\to 3A 3B 4A 4B 5A 5B Total %correct
3A 21 0 0 0 0 0 21 100.00
3B
0 19 0 0 0 0 19 100.00
4A
0 0 13 2 0 0 15 86.67
4B
0 0 1 17 0 0 18 94.44
5A
0 0 0 0 19 1 20 95.00
5B
0 0 0 0 0 20 20 100.00%
Total 21 19 14 19 19 21 113 96.46%
Example 3 use of body after taste discrimination model for discriminating after taste intensity in Maotai-flavor liquor
Predicting 36 externally tested Maotai-flavor liquor samples by using the liquor aftertaste discrimination model established in the embodiment 2, wherein the accuracy of the discrimination model on aftertaste short samples is 83.3% in three rounds of 12 (6A-class and 6B-class), four rounds of 12 (6A-class and 6B-class) and five rounds of 12 (6A-class and 6B-class); the accuracy of the aftertaste long sample is 94.4%; the comprehensive judgment accuracy of 36 prediction samples is 88.9%, and the result further shows that the built model has a good effect of identifying the aftertaste intensity of the Maotai-flavor liquor (the result is shown in Table 4).
TABLE 4 discriminant analysis of 36 external validation set samples based on a discriminant model of the example of the present application
Figure BDA0003279319680000101
Note that: a represents a sample with short aftertaste; b: samples representing long aftertaste
Example 4 method for discriminating after-taste of Maotai-flavor liquor based on five difficultly volatile organic acids
1. Construction of white wine aftertaste discrimination model
The method of example 2 was used to analyze 149 liquor samples from three, four and five rounds of Maotai-flavor liquor from a certain factory, the length of aftertaste of the liquor samples was first scored by a sensory panel, and the samples were collected and classified into two classes, class a (short aftertaste) and class B (long aftertaste) according to the scoring result.
And then further detecting and analyzing 113 Maotai-flavor liquor samples, respectively taking 5mL of liquor samples, concentrating in a vacuum concentration rotary evaporator at 45 ℃ for 2 hours, adopting ultrapure water to fix the volume to 2mL, adding 1.8g of sodium chloride to saturation, adding 1.0mL of diethyl ether for liquid-liquid micro extraction, and sucking an upper organic phase to be detected, wherein the testing method is a gas chromatography-mass spectrometry combination method.
The quantitative analysis substance is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid. 5 poorly volatile organic acid compounds, respectively designated: C1-C5.
And according to the measurement result of the instrument, combining the corresponding standard curve to obtain the concentration of the corresponding organic acid in the wine sample.
Taking the detection result of each difficultly volatile organic acid in three rounds of wine samples as an example, the content of tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid in the three rounds of wine samples is consistent with that of embodiment 2, and the analysis result shows that the content of the difficultly volatile organic acid compounds in the A-class samples is obviously higher than that of the B-class samples in the rounds.
Analytical modeling was performed based on 5 hard-to-volatilize organic acid species content: and according to the measurement result of the instrument, combining the corresponding standard curve to obtain the concentration of the corresponding organic acid in the wine sample. And then according to the concentration of the organic acid and the grade of the aftertaste of the white spirit obtained by the sensory evaluation, establishing a corresponding relation between the content of the organic acid and the grade of the aftertaste of the white spirit, thereby obtaining a judgment model of the aftertaste of the white spirit, wherein the judgment function is as follows:
F1=-11.018xC1+121.191XC2-0.481xC3-1.215xC4-1.786xC5-12.907
F2=-25.680xC1-7.347xC2+0.159xC3+61.705xC4+1.837xC5-13.576
note that: c1 to C5 refer to the content of the corresponding organic acid difficult to volatilize respectively
When the calculated result f1=4.831-9.595 and f2= 5.161-12.915, the wine sample type is 3A;
when the calculated result f1=5.208-12.668 and f2= 3.670-7.955, the wine sample type is 3B;
when the calculated result F1= -14.462 to-8.972 and F2= -0.095 to 4.963, the wine sample type is 4A;
when the calculated result F1= -14.618 to-12.725 and F2= 0.621-2.742, the wine sample type is 4B;
when the calculated result F1=2.501-4.740, F2= -9.058 to-6.941, the wine sample type is 5A;
when the calculated result f1=4.100-4.933 and f2= -9.457 to-7.717, the wine sample type is 5B.
As a result, as shown in FIG. 3, the content of the hard volatile organic acids in 113 liquor samples with different rounds and different liquor aftertastes is subjected to discriminant analysis, in the model, the base liquor with different rounds can be well distinguished, the distribution of the base liquor with different liquor aftertastes in the same round also shows a certain regularity, and the A class and the B class of the Maotai-flavor liquor samples with different content of the hard volatile organic acids can be well separated.
2. Verification of discriminant model
The result of discriminant analysis of the data of the content of the difficult volatile organic acids of 113 wine samples shows that the cross-validation accuracy of 113 training samples in all three rounds is about 95% (the result is shown in table 5). In conclusion, the distribution difference of the content of the difficultly volatile organic acid substances in the sample can cause the Maotai-flavor liquor to present different aftertaste length characteristics.
Table 5 training sample cross-validation results
from\to 3A 3B 4A 4B 5A 5B Total correct
3A
20 1 0 0 0 0 21 95.24
3B
0 19 0 0 0 0 19 100.00
4A
0 0 13 2 0 0 15 86.67
4B
0 0 1 17 0 0 18 94.44
5A
0 0 0 0 18 2 20 90.00
5B
0 0 0 0 0 20 20 100.00
Total
20 20 14 19 18 22 113 94.69%
Example 5 use of body after taste discrimination model for discriminating after taste intensity in Maotai-flavor liquor
Predicting 36 externally tested Maotai-flavor liquor samples by using the liquor aftertaste discrimination model established in the embodiment 4, wherein 12 samples are detected by three times (6A and 6B), 12 samples are detected by four times (6A and 6B) and 12 samples are detected by five times (6A and 6B), and the accuracy of the discrimination model in judging the aftertaste short samples is 83.3 percent; the accuracy rate of the aftertaste long sample is 100%; the comprehensive judgment accuracy of 36 prediction samples is 91.7%, and the result further shows that the built model has a good effect of identifying the aftertaste intensity of the Maotai-flavor liquor (the result is shown in Table 6).
TABLE 6 discriminant analysis of 36 external validation set samples based on a discriminant model of the example of the present application
Figure BDA0003279319680000121
Note that: a represents a sample with short aftertaste; b: samples representing long aftertaste
Example 6 pretreatment method optimization:
when the initial volume of the wine sample is 5mL and the extraction solvent is diethyl ether, the effect of different pretreatment methods on the extraction of the wine sample is compared. The rest of the procedure is the same as in example 1.
The results are shown in FIG. 4: the peak area of the extraction target substance after the vacuum concentration pretreatment is higher than that of the peak area of the direct extraction sample injection test analysis without concentration, and the response of the measured substance after the vacuum concentration pretreatment reaches the quantitative limit of the method. Therefore, the wine-like concentration treatment can have the effect of enriching the difficultly volatile organic acid substances in the wine body, and can improve the response and the signal-to-noise ratio of the target compound.
Example 7 concentrated volume optimization
Taking three parts of wine samples, wherein the volumes are respectively 10mL, 5mL and 2mL, concentrating for 2 hours to a certain amount by using a rotary evaporator at 45 ℃, and fixing the volume by using ultrapure water until the volume ratio of the volume of the wine samples to the volume of the concentrated samples is 2.5:1, namely, the volumes after fixing the volume are respectively 4mL, 2mL and 0.8mL, and adding sodium chloride to be saturated; and respectively adding 1.0mL of analytically pure diethyl ether into the solution after constant volume and salting-out, performing liquid-liquid microextraction, collecting an upper organic phase, and measuring by using the total peak area of the 14 detected difficult-to-volatilize organic acid compounds as a measurement index and using a gas chromatography-mass spectrometry method. As a result, as shown in FIG. 5, when the concentration volume was selected to be 2mL, the heptadecanoic acid response of the sample at a lower level was lower than the quantitative limit of the established method, and therefore, based on the linear range and economy of the method, the concentration volume was selected to be 5mL as the initial amount.
Example 8 optimization of extraction solvent
Taking six parts of Maotai-flavor liquor samples, wherein each part has a volume of 5mL, concentrating for 2 hours to a certain amount by a rotary evaporator at 45 ℃, and fixing the volume by ultrapure water until the volume ratio of the liquor sample volume to the concentrated sample volume is 2.5:1, namely the volume after fixing the volume is 2mL, and adding sodium chloride to be saturated; and respectively adding pentane, ethyl acetate, normal hexane, propyl acetate, methylene dichloride and diethyl ether with the volume of 1mL into 6 parts of solution after constant volume and salting-out, carrying out liquid-liquid microextraction, collecting an upper organic phase, and measuring the total peak area of 14 organic acids (tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, linoleic acid, linolenic acid, palmitoleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid and 3-phenylpropionic acid) as a measurement index by using a gas chromatography mass spectrometry method.
The results are shown in FIG. 6. Since the signal of the target substance is highest when diethyl ether is used for extraction, diethyl ether is selected as the extraction solvent.

Claims (23)

1. The method for distinguishing the aftertaste of the Maotai-flavor white spirit is characterized by distinguishing the aftertaste of the white spirit according to the composition of organic acids, wherein the organic acids comprise tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid;
the aftertaste of the white spirit is judged by the functional relation between the content of the organic acid and the aftertaste grade of the white spirit; the functional relation is a linear model, Y=K×X+b, K is a functional coefficient, b is a constant, X is the concentration of organic acid, and the score Y has a corresponding grade of the aftertaste of white spirit; when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid, the functional relationship includes
Y1=-11.018×C1+121.191×C2-0.481×C3-1.215×C4-1.786×C5-12.907;
Y2=-25.680×C1-7.347×C2+0.159×C3+61.705×C4+1.837×C5-13.576;
The white spirit is any round of base spirit from one round to five rounds;
the concentration of C1 is tetradecanoic acid, the concentration of C2 is pentadecanoic acid, the concentration of C3 is hexadecanoic acid, the concentration of C4 is heptadecanoic acid, and the concentration of C5 is oleic acid.
2. The method of claim 1, wherein the organic acid further comprises octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, or linolenic acid.
3. The method for distinguishing the aftertaste of the Maotai-flavor liquor is characterized by comprising the following steps of:
obtaining the content of organic acid in a white spirit sample; inputting the content of the organic acid into a judging model to obtain a judging result of the grade of the aftertaste of the white wine; the judging model is a functional relation between the content of organic acid and the grade of the aftertaste of the white spirit; the organic acid comprises tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid; the functional relation is a linear model, Y=K×X+b, K is a functional coefficient, b is a constant, X is the concentration of organic acid, and the score Y has a corresponding grade of the aftertaste of white spirit; when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid, the functional relationship includes
Y1=-11.018×C1+121.191×C2-0.481×C3-1.215×C4-1.786×C5-12.907;
Y2=-25.680×C1-7.347×C2+0.159×C3+61.705×C4+1.837×C5-13.576;
The white spirit is any round of base spirit from one round to five rounds;
the concentration of C1 is tetradecanoic acid, the concentration of C2 is pentadecanoic acid, the concentration of C3 is hexadecanoic acid, the concentration of C4 is heptadecanoic acid, and the concentration of C5 is oleic acid.
4. The method of claim 3, wherein the organic acid further comprises octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, or linolenic acid.
5. A method of discriminating as defined in claim 1 or 3, wherein for the after-taste classes Y1 and Y2, comprising:
when y1=4.831 to 9.595 and y2= 5.161 to 12.915, the wine-like type is three times of low-aftertaste wine;
when y1=5.208-12.668 and y2= 3.670-7.955, the wine-like type is three times of long-aftertaste wine;
when Y1= -14.462 to-8.972 and Y2= -0.095-4.963, the wine sample type is four times of wine with short aftertaste;
when y1= -14.618 to-12.725 and y2= 0.621-2.742, the wine sample type is four times of long-aftertaste wine;
when y1=2.501-4.740 and y2= -9.058 to-6.941, the wine sample type is five rounds of wine with short aftertaste; when y1=4.100-4.933 and y2= -9.457 to-7.717, the wine sample type is five rounds of wine with long aftertaste.
6. The method of claim 1 or 3, wherein when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid, the functional relationship comprises:
Y1=-29.099×C1+108.74×C2-0.554×C3+6.945×C4+1.248×C5+0.548×C6+4.114×C7-0.454×C8-1.769×C9+0.715×C10-2.569×C11-1.836×C12-1.13×C13-1.43×C14-14.672,
Y2=-13.499×C1-56.82×C2-0.151×C3+18.102×C4+0.991×C5+3.663×C6+7.12×C7+
1.582×C8-2.398×C9+0.203×C10+0.911×C11-3.713×C12+0.665×C13-3.662×C14-0.7;
the C1 is the concentration of tetradecanoic acid, the C2 is the concentration of pentadecanoic acid, the C3 is the concentration of hexadecanoic acid, the C4 is the concentration of heptadecanoic acid, the C5 is the concentration of oleic acid, the C6 is the concentration of octadecanoic acid, the C7 is the concentration of L-lactic acid, the C8 is the concentration of benzoic acid, the C9 is the concentration of 2-furancarboxylic acid, the C10 is the concentration of benzoic acid, the C11 is the concentration of 3-phenylpropionic acid, the C12 is the concentration of palmic acid, the C13 is the concentration of linolic acid, and the C14 is the concentration of linolenic acid.
7. A method of discriminating as defined in claim 1 or 3, wherein for the after-taste classes Y1 and Y2, comprising:
when y1= 13.007-18.384 and y2=1.487-6.067, the wine-like type is three times of short-aftertaste wine;
when y1=9.100-15.389 and y2= -1.803-2.460, the wine sample type is three times of long-aftertaste wine;
when y1= -12.195 to-7.701 and y2= 8.102 to 12.339, the wine sample type is four times of wine with short aftertaste;
when y1= -10.755 to-9.363 and y2= 9.907 to 12.994, the wine sample type is four times of long-aftertaste wine;
when Y1 = -7.211 = -4.645 and Y2 = -12.943 = -9.108, the wine sample type is five times of wine with short aftertaste;
when Y1 = -5.812-3.788 and Y2 = -13.400-10.773, the wine sample type is five times of long-aftertaste wine.
8. The method of any one of claims 1-4, wherein the organic acid content is determined using a gas chromatography mass spectrometry method.
9. The method of claim 8, wherein the step of determining the organic acid content comprises:
(1) Concentrating the wine sample;
(2) Concentrating the constant volume and saturation of the sample;
(3) Carrying out liquid-liquid microextraction on the solution in the step (2) by using an organic solvent, and extracting an organic phase to be detected;
(4) The organic phase obtained in the step (3) is measured by a gas chromatography-mass spectrometry method.
10. The method of claim 9, wherein step (1) comprises taking the white spirit and vacuum concentrating the white spirit in a vacuum concentrating rotary evaporator.
11. The method of claim 10, wherein the vacuum concentration conditions in step (1) are 35 to 50 ℃.
12. The method of claim 10, wherein the ratio of the volume of the original white spirit in step (1) to the volume of the concentrated sample after the constant volume in step (2) is 2-4:1.
13. The method of claim 9, wherein the organic solvent in step (3) comprises n-hexane, diethyl ether, ethyl acetate, or dichloromethane.
14. The method of claim 9, wherein the organic solvent in step (3) is diethyl ether.
15. The method of claim 14, wherein the ratio of the volume of the diethyl ether to the volume of the sample of step (2) after sizing is 1 to 3:2 to 5.
16. The method of any one of claims 9-15, wherein the chromatographic conditions for gas chromatography mass spectrometry include: a capillary gas chromatographic column is adopted, wherein the chromatographic column is DB-WAX UI, and the specification is 30m multiplied by 0.25mm multiplied by 0.25 mu m; setting the ionization mode as EI, setting the temperature of an ion source at 230 ℃ and setting the temperature of a transmission line at 250 ℃; helium is used as carrier gas, and the flow rate is 1.2mL/min; the gas chromatography temperature program was set to an initial temperature of 40℃and was raised to 230℃at a rate of 6℃per minute and maintained for 14 minutes.
17. The method of any one of claims 9-15, wherein the mass spectrometry conditions for the gas chromatography mass spectrometry comprise: the mass spectrum scanning adopts an ion scanning mode and a full scanning mode, and the scanning range is 35-350 amu.
18. Use of the method according to any one of claims 1-17 for discriminating the aftertaste of white wine.
19. A soy sauce flavor type white spirit aftertaste discriminating apparatus, the apparatus comprising:
the data acquisition module is used for acquiring the content of the organic acid in the white spirit sample;
the judging module is used for inputting the content of the organic acid into a judging model to obtain a white wine aftertaste judging result; the judging model is a functional relation between the content of organic acid and the grade of the aftertaste of the white spirit; the organic acid comprises tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid and oleic acid;
the functional relation is a linear model, Y=K×X+b, K is a functional coefficient, b is a constant, X is the concentration of organic acid, and the score Y has a corresponding grade of the aftertaste of white spirit; when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and oleic acid, the functional relationship includes
Y1=-11.018×C1+121.191×C2-0.481×C3-1.215×C4-1.786×C5-12.907;
Y2=-25.680×C1-7.347×C2+0.159×C3+61.705×C4+1.837×C5-13.576;
The white spirit is any round of base spirit from one round to five rounds;
the concentration of C1 is tetradecanoic acid, the concentration of C2 is pentadecanoic acid, the concentration of C3 is hexadecanoic acid, the concentration of C4 is heptadecanoic acid, and the concentration of C5 is oleic acid.
20. The discriminating apparatus of claim 19, wherein the organic acid further comprises octadecanoic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, or linolenic acid.
21. The discriminating apparatus as defined in claim 19, wherein for the after-taste classes Y1 and Y2, comprising:
when y1=4.831 to 9.595 and y2= 5.161 to 12.915, the wine-like type is three times of low-aftertaste wine;
when y1=5.208-12.668 and y2= 3.670-7.955, the wine-like type is three times of long-aftertaste wine;
when Y1= -14.462 to-8.972 and Y2= -0.095-4.963, the wine sample type is four times of wine with short aftertaste;
when y1= -14.618 to-12.725 and y2= 0.621-2.742, the wine sample type is four times of long-aftertaste wine;
when y1=2.501-4.740 and y2= -9.058 to-6.941, the wine sample type is five rounds of wine with short aftertaste;
when y1=4.100-4.933 and y2= -9.457 to-7.717, the wine sample type is five rounds of wine with long aftertaste.
22. The distinguishing device of claim 19, wherein when the organic acid is tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, oleic acid, L-lactic acid, benzoic acid, 2-furancarboxylic acid, phenylacetic acid, 3-phenylpropionic acid, palmitoleic acid, linoleic acid, linolenic acid, the functional relationship comprises:
Y1=-29.099×C1+108.74×C2-0.554×C3+6.945×C4+1.248×C5+0.548×C6+4.114×C7-0.454×C8-1.769×C9+0.715×C10-2.569×C11-1.836×C12-1.13×C13-1.43×C14-14.672,
Y2=-13.499×C1-56.82×C2-0.151×C3+18.102×C4+0.991×C5+3.663×C6+7.12×C7+
1.582×C8-2.398×C9+0.203×C10+0.911×C11-3.713×C12+0.665×C13-3.662×C14-0.7;
the C1 is the concentration of tetradecanoic acid, the C2 is the concentration of pentadecanoic acid, the C3 is the concentration of hexadecanoic acid, the C4 is the concentration of heptadecanoic acid, the C5 is the concentration of oleic acid, the C6 is the concentration of octadecanoic acid, the C7 is the concentration of L-lactic acid, the C8 is the concentration of benzoic acid, the C9 is the concentration of 2-furancarboxylic acid, the C10 is the concentration of benzoic acid, the C11 is the concentration of 3-phenylpropionic acid, the C12 is the concentration of palmic acid, the C13 is the concentration of linolic acid, and the C14 is the concentration of linolenic acid.
23. The discriminating apparatus as defined in claim 19, wherein for the after-taste classes Y1 and Y2, comprising:
when y1= 13.007-18.384 and y2=1.487-6.067, the wine-like type is three times of short-aftertaste wine;
when y1=9.100-15.389 and y2= -1.803-2.460, the wine sample type is three times of long-aftertaste wine;
when y1= -12.195 to-7.701 and y2= 8.102 to 12.339, the wine sample type is four times of wine with short aftertaste;
when y1= -10.755 to-9.363 and y2= 9.907 to 12.994, the wine sample type is four times of long-aftertaste wine;
when Y1 = -7.211 = -4.645 and Y2 = -12.943 = -9.108, the wine sample type is five times of wine with short aftertaste;
when Y1 = -5.812-3.788 and Y2 = -13.400-10.773, the wine sample type is five times of long-aftertaste wine.
CN202111127944.1A 2021-09-26 2021-09-26 Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid Active CN114113360B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111127944.1A CN114113360B (en) 2021-09-26 2021-09-26 Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111127944.1A CN114113360B (en) 2021-09-26 2021-09-26 Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid

Publications (2)

Publication Number Publication Date
CN114113360A CN114113360A (en) 2022-03-01
CN114113360B true CN114113360B (en) 2023-05-09

Family

ID=80441263

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111127944.1A Active CN114113360B (en) 2021-09-26 2021-09-26 Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid

Country Status (1)

Country Link
CN (1) CN114113360B (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105985877A (en) * 2015-02-12 2016-10-05 北京红星股份有限公司 Production method of acid flavoring liquor
CN107475012A (en) * 2017-09-14 2017-12-15 山西杏花村汾酒厂股份有限公司 A kind of production method of multi-cultur es strengthening porcelain fermented soy fen-flavor type white spirit
CN110804523A (en) * 2019-11-25 2020-02-18 四川大学 Method for producing high-quality mulberry wine by fermentation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105985877A (en) * 2015-02-12 2016-10-05 北京红星股份有限公司 Production method of acid flavoring liquor
CN107475012A (en) * 2017-09-14 2017-12-15 山西杏花村汾酒厂股份有限公司 A kind of production method of multi-cultur es strengthening porcelain fermented soy fen-flavor type white spirit
CN110804523A (en) * 2019-11-25 2020-02-18 四川大学 Method for producing high-quality mulberry wine by fermentation

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Integrative Metagenomics-Metabolo mics for Analyzing the Relationship Between Microorganisms and Non-volatile Profiles of Traditional Xiaoqu;Chi Zhao et al;Front Microbiol;第11卷;617030 *
白酒中有机酸测定方法综述;荆春海等;山东轻工业学院学报(自然科学版);第25卷(第03期);30-33 *
白酒风味化 学研究方法及酱香型白酒风味化学研究进展;唐平;食品科学;第41卷(第17期);315-324 *
高效液相色谱四级 杆飞行时间质谱联用技术检测白酒中高级脂肪酸;廖勤俭等;酿酒科技;第10卷;97-99 *

Also Published As

Publication number Publication date
CN114113360A (en) 2022-03-01

Similar Documents

Publication Publication Date Title
CN104316635A (en) Method for rapidly identifying flavor and quality of fruits
CN107144646B (en) Analysis method for distinguishing true honey and syrup adulterated honey by applying liquid chromatography-mass spectrometry combined with metabonomics method
CN101943686B (en) Method for detecting polydimethylsiloxane
CN103134850A (en) Tea quality rapid detection apparatus and detection method based on characteristic fragrance
CN106353419B (en) Method for measuring flavor components in cigarette mainstream smoke
CN109738569B (en) High-imitation cigarette identification method based on SPME-GC-MS
CN111521722A (en) Method for identifying storage years of fragrant odor type finished product white spirit bottles
CN111060642A (en) Method for classifying and identifying tobacco leaves of same variety and different producing areas
CN113533549B (en) White spirit taste material identification analysis system
CN106404884A (en) Method for quickly evaluating quality consistency of flavors and fragrances of volatile cigarettes by HS-IMR-MS
CN109061017B (en) Method for evaluating cigarette perfuming uniformity
CN113125590A (en) Objective evaluation method for aroma quality of Yunnan red congou tea soup based on rapid gas-phase electronic nose technology
CN107290458A (en) It is a kind of while determining the method for 12 kinds of alkaloids in tobacco and tobacco product
KR20180036354A (en) Method for evaluating a quality of camellia seed oil using Gas Chromatography Ion Mobility Spectrometer(GC-IMS)
CN113917014A (en) Method for rapidly distinguishing production places of jasmine-fragrance grapes based on GC-IMS fingerprint
CN109738567B (en) Method for evaluating uniformity of cut tobacco flavoring mode
CN111505174A (en) Method for identifying true and false cigarettes
Wang et al. An isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of sugars and humectants in tobacco products
CN114113360B (en) Method for distinguishing aftertaste of Maotai-flavor liquor based on hard-volatile organic acid
Xing et al. Characterization of volatile organic compounds in Polygonum multiflorum and two of its processed products based on multivariate statistical analysis for processing technology monitoring
CN109613141B (en) Method for detecting gamma-lactone and delta-lactone compounds in bead blasting liquid of cigarette filter tip
CN112220095A (en) Cigarette production method based on temperature of moisture regain area and cigarette
CN115097021B (en) Method for researching chemical composition difference of cigarette smoke based on gas chromatography-quadrupole electrostatic field orbit trap high-resolution mass spectrum
CN106404877B (en) Flavors and fragrances Fourier Transform Ion cyclotron Resonance mass spectrum fingerprint pattern analysis method
CN102636588A (en) Method for discriminating white spirits by using quartz crystal oscillator electronic nose

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant