CN113155984A - Method for extracting and identifying regional characteristics of white spirit based on gas chromatography-ion mobility spectrometry (GC-IMS) - Google Patents
Method for extracting and identifying regional characteristics of white spirit based on gas chromatography-ion mobility spectrometry (GC-IMS) Download PDFInfo
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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Abstract
The invention discloses a method for quickly extracting regional characteristics of white spirit, and belongs to the field of white spirit quality monitoring, identification and origin identification. The method detects the volatile components of the white spirit by a gas chromatography-ion mobility spectrometry (GC-IMS), analyzes and extracts the characteristics of the white spirit by a data processing method, establishes a database of the characteristic spectrum database of the white spirit, and further performs quality monitoring, identification and origin identification of the white spirit by comparison. Compared with the traditional method, the method does not need sample pretreatment, is simple to operate, high in sensitivity, effective and accurate, and can realize rapid detection of the sample.
Description
Technical Field
The invention relates to a method for extracting and identifying regional characteristics of white spirit based on gas chromatography-ion mobility spectrometry (GC-IMS), belonging to the field of white spirit quality monitoring, identification and origin identification.
Background
The white spirit is one of six distilled spirits listed in the world and brewed by Chinese nationality. The white spirit is made up by using grain as raw material, using distiller's yeast or yeast as saccharification leaven and making them pass through such processes of cooking, saccharification, fermentation, distillation, storage and blending. The unique brewing process in different regions produces diversified white spirit flavors, forms 12 kinds of flavors such as strong aroma, sauce aroma, faint scent, rice aroma, medicine aroma, mixed aroma, phoenix aroma, special aroma, fermented soybean aroma, sesame aroma, fragrant and white spirit, and is deeply loved by consumers. The white spirit has complex components, the stability of batches in production is very important, and in addition, the brands of the white spirit on the market are complex and various in series and the quality is also good and uneven. Therefore, a simple and effective method for identifying and identifying white spirit is urgently needed.
The white spirit produced in different regions is endowed with rich and complex trace components and unique flavor characteristics due to different geographic environments, climates, raw materials, flora and brewing processes. The traditional regional liquor identification method mainly depends on human senses, has high comprehensive evaluation accuracy, is easily influenced by subjectivity, is fuzzy in standard definition, lacks quantitative basis, and has long period for cultivating professional wine tasters and incapability of carrying out large-batch identification, so that an instrumental analysis method is gradually developed. The prior domestic identification method mainly focuses on detecting volatile substances, such as a gas chromatography-mass spectrometry combined method, a near infrared spectroscopy method, an ultraviolet-visible spectroscopy method and the like, and in addition, methods such as an inductively coupled plasma mass spectrometry method, an isotope analysis and the like which take element analysis as a core are explored. Although these methods can identify the origin of the white spirit to some extent, various drawbacks still remain. The water and ethanol abundantly present in wine limit the use of chromatography (such as gas chromatography, GC-MS, etc.), increasing the difficulty of detection. Therefore, complex sample preprocessing is required, which results in a greatly increased probability that the detection result is influenced by human. In addition, quantitative methods (such as area normalization) can also have errors. Although the wine can be directly detected by the spectrometry (such as near infrared spectrometry, ultraviolet-visible absorption spectrometry and the like), the peak type is easily affected by water and ethanol, and if measures are taken to remove the water and the ethanol, the experimental conditions are harsh, the separation process is complex, and the detection result has errors. In addition, the spectroscopy is mainly directed at a certain class of substances, and characteristic substance peaks are not easy to discriminate. Because white spirit belongs to distilled spirit, it is necessary to examine whether isotopes (such as carbon isotopes) and inorganic elements (such as magnesium, iron and barium) in raw materials (such as grains and water) remained in the white spirit can reflect geographical features.
In view of this, it is very important to explore a method for identifying and identifying white spirit rapidly and accurately without complex pretreatment. The invention adopts a gas chromatography-ion mobility spectrometry combination instrument, does not dilute or otherwise process the original white spirit, directly detects, retains the original flavor, truly reflects the regional characteristics of the white spirit, analyzes the obtained three-dimensional spectrogram information through a scientific data processing method, acquires a fingerprint, extracts the regional characteristics, establishes a white spirit characteristic spectrogram database, and further realizes quality monitoring and identification of old wine, year wine and origin in the white spirit production process through spectrogram data comparison.
Disclosure of Invention
The invention aims to provide a method for rapidly extracting different regional characteristics of white spirit, which is used for quality monitoring, identification and origin place identification. The invention adopts two methods of closed volatilization balance and open volatilization to prepare samples: the closed volatilization balance sample preparation is to inject an original white spirit sample into a headspace sample injection bottle, and sample is taken from the upper space of the headspace bottle after the liquid-gas volatilization balance is achieved; the open type volatilization sample preparation is to put the original white spirit sample into an open container to volatilize the original white spirit sample, and to sample the white spirit sample at different volatilization time. Detecting volatile substances in the white spirit by a gas chromatography-ion mobility spectrometry (GC-IMS), analyzing spectrograms by combining a data processing method to obtain fingerprint spectrograms, extracting main regional characteristics, carrying out identification analysis, establishing a characteristic spectrogram database of a white spirit origin place, and identifying the origin place by comparison. The method provided by the invention does not need to carry out complex pretreatment work on the white spirit, directly carries out detection and analysis on the original white spirit, and has the advantages of simple operation, quickness, effectiveness, high sensitivity and objective, real and reliable results.
A method for rapidly extracting the regional characteristics of white spirit based on a gas chromatography-ion mobility spectrometry combined technology comprises the following steps:
step one, preparing a sample (sample incubation): preparing N real white spirit samples, and preparing the samples by adopting two methods of closed volatilization balance and open volatilization. The closed volatilization equilibrium incubation temperature is 10-80 ℃, the equilibrium time is 1-60 min, and a gas sample to be detected is obtained; the incubation temperature of the open volatilization is 10-80 ℃, the total volatilization time is 0-1200 min, and the sampling interval is 1-300 min;
step two, detecting by gas chromatography-ion mobility spectrometry (GC-IMS): gas chromatography (G)C) The sample injection volume is 50-1000 mu L, the sample injection needle temperature is 30-120 ℃, the column temperature is 25-80 ℃, and the carrier gas is high-purity nitrogen (N) with the purity of 99.999%2) Eluting by adopting a programmed pressure boosting mode, and detecting gas molecules separated by a gas chromatography capillary column in an ion migration tube at the temperature of 25-200 ℃ under the condition that the drift gas (purge gas) is high-purity nitrogen (N) with the purity of 99.999%2) The flow rate is 10-500 mL/min, and three-dimensional spectrogram data of a real white spirit sample is obtained after detection;
step three, spectrogram data processing: and D, processing the three-dimensional spectrogram data obtained in the step two by adopting a data processing method to obtain a fingerprint, extracting and identifying main characteristics, and establishing a liquor characteristic spectrogram database.
The invention has the beneficial effects that:
the method adopts a gas chromatography-ion mobility spectrometry combined technology, realizes the detection of volatile components in the white spirit in different regions simply and quickly, can determine a substance fingerprint spectrum through data processing under the condition of not knowing specific components exactly, and then extracts main characteristic substances to realize the identification of the white spirit. The method does not need complex sample pretreatment, is simple to operate, consumes short time, and has great significance for quality monitoring, liquor variety identification and origin identification in the liquor production process.
Drawings
FIG. 1 closed volatile equilibrium gas chromatography carrier gas flow velocity diagram
FIG. 2 finger print of white spirit with balanced sealed volatilization
FIG. 3 is a three-dimensional analysis chart of the principal components of a white spirit with balanced sealed volatilization
FIG. 4 open volatized gas chromatography carrier gas flow rate diagram
FIG. 5 is an original three-dimensional spectrogram of open-type volatilized Chinese liquor
FIG. 6 fingerprint of open-type volatile Chinese liquor
FIG. 7 is a three-dimensional analysis chart of main components of open-type volatilized white spirit
FIG. 8 is a two-dimensional graph of the principal component analysis of open-type volatilized spirit
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
The method is mainly suitable for extracting and identifying the regional characteristics of the white spirit. In the example, white spirit of two different series (A series and B series) of the same brand in a certain region is taken as a detection object, samples are prepared by adopting two methods of closed volatilization balance and open volatilization respectively, a gas chromatography-ion mobility spectrometry combined instrument is used for detection, obtained three-dimensional spectrogram information is analyzed by a scientific data processing method, region characteristics are extracted, and a white spirit original production region spectrogram database is established. The quality monitoring, the identification of old wine, wine of the year and the like in the white wine production process and the identification of the origin of the white wine can be carried out by comparing the spectrogram data.
Example 1: regional characteristic extraction and identification of closed volatile balanced white spirit
(1) Preparation of samples (sample incubation): preparing two batches of 6 real white spirit samples (comprising A, B series) respectively, preparing samples by adopting a closed volatilization balance method, respectively placing the samples in 20mL headspace bottles, vibrating, heating and incubating at the incubation temperature of 60 ℃ for 20min, and obtaining a gas sample to be detected;
(2) gas chromatography-ion mobility spectrometry (GC-IMS) detection: the sample introduction volume of the Gas Chromatography (GC) was 200. mu.L, the needle temperature was 80 ℃, the column temperature was 60 ℃, and the carrier gas was 99.999% high purity nitrogen (N)2) Eluting by using programmed pressure boosting mode, wherein the flow rate of carrier gas is shown in figure 1, detecting the gas molecules separated by gas chromatography capillary column in an ion mobility spectrometer at 50 deg.C with drift gas (sweep gas) of 99.999% high purity nitrogen (N)2) The flow rate is 150mL/min, and each sample is parallelly measured for 3 times;
(3) step three, spectrogram data processing: and (3) processing the three-dimensional spectrogram obtained in the step two by adopting different data processing methods to obtain a fingerprint (figure 2), and extracting main characteristics for identification (figure 3).
FIG. 2 shows two batches of 42-degree A series (42-1-1, 42-1-2, 42-2-1, 42-2-2, 42-3-1, 42-3-2, 42-4-1, 42-4-2, 42-5-1, 42-5-2) and B series (42-6-1, 42-6-2) (the first digit 42 in the sample name represents the degree, the middle digit represents different sample numbers, and the last digits 1 and 2 represent batch 1 and batch 2, respectively) closed volatilization equilibrium fingerprint of white spirit. Quality monitoring can be carried out according to the fingerprint spectrums of the white spirits of different batches. The content of substances in the three types of white spirits of 42-1, 42-2 and 42-4 in different batches is not greatly changed when observed from the fingerprint, which shows that the batches have good stability and stable quality; the content of a small part of substances in the two types of white spirits of 42-5 and 42-6 in different batches is obviously changed, which indicates that the batches have better stability and more stable quality; the content of most substances in the 42-3 white spirit in different batches is greatly changed, which indicates that the stability of the batches is poor and the quality is unstable. In addition, the obvious difference of the white spirits of different series can be visually seen from the fingerprint, and the obvious difference can be observed for different samples of the same series (A series).
The principal component analysis method is used to extract the main features for identification (fig. 3). The extracted characteristic substances can obviously identify 6 types of wines, indicate the characteristics of closed volatilization balance of the extracted white spirit, and can be used for quality monitoring and identification and origin place identification in the white spirit production process.
Example 2: regional characteristic extraction and identification of open volatile white spirit
(1) Preparation of samples (sample incubation): preparing 5 real white spirit samples (comprising A, B series), preparing samples by an open volatilization method, respectively placing in an open bottle container, vibrating, heating and incubating at 60 deg.C for 180min to obtain gas samples to be tested;
(2) gas chromatography-ion mobility spectrometry (GC-IMS) detection: the sample introduction volume of the Gas Chromatography (GC) was 200. mu.L, the needle temperature was 80 ℃, the column temperature was 60 ℃, and the carrier gas was 99.999% high purity nitrogen (N)2) Eluting with programmed pressure boosting mode, with carrier gas flow rate as shown in FIG. 4, sampling detection time interval of 30min, detecting gas molecules separated by gas chromatography capillary column with drift tube temperature of 50 deg.C and drift gas (sweep gas) of 99.999% high purity nitrogen (N)2) The flow rate is 150mL/min, and a three-dimensional spectrogram (figure 5) of a real white spirit sample is obtained after detection;
(3) step three, spectrogram data processing: and (3) processing the three-dimensional spectrogram obtained in the step two by adopting different data processing methods to obtain a fingerprint (figure 6) and extracting main characteristics for identification (figures 7 and 8).
FIG. 5 is the original three-dimensional spectrogram of open volatilization of Chinese liquor. Wherein the Chinese liquor is divided into A series (38 degree in FIG. 5a, 42 degree in FIG. 5B, 52 degree in FIG. 5 c) and B series (42 degree in FIG. 5d, 52 degree in FIG. 5 e). The three-dimensional spectrogram shows that the content of the volatile substances in the white spirit changes obviously with the passage of time. According to fig. 6, it can be seen that the types and contents of the aroma substances of the white spirit are less and less, the contents of most ester substances are reduced continuously, but the content of partial substances (alcohols such as propanol, butanol, hexanol and the like, aldehydes such as hexanal, benzaldehyde, furfural and the like) tends to increase first and then decrease, and the content of small-amount components (such as acetic acid) is increased continuously. In addition, the peak value of the alcohol substances in the high-alcohol-content white spirit appears later than that of the low-alcohol-content white spirit, and partial ester substances and the alcohol substances have similar changes, namely the trend of increasing firstly and then decreasing later, for example, the contents of octyl acetate, heptyl acetate, ethyl caprylate and ethyl heptanoate in the A series of 52-alcohol-content white spirits increase firstly and decrease after half an hour. By observing the figure 6, the difference of the volatilization properties of the white spirits with different alcoholic contents can be visually observed, the obvious difference of A, B series can be visually observed, and the great difference of the substance content in the same time period is mainly reflected.
The principal component analysis method is adopted to extract the main characteristics for identification (figure 7, figure 8). According to the discrete degree of the 5 samples in each time period, whether the selected characteristic substances can better identify the white spirit can be judged. The discreteness is obvious, which indicates that the extracted characteristic substances can be used for identifying the 5 samples, and the contrary is not possible. The method extracts the volatility characteristics of the white spirit through PCA analysis, and can be used for quality monitoring, identification, origin place identification and other aspects in the white spirit production process.
The data processing method used in the above embodiments is a principal component analysis method, and is only for illustrating the present invention. The data processing method is variable within the scope of the invention, and the invention is also suitable for extracting and identifying other liquor regional characteristics. All equivalent changes and modifications based on the present invention should not be excluded from the scope of the present invention.
Claims (5)
1. The invention relates to a method for rapidly extracting regional characteristics of white spirit, which is used for detecting the white spirit by a gas chromatography-ion mobility spectrometry (GC-IMS) and can be used for monitoring and identifying the quality of the white spirit and identifying the origin.
2. The detection method according to claim 1, wherein the sample preparation method comprises both closed volatilization equilibrium and open volatilization, and is characterized in that:
the method comprises the steps of (1) adopting undiluted or other processed original liquor samples, performing closed volatilization balance sample preparation, namely injecting the original liquor samples into a headspace sample injection bottle, sampling from the upper space of the headspace bottle after liquid-gas volatilization balance is achieved, and detecting by adopting GC-IMS (gas chromatography-ion mobility spectrometry), wherein the sample preparation conditions are that the incubation temperature is 10-80 ℃, the incubation temperature is 30-70 ℃, the balance time is 1-60 min, and the incubation time is 5-30 min; the open type volatilization sample preparation is to put an original white spirit sample into an open container to volatilize the original white spirit sample, sample at different volatilization time, and then detect the original white spirit sample by adopting GC-IMS, wherein the sample preparation conditions are that the incubation temperature is 10-80 ℃, the recommended temperature is 30-60 ℃, the total volatilization time is 0-1200 min, and the sampling interval is 1-300 min, and the recommended time is 5-30 min.
3. A liquor regional characteristic extraction method according to claim 1, which is characterized by comprising the following detection steps:
step one, preparing a sample (sample incubation): preparing N real white spirit samples, and preparing samples according to the characteristics of claim 2;
step two, detecting by gas chromatography-ion mobility spectrometry (GC-IMS): the sample introduction volume of the Gas Chromatography (GC) is 50-1000 mu L, the temperature of a sample introduction needle is 30-120 ℃, the temperature of a column is 25-80 ℃, and the carrier gas is high-purity nitrogen (N) with the purity of 99.999 percent2) Eluting by adopting a program boosting mode; gas molecules separated by a gas chromatography capillary column enter an ion mobility spectrometer for detection, the temperature of a drift tube is 25-200 ℃, and the temperature of drift gas (purge gas) is 99.999 percent of high-purity nitrogen (N)2) The flow rate is 10-500 mL/min, and three-dimensional spectrogram data of a real white spirit sample is obtained after detection;
step three, spectrogram data processing: and D, processing the three-dimensional spectrogram data obtained in the step two by adopting a data processing method to obtain a fingerprint, extracting and identifying main characteristics, and establishing a liquor characteristic spectrogram database.
4. A data processing method according to step three of claim 3, including but not limited to the following methods:
and (3) extracting characteristics by adopting methods such as a filtering method (Filter), a wrapping method (Wrapper), an embedding method (Embedded), Principal Component Analysis (PCA), Linear Discriminant Analysis (LDA) and the like.
5. The application of the method for rapidly extracting the regional characteristics of the white spirit according to claim 1 includes but is not limited to the following aspects:
by comparing the spectrogram data of the white spirit, the quality monitoring, the identification of the old spirit and the wine of the year and the identification of the origin of the white spirit in the production process of the white spirit are realized.
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| CN114428135A (en) * | 2022-01-19 | 2022-05-03 | 上海应用技术大学 | Identification method of edible fungus flavor components based on gas chromatography-ion mobility spectrometry |
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