CN114166955A - Analysis method for influence of storage time on quality of Fotiaoqiang - Google Patents
Analysis method for influence of storage time on quality of Fotiaoqiang Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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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- G01N27/622—Ion mobility spectrometry
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
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- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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Abstract
The invention relates to the technical field of food, in particular to an analysis method for the influence of storage time on the quality of a Fotiaoqiang. Which comprises the following steps: respectively storing the same type of Fotiaoqiang at the temperature of below 18 ℃ below zero for different times to obtain Fotiaoqiang samples with different storage times; obtaining gas chromatography-ion mobility spectrograms of the Fotiaoqiang samples with different storage times through gas chromatography-ion mobility spectrometry (GC-IMS) analysis; determining the concentration change of all volatile organic compounds in different storage time, the dynamic change of different types of volatile organic compounds in different storage time and the distribution condition of main components in different storage time through a gas chromatography-ion mobility spectrogram, and determining the influence of the storage time on the quality of the Fotiaoqiang. The invention determines the influence of the storage time on the quality of the Fotiaoqiang by qualitatively and quantitatively analyzing the difference of all volatile organic compounds of the Fotiaoqiang sample, and can predict the storage time of the Fotiaoqiang product.
Description
Technical Field
The invention relates to the technical field of food, in particular to an analysis method for influence of storage time on the quality of a Fotiaoqiang wall.
Background
The Buddha jumping wall, also known as "altar incense" and "good fortune and longevity whole", is a head dish of traditional Mincai, and the processing process thereof integrates various cooking techniques of frying, stir-frying, steaming, stewing and the like. The main raw materials of the soup comprise abalone, sea cucumber, turtle shell, yellow croaker gelatin, mushroom, tendon, flower mushroom, dried scallop, quail egg and the like, and the soup is added with prepared soup-stock and then stewed with slow fire. The Buddha jumping wall is delicious in taste, mellow in mouthfeel and high in nutritional value, and is popular with consumers.
At present, the quality of the Fotiaoqiang is mostly evaluated by sense organs, electronic tongues or texture instruments, and the obtained conclusions are isolated from each other, so that the quality of the Fotiaoqiang cannot be systematically and scientifically evaluated. The enterprise technicians select the unfreezing mode according to experience or subjectively, so that the loss of the flavor substances of the Fotiaoqiang or the flavor substances of the Fotiaoqiang cannot be found out.
The method mainly comprises methods such as sensory analysis and the like, and the method can be relatively reliably evaluated by a master with abundant tasting experience on the Fotiaoqiang flavor, but is easy to be interfered by external factors and has certain subjectivity. In order to obtain a more accurate result, the existing method uses equipment such as an electronic nose, an electronic tongue and the like for evaluation, but the precision of detection is poor, and the components cannot be determined qualitatively; the sample is qualitatively and quantitatively analyzed by adopting analysis technologies such as High Performance Liquid Chromatography (HPLC), Gas Chromatography (GC), chromatography-mass spectrometry (GC-MS) and the like in combination with a chemometric method, the obtained experimental result is relatively accurate, but the operation is complex, the analysis time is long, the rapid analysis of the sample is not facilitated, and the requirement of rapid detection of a large number of samples cannot be met.
Disclosure of Invention
Technical problem to be solved
In view of the above disadvantages and shortcomings of the prior art, the present invention provides an analysis method for analyzing the influence of storage time on the quality of a Buddha jumping wall, which qualitatively and quantitatively obtains the influence of different storage times on the quality of the Buddha jumping wall sample by establishing gas chromatography-ion mobility spectrograms of the Buddha jumping wall sample at different storage times, and is convenient for reversely verifying the storage time of an unknown Buddha jumping wall sample.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
in a first aspect, the present invention provides a method for analyzing the influence of storage time on the quality of a Buddha jumping wall, comprising the following steps:
s1 includes: storing the same Fotiaoqiang for different times below-18 ℃ respectively to obtain Fotiaoqiang samples corresponding to different storage times;
s2 includes: obtaining gas chromatography-ion mobility spectrograms of the Fotiaoqiang samples with different storage times through gas chromatography-ion mobility spectrometry;
s3 includes: extracting volatile substances of the Fotiaoqiang sample in different storage time to obtain the concentration change condition of all volatile organic compounds;
s4 includes: qualitatively analyzing all volatile organic compounds on a gas chromatography-ion mobility spectrogram of the Fotiaoqiang sample with different storage times to obtain dynamic change conditions of different types of volatile organic compounds at different storage times;
s5 includes: performing principal component analysis by taking all volatile substance peak intensities of the Fotiaoqiang samples in different storage times as analysis objects to determine the distribution condition of the principal components;
s6 determines the influence of the storage time on the quality of the Fotiaoqiang by the concentration change of all volatile organic compounds in steps S3-S5 under different storage times, the dynamic change of different types of volatile organic compounds under different storage times and the distribution condition of main components under different storage times.
Storage time Buddha of the inventionIn an optional scheme of the analysis method for the influence of the wall jump quality, in step S2, the detection conditions of the gas chromatography-ion mobility spectrometry combination are as follows: automatic headspace sample introduction unit: the sample volume is 500 mu L, the incubation time is 15min, the incubation temperature is 80 ℃, the sample injection needle temperature is 85 ℃, and the incubation rotation speed is 500 rpm; a chromatographic column: FS-SE-54-CB-1 quartz capillary column (15m × 0.53mm, 0.5 μm), analysis time 30min, chromatographic column temperature 60 deg.C, carrier gas N2(the purity is more than or equal to 99.999%); IMS conditions: by using N2(purity 99.999%) as drift gas for IMS, the drift tube temperature was set at 45 deg.C.
In the optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the reverse-2-pentenal, the furfural, the green leaf aldehyde, the n-hexanal, the heptanal, the reverse-2-heptenal, the benzaldehyde, the reverse-2-octenal, the phenylacetaldehyde, the n-octanal, the nonanal and the isovaleraldehyde are taken as characteristic aldehyde substances, and the influence of the storage time on the quality of the Fotiaoqiang is determined by determining the content of the characteristic aldehyde substances in the Fotiaoqiang samples with different storage times.
In an optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the method further comprises the following steps:
s7, comparing the richness of aldehyde substances in the Fotiaoqiang samples with different storage time to determine the influence of the storage time on the quality of the Fotiaoqiang:
the comparative calculation of the evaluation of the richness of the aldehyde substances comprises the following formula I:
wherein, ynAnd y'nRespectively obtaining the content of the nth same aldehyde substance for the stored Fotiaoqiang sample and the non-stored Fotiaoqiang sample;
when the value of Y is less than n, the richness of the aldehyde substances in the stored Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang sample, and the richness of the aldehyde substances in the stored Fotiaoqiang sample is influenced.
In an optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the method further comprises the following steps:
s7, comparing the abundance of flavor substances of the Fotiaoqiang samples in different storage times to determine the influence of the storage time on the quality of the Fotiaoqiang;
the calculation of the flavor richness ratio comprises the following formula II:
wherein:
xmand x'mRespectively determining the content of the mth same flavor substance in the stored Fotiaoqiang sample and the content of the mth same flavor substance in the non-stored Fotiaoqiang sample;
when the numerical value of X is less than m, the richness of the flavor substances obtained by the Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang, and the richness of the flavor substances of the stored Fotiaoqiang is influenced;
the larger the X value obtained, the closer to the m value, which indicates that the influence of the corresponding storage time on the flavor substances of the Fotiaoqiang sample is smaller.
In an optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the method further comprises the following steps:
s7, determining the influence of the storage time on the quality of the Fotiaoqiang by comprehensively comparing the flavor substances of the Fotiaoqiang samples in different storage times;
the calculation of the comprehensive alignment comprises the formula three:
m is 0.6X +0.4Y, formula three;
wherein X and Y are obtained according to the methods of formula two and formula one respectively;
when the M value is less than 0.6M +0.4n, the quality of the stored Fotiaoqiang sample is judged to be poor compared with the quality of the stored Fotiaoqiang sample.
In an optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the method further comprises the following steps: the influence of the storage time on the quality of the Fotiaoqiang is determined by measuring the protein content in the Fotiaoqiang samples with different storage times.
In an optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the method further comprises the following steps: the influence of the storage time on the quality of the Fotiaoqiang is determined by measuring the amino acid composition condition and the corresponding taste activity value in the Fotiaoqiang sample with different storage times.
In the optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the influence of the storage time on the quality of the Fotiaoqiang is determined according to the contents of glutamic acid, arginine and alanine.
In an optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the method further comprises the following steps: determining the influence of the storage time on the quality of the Fotiaoqiang according to the richness of the taste of the Fotiaoqiang in different storage times, wherein the taste comprises salty taste, delicate flavor aftertaste, astringent taste, bitter taste and bitter aftertaste.
In an optional scheme of the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the method further comprises the following steps: determining the influence of the storage time on the quality of the Fotiaoqiang can reversely determine the storage time of an unknown Fotiaoqiang sample.
(III) advantageous effects
The invention has the beneficial effects that:
in the analysis method for the influence of the storage time on the quality of the Fotiaoqiang, the difference of all volatile organic compounds of samples of the Fotiaoqiang in different storage times is qualitatively and quantitatively analyzed, so that the influence of the storage time on the quality of the Fotiaoqiang can be systematically, comprehensively or accurately determined, and the storage time of unknown Fotiaoqiang samples can be reversely determined.
Furthermore, tests show that the influence of different thawing modes on the quality of the Fotiaoqiang sample can be analyzed more simply and scientifically by only measuring the change of characteristic aldehyde substances.
Furthermore, the problem that different thawing modes can lead to the fact that the content of partial flavor substances or aldehydes is increased or the content of partial flavor substances is reduced, and therefore a conclusion cannot be directly drawn can be solved through a formula method.
Drawings
FIG. 1 shows a method for preparing Fotiaoqiang;
FIG. 2 is a gas chromatography-ion mobility spectrum of Fotiaoqiang samples of example 1 with different storage times;
FIG. 3 is a comparison graph of gas chromatography-ion mobility spectrometry fingerprints of Fotiaoqiang samples of example 1 with different storage times;
FIG. 4 is a GC-IMS principal component analysis chart in inventive example 1;
FIG. 5 is a graph of salty taste, umami taste and richness of Fotiaoqiang in example 3 of the present invention at different storage times;
FIG. 6 is a graph of the bitter, astringent and bitter aftertaste blisters of Fotiaoqiang of example 3 of the present invention during different storage times.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present invention by way of specific embodiments thereof.
The invention provides an analysis method for comprehensively and systematically determining the influence of storage time on the quality of a Fotiaoqiang, which comprises the following steps:
s1 includes: storing the same Fotiaoqiang for different times below-18 ℃ respectively to obtain Fotiaoqiang samples corresponding to different storage times;
s2 includes: obtaining gas chromatography-ion mobility spectrograms of the Fotiaoqiang samples with different storage times through gas chromatography-ion mobility spectrometry;
s3 includes: extracting volatile substances of the Fotiaoqiang sample in different storage time to obtain the concentration change condition of all volatile organic compounds;
s4 includes: qualitatively analyzing all volatile organic compounds on a gas chromatography-ion mobility spectrogram of the Fotiaoqiang sample with different storage times to obtain dynamic change conditions of different types of volatile organic compounds at different storage times;
s5 includes: performing principal component analysis by taking all volatile substance peak intensities of the Fotiaoqiang samples in different storage times as analysis objects to determine the distribution condition of the principal components;
s6 determines the influence of the storage time on the quality of the Fotiaoqiang by the concentration change of all volatile organic compounds in steps S3-S5 under different storage times, the dynamic change of different types of volatile organic compounds under different storage times and the distribution condition of main components under different storage times.
The Fotiaoqiang is taken as a traditional well-known food, and the composition and the content of flavor substances are important standards for evaluating the quality of the Fotiaoqiang, so that the influence of different storage times on the Fotiaoqiang is comprehensively and scientifically analyzed by measuring the content and the composition of all flavor substances in a Fotiaoqiang sample.
All volatile organic compounds in the Fotiaoqiang sample in different storage time are used as the object of analysis, and the quality of the Fotiaoqiang sample is determined from the aspect of the volatile organic compounds. Specifically, gas chromatography-ion mobility spectrometry of the Fotiaoqiang samples with different storage times is determined through gas chromatography-ion mobility spectrometry, and comparison is carried out to obtain characteristic peaks of all volatile organic compounds.
Wherein use is made of
The Gallery Plut plug-in software in the flavor analyzer compares fingerprint spectrograms of Fotiaoqiang samples with different storage times, each row in the fingerprint spectrogram represents all signal peaks selected from one Fotiaoqiang sample with different storage times, each column in the fingerprint spectrogram represents signal peaks of the same volatile organic compound in the Fotiaoqiang samples with different storage times, and the complete volatile organic compound information of each Fotiaoqiang sample and the difference of the volatile organic compounds among the Fotiaoqiang samples with different storage times can be seen from the fingerprint spectrograms, so that the change of all flavor substances in the Fotiaoqiang samples with different storage times can be visually determined.
The method can be used for qualitatively analyzing the Fotiaoqiang samples with different storage times by using an NIST database and an IMS database which are built in GC-IMS Library Search software, and qualitatively analyzing to obtain specific organic flavor substances including aldehydes, alcohols, esters, ketones, terpenes and other categories, including migration time and other parameters, and determining the content of each substance, thereby analyzing and determining the specific flavor of the Fotiaoqiang samples with different storage times.
The invention also obtains a principal component analysis diagram through GC-IMS principal component analysis, and the principal component analysis diagram can be used for determining Fotiaoqiang samples with different storage times.
In conclusion, the method can obtain specific flavor conditions from the macroscopic change condition of all volatile organic compounds to the specific qualitative and quantitative change of the concentration of each volatile organic compound, and finally can judge the Fotiaoqiang wall samples with different storage times by drawing a principal component analysis chart.
The invention can be used for judging the specific storage time of the same type of Buddha jumping wall sample to be detected by taking the drawn principal component analysis chart as a standard analysis chart. The method specifically comprises the steps of detecting a Fotiaoqiang sample to be detected through GC-IMS, obtaining a principal component analysis chart to be detected through principal component analysis, and comparing similarity of the principal component analysis chart to a standard analysis chart to obtain storage time corresponding to similar data in the standard analysis chart.
In this embodiment, the detection conditions of the gas chromatograph-ion mobility spectrometer are as follows: automatic headspace sample introduction unit: the sample injection volume is 500 mu L, the incubation time is 15min, the incubation temperature is 80 ℃, the sample injection needle temperature is 85 ℃, and the incubation rotation speed is 500 rpm; a chromatographic column: FS-SE-54-CB-1 quartz capillary column (15m is multiplied by 0.53mm, 0.5 mu m), analysis time is 30min, chromatographic column temperature is 60 ℃, and carrier gas N2 (purity is more than or equal to 99.999 percent); IMS conditions: by using N2(purity 99.999%) as drift gas for IMS, the drift tube temperature was set at 45 deg.C.
In order to determine the influence of the storage time on the quality of the Fotiaoqiang in a quantitative and simplified mode, the method further comprises the following steps:
comparing the richness of aldehyde substances in the Fotiaoqiang samples with different storage time to determine the influence of the storage time on the quality of the Fotiaoqiang:
the comparative calculation of the evaluation of the richness of the aldehyde substances comprises the following formula I:
wherein, ynAnd y'nRespectively obtaining the content of the nth same aldehyde substance for the stored Fotiaoqiang sample and the non-stored Fotiaoqiang sample;
when the value of Y is less than n, the richness of the aldehyde substances in the stored Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang sample, and the richness of the aldehyde substances in the stored Fotiaoqiang sample is influenced.
Tests show that the quality of the Fotiaoqiang sample is better, the richness of the aldehyde substances is higher, and therefore, the influence of the storage time on the Fotiaoqiang sample can be determined only by comparing the richness of the aldehyde substances. By means of the size of the result, the quality of any two unknown Fotiaoqiang samples of the same Fotiaoqiang can be compared, and the method for quantitatively evaluating the Fotiaoqiang samples is achieved.
Wherein, the trans-2-pentenal, the furfural, the green leaf aldehyde, the n-hexanal, the heptanal, the trans-2-heptenal, the benzaldehyde, the trans-2-octenal, the phenylacetaldehyde, the n-octenal, the nonanal and the isovaleraldehyde are taken as characteristic aldehyde substances for detection and calculation.
The invention also comprises the following steps:
comparing the richness of flavor substances of the Fotiaoqiang samples in different storage times to determine the influence of the storage time on the quality of the Fotiaoqiang;
the calculation of the richness ratio of the flavor substances comprises the following formula II:
wherein:
xmand x'mRespectively determining the content of the mth same flavor substance in the stored Fotiaoqiang sample and the content of the mth same flavor substance in the non-stored Fotiaoqiang sample;
when the numerical value of X is less than m, the richness of the flavor substances obtained by the Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang, and the richness of the flavor substances of the stored Fotiaoqiang is influenced;
the larger the X value obtained, the closer to the m value, which indicates that the influence of the corresponding storage time on the flavor substances of the Fotiaoqiang sample is smaller.
And the influence of the storage time on the Fotiaoqiang sample can be presented in a quantitative mode through the calculation of the formula II, so that the calculation and comparison are convenient.
In order to better consider the contribution of aldehyde substances to the flavor substances, the embodiment of the invention corrects and compares the change of the flavor substances in a comprehensive comparison mode,
the calculation of the comprehensive alignment comprises the formula three:
m is 0.6X +0.4Y, formula three;
wherein X and Y are obtained according to the methods of formula two and formula one respectively;
when the M value is less than 0.6M +0.4n, the quality of the stored Fotiaoqiang sample is judged to be poor compared with the quality of the stored Fotiaoqiang sample.
And the change of the flavor substances of the Fotiaoqiang wall samples in different storage times can be comprehensively determined by the calculation of the formula III so as to determine different qualities. Wherein, the weighted values of X and Y are 0.6 and 0.4 respectively, the weighted calculation is carried out according to the higher contribution of the aldehyde substance to the flavor substance, and the change of all the flavor substances has higher contribution relative to the aldehyde substance, therefore, the influence of different storage time on the Fotiaoqiang sample can be quantified through the weighting. The higher the value of M, the better the quality and the less the corresponding storage time has an effect on the quality.
In order to evaluate the influence of the storage time on the quality of the Fotiaoqiang wall comprehensively and scientifically from the aspect of volatile organic compounds, the method determines the content of protein in the Fotiaoqiang wall samples with different storage times, the amino acid composition condition and the corresponding taste activity value in the Fotiaoqiang wall samples with different storage times and the taste abundance of the Fotiaoqiang wall with different storage times, and further determines the influence of the storage time on the quality of the Fotiaoqiang wall.
As shown by tests: the protein content of the Fotiaoqiang has no significant difference in the first 3 months (p >0.05), and the decrease is significant by 6 months. The contents of hydroxyproline, fat and total sugar are not obviously different (p is more than 0.05), mainly because the activity of microorganisms and enzymes is inhibited by the Fotiaoqiang at the low temperature of-18 ℃, the Fotiaoqiang is not easy to contact with external oxygen, and a sample system is relatively stable. Therefore, only the protein and its corresponding amino acid profile were selected as evaluation indices.
In the amino acid distribution of the Fotiaoqiang, the influence of the storage time on the quality of the Fotiaoqiang is preferably determined according to the content of glutamic acid, arginine and alanine. The test shows that the Fotiaoqiang sample has the largest contribution value of glutamic acid, arginine and alanine to the taste.
In the present invention, preferably, salty taste, umami taste, astringent taste and bitter aftertaste are used as evaluation indexes in taste. The test shows that: the storage time has no significant influence on the sour taste, the sweet taste, the bitter taste and the aftertaste of the delicate flavor of the Fotiaoqiang.
On the basis of taking volatile organic compounds as evaluation indexes, the invention can further analyze the influence of storage time on the quality of the Fotiaoqiang wall from the taste perspective by taking the contents of protein, glutamic acid, arginine and alanine, and salty taste, delicate taste, astringent taste and bitter aftertaste as further evaluation indexes.
Among them, the contents of protein, glutamic acid, arginine and alanine, and the evaluation results of salty, umami, astringent and bitter aftertastes and flavor substances have correlations. Thus, in embodiments of the present invention, the effect of two different thawing patterns on the quality of the Buddha jumping wall can be determined and compared by merely evaluating the salty, umami, astringent and bitter aftertastes and the flavor substances.
The evaluation of salty, umami, astringent and bitter aftertastes and flavor substances may be contrary to the evaluation results of flavor substances, and thus, there may be an optimum storage time to optimize the salty, umami, astringent and bitter aftertastes and the evaluation results of flavor substances.
The results of the influence of the storage time on the quality of the Fotiaoqiang can be used for determining the storage time of unknown Fotiaoqiang samples.
In order to better understand the above technical solutions, exemplary embodiments of the present invention will be described in more detail below. While the following shows exemplary embodiments of the invention, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1
A method for evaluating the influence of storage time on the quality of a Fotiaoqiang comprises the following steps:
s1 preparation of Fotiaoqiang sample: dividing the Fotiaoqiang prepared by the method shown in figure 1 into seven groups, respectively storing at-18 ℃ for 0 day, 1 week, 1 month, 3 months, 6 months, 9 months and 12 months, respectively taking out the products, thawing, stirring uniformly, and respectively taking soup to obtain samples of the Fotiaoqiang corresponding to different storage times;
s2, detecting by a gas chromatography-ion mobility spectrometry instrument to obtain Fotiaoqiang sample GC-IMS (gas chromatography-ion mobility spectrometry) spectrograms corresponding to different storage times as shown in figure 2, wherein the abscissa represents ion mobility time (Drifttime, Dt), the ordinate represents retention time (Retentitime, Rt) of the gas chromatography, and each point in figure 2 represents a volatile organic compound;
s3 application
The Gallery Plot plug-in the flavor analyzer extracts all volatile substances in a sample spectrogram to form a fingerprint map, so that the change rule of the volatile substance composition of the Fotiaoqiang sample in different storage times can be comprehensively and visually analyzed;
in FIG. 3, each row of the graph represents the total signal peaks selected in one sample, each column of the graph represents the signal peaks of the same volatile organic compound in different samples, the color of each point in the graph represents the concentration of the substance, white represents lower concentration, red represents higher concentration, and darker color represents higher concentration; although fig. 3 is presented in a grayscale, the results obtained with this embodiment are not affected:
s4, performing qualitative analysis on volatile organic compounds of the Fotiaoqiang samples obtained in 6 different storage times by using an NIST database and an IMS database built in GC-IMSLibrarySearch software, and qualitatively detecting that the volatile substances are 63 monomers and dimers of partial substances, wherein the dimers mainly comprise aldehydes, alcohols, esters, ketones, terpenes and other categories; specific results are shown in table 1:
TABLE 1 qualitative analysis of volatile substances in Fotiaoqiang at different storage times
TABLE 1 (continuation)
TABLE 1 (continuation)
TABLE 1 (continuation)
In summary, the following results can be obtained: the composition of volatile substances of the Fotiaoqiang sample is not changed greatly in the first 3 months, the contained aldehyde and alcohol volatile substances are more, the change is obvious when the Fotiaoqiang sample is stored for 6 months, the change of the Fotiaoqiang sample is larger when the Fotiaoqiang sample is stored for 9 months and 12 months, and at the moment, ester substances and ketone substances in the Fotiaoqiang are more abundant.
S5 GC-IMS principal component analysis
The results of the principal component analysis using the peak intensities of all volatile substances of the Buddha rampart samples stored at different times as the analysis objects are shown in FIG. 4, in which the PC1 contribution rate is 65%, the PC2 contribution rate is 11%, and the cumulative contribution rate is 76% (> 70%), indicating that the volatile substance information can represent the Buddha rampart. As can be seen from the observation of FIGS. 4-6, the Fotiaoqiang samples in 6 different storage periods are clustered respectively, and the distances between the samples in 1 week, 1 month and 3 months are relatively close, which indicates that the volatile substances of the three samples are relatively similar, while the samples in 6 months, 9 months and 12 months are relatively far from the first three samples, which indicates that the volatile flavor differences between the samples in 6 months, 9 months and 12 months and the volatile flavor differences between the samples in 1 week, 1 month and 3 months are relatively large.
Example 2
The graph of the principal component analysis obtained in example 1 was used to determine the storage time of the test Fotiaoqiang. The method specifically comprises the steps of detecting a Fotiaoqiang sample to be detected through a GC-IMS, obtaining a principal component analysis chart to be detected through principal component analysis, and comparing similarity with a standard analysis chart to obtain storage time corresponding to similar data in the standard analysis chart.
In this embodiment, the detection conditions of the gas chromatography-ion mobility spectrometry combination apparatus are as follows: automatic headspace sample introduction unit: the sample injection volume is 500 mu L, the incubation time is 15min, the incubation temperature is 80 ℃, the sample injection needle temperature is 85 ℃, and the incubation rotation speed is 500 rpm; a chromatographic column: FS-SE-54-CB-1 quartz capillary column (15m × 0.53mm, 0.5 μm), analysis time 30min, chromatographic column temperature 60 deg.C, carrier gas N2(the purity is more than or equal to 99.999%); IMS conditions: by using N2(purity 99.999%) as drift gas for IMS, the drift tube temperature was set at 45 deg.C.
Example 3
On the basis of the embodiment 1, the influence of the storage time on the quality of the Fotiaoqiang is determined by directly calculating the richness of aldehyde substances in the Fotiaoqiang samples with different storage times:
the comparative calculation of the evaluation of the richness of the aldehyde substances comprises the following formula I:
wherein, ynAnd y'nRespectively obtaining the content of the nth same aldehyde substance for the stored Fotiaoqiang sample and the non-stored Fotiaoqiang sample;
when the value of Y is less than n, the richness of the aldehyde substances in the stored Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang sample, and the richness of the aldehyde substances in the stored Fotiaoqiang sample is influenced. Detecting and calculating by taking trans-2-pentenal, furfural, myrobalal, n-hexanal, heptanal, trans-2-heptenal, benzaldehyde, trans-2-octenal, phenylacetaldehyde, n-octanal, nonanal and isovaleraldehyde as characteristic aldehyde substances. At this time, n has a value of 12.
The Y value can all be obtained to different fo tiao qiang samples, also can confirm the quality of different fo tiao qiang samples through the size of Y value.
Example 4
On the basis of the example 1, the influence of the storage time on the quality of the Fotiaoqiang is determined by directly calculating the richness of flavor substances in the Fotiaoqiang samples with different storage times:
the calculation of the flavor richness ratio comprises the following formula II:
wherein:
xmand x'mRespectively determining the content of the mth same flavor substance in the stored Fotiaoqiang sample and the content of the mth same flavor substance in the non-stored Fotiaoqiang sample;
when the numerical value of X is less than m, the richness of the flavor substances obtained by the Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang, and the richness of the flavor substances of the stored Fotiaoqiang is influenced;
the larger the X value obtained, the closer to the m value, which indicates that the influence of the corresponding storage time on the flavor substances of the Fotiaoqiang sample is smaller.
Example 5
On the basis of the example 1, the influence of the storage time on the quality of the Fotiaoqiang is determined by directly calculating the comprehensive comparison of the flavor substances of the Fotiaoqiang samples with different storage times;
the calculation of the comprehensive alignment comprises the formula three:
m is 0.6X +0.4Y, formula three;
wherein X and Y are obtained by the methods of example 4 and example 3, respectively;
when the M value is less than 0.6M +0.4n, the quality of the stored Fotiaoqiang sample is judged to be poor compared with the quality of the stored Fotiaoqiang sample. The larger the M value, the better the quality of the Fotiaoqiang sample.
Example 6
On the basis of example 1, the influence of storage time on the quality of the Fotiaoqiang sample is further evaluated by measuring the content of protein, the content of glutamic acid, arginine and alanine in the Fotiaoqiang sample, and measuring salty taste, umami taste, astringent taste and bitter aftertaste through an electronic tongue as evaluation indexes.
The following can be obtained through measurement:
1. in different storage periods, the content of glutamic acid in the detected amino acid is the highest, the percentage of glutamic acid in 1 week, 1 month, 3 months, 6 months, 9 months and 12 months is respectively 27.18%, 30.07%, 27.70%, 28.20%, 29.03% and 28.97%, and the glutamic acid is main umami amino acid and also is a main source presenting the delicate flavor of the Fotiaoqiang; and the shorter the storage period is, the higher the glutamic acid content of the Fotiaoqiang is. Wherein alanine is a sweet amino acid and arginine is a bitter amino acid, as shown in Table 2.
2. As shown in fig. 5: the sample with 1 week storage period has light salty taste, and the salty taste is partially accumulated along with the extension of the storage period; the fresh taste of the Fotiaoqiang is the most concentrated in the storage period of 1 week, the difference of the fresh taste is not obvious in the storage periods of 1 month, 3 months and 6 months, the concentration of the fresh taste is obviously weakened to the 9 th month, and the concentration of the fresh taste is the lowest in the storage period of 12 months. It is clear that the richness of the sample gradually decreases with the increase of the storage time, but the difference is not obvious when the storage period is 1, 3 and 6 months.
3. As shown in fig. 6: the abscissa and ordinate represent the bitterness and astringency of the sample, respectively, and the size of the bubbles represents the bitter aftertaste. Three parallels of the same sample are partially overlapped, and the sample has better parallelism; the bitter and astringent taste of the sample with the storage period of 1 week is the greatest when viewed from the horizontal and vertical coordinates; samples with storage periods of 1, 3, 6, 9, 12 months showed no significant difference in bitterness (p >0.05), while astringency decreased gradually with storage period. From the size of the bubbles, the bitterness and aftertaste of the sample stored for 1 week were the greatest, and as the time elapsed, the bubbles gradually decreased and the bitterness and aftertaste gradually decreased. In summary, the taste intensity such as the umami taste and the richness of the sample in the storage period of 1 week is higher, but the bitterness and the aftertaste are also larger, the total taste is richer, the umami taste and the richness of the sample are gradually weakened along with the extension of the storage period, and the bitterness is also reduced along with the extension of the storage period.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for analyzing the influence of storage time on the quality of a Fotiaoqiang is characterized by comprising the following steps:
s1 includes: storing the same Fotiaoqiang for different times below-18 ℃ respectively to obtain Fotiaoqiang samples corresponding to different storage times;
s2 includes: obtaining gas chromatography-ion mobility spectrograms of the Fotiaoqiang samples with different storage times through gas chromatography-ion mobility spectrometry;
s3 includes: extracting volatile substances of the Fotiaoqiang sample in different storage time to obtain the concentration change condition of all volatile organic compounds;
s4 includes: qualitatively analyzing all volatile organic compounds on a gas chromatography-ion mobility spectrogram of the Fotiaoqiang sample with different storage times to obtain dynamic change conditions of different types of volatile organic compounds in different storage times;
s5 includes: performing principal component analysis by taking all volatile substance peak intensities of the Fotiaoqiang samples in different storage times as analysis objects to determine the distribution condition of the principal components;
s6 determines the influence of the storage time on the quality of the Fotiaoqiang by the concentration change of all volatile organic compounds in steps S3-S5 under different storage times, the dynamic change of different types of volatile organic compounds under different storage times and the distribution condition of main components under different storage times.
2. The method of claim 1, wherein the method comprises the following steps:
in step S2, the detection conditions of the gas chromatograph-ion mobility spectrometer are as follows: automatic headspace sample introduction unit: the sample injection volume is 500 mu L, the incubation time is 15min, the incubation temperature is 80 ℃, the sample injection needle temperature is 85 ℃, and the incubation rotation speed is 500 rpm; a chromatographic column: FS-SE-54-CB-1 quartz capillary column (15m × 0.53mm, 0.5 μm), analysis time 30min, chromatographic column temperature 60 deg.C, carrier gas N2(the purity is more than or equal to 99.999%); IMS conditions: by using N2(purity 99.999%) as drift gas for IMS, the drift tube temperature was set at 45 deg.C.
3. The method of claim 1, wherein the method comprises the steps of: the method is characterized in that trans-2-pentenal, furfural, myrobalal, n-hexanal, heptanal, trans-2-heptenal, benzaldehyde, trans-2-octenal, phenylacetaldehyde, n-octanal, nonanal and isovaleraldehyde are used as characteristic aldehyde substances, and the influence of the storage time on the quality of the Fotiaoqiao is determined by determining the content of the characteristic aldehyde substances in the Fotiao samples at different storage times.
4. The method of claim 1, further comprising the steps of:
s7, comparing the richness of aldehyde substances in the Fotiaoqiang samples with different storage time to determine the influence of the storage time on the quality of the Fotiaoqiang:
the comparative calculation of the evaluation of the richness of the aldehyde substances comprises the following formula I:
wherein, ynAnd y'nRespectively obtaining the content of the nth same aldehyde substance of the stored Fotiaoqiang sample and the content of the nth same aldehyde substance of the stored Fotiaoqiang sample;
when the value of Y is less than n, the richness of the aldehyde substances in the stored Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang sample, and the richness of the aldehyde substances in the stored Fotiaoqiang sample is influenced.
5. The method of claim 1, further comprising the steps of:
s7, comparing the abundance of flavor substances of the Fotiaoqiang samples in different storage times to determine the influence of the storage time on the quality of the Fotiaoqiang;
the calculation of the flavor richness ratio comprises the following formula II:
wherein:
xmand x'mRespectively determining the content of the mth same flavor substance in the stored Fotiaoqiang sample and the content of the mth same flavor substance in the non-stored Fotiaoqiang sample;
when the numerical value of X is less than m, the richness of the flavor substances obtained by the Fotiaoqiang sample can be judged to be lower than that of the stored Fotiaoqiang, and the richness of the flavor substances of the stored Fotiaoqiang is influenced;
the larger the X value obtained, the closer to the m value, which indicates that the influence of the corresponding storage time on the flavor substances of the Fotiaoqiang sample is smaller.
6. The method of claim 1, further comprising the steps of:
s7, determining the influence of the storage time on the quality of the Fotiaoqiang by comprehensively comparing the flavor substances of the Fotiaoqiang samples in different storage times;
the calculation of the comprehensive alignment comprises the formula three:
m is 0.6X +0.4Y, formula three;
wherein X and Y are obtained according to the methods of formula two and formula one respectively;
when the M value is less than 0.6M +0.4n, the quality of the stored Fotiaoqiang sample is judged to be poor compared with the quality of the stored Fotiaoqiang sample.
7. The method of claim 1, further comprising the steps of: and determining the influence of the storage time on the quality of the Fotiaoqiang by measuring the protein in the Fotiaoqiang samples with different storage times.
8. The method of claim 1, further comprising the steps of: the influence of the storage time on the quality of the Fotiaoqiang is determined by measuring the amino acid composition condition and the corresponding taste activity value in the Fotiaoqiang sample with different storage times.
9. The method of claim 1, wherein the method comprises the following steps: the influence of the storage time on the quality of the Fotiaoqiang is determined according to the content of glutamic acid, arginine and alanine.
10. The method of claim 1, further comprising the steps of:
determining the influence of the storage time on the quality of the Fotiaoqiang according to the richness of the taste of the Fotiaoqiang in different storage times, wherein the taste comprises salty taste, delicate flavor, astringent taste and bitter aftertaste.
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