CN115047098A - Fingerprint spectrum analysis method for aroma components of different aromatized cigarette paper - Google Patents
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Abstract
The invention discloses a fingerprint spectrum analysis method of aroma components of different aromatized cigarette paper, which comprises the following steps: carrying out headspace sample injection treatment on different batches of aromatized cigarette paper samples produced by different paper mills, and then carrying out gas chromatography-ion mobility spectrometry analysis to obtain a multi-angle GC-IMS spectrogram; qualitatively analyzing volatile aroma substances according to the gas chromatography retention time and the ion migration time of aroma components in the spectrogram; carrying out GC-IMS fingerprint analysis on the aroma components according to the qualitative analysis result, and determining a characteristic peak area; and carrying out chemometric analysis according to the fingerprint analysis result. According to the fingerprint spectrum analysis method for the aroma components of different aromatized cigarette papers, provided by the invention, the HS-GC-IMS technology is combined with a chemometrics method to analyze the difference of aroma substances among different aromatized cigarette papers, so that theoretical basis and technical support are provided for the quality stability maintenance and identification of the aromatized cigarette paper products processed in different places.
Description
Technical Field
The invention relates to the technical field of quality evaluation of tobacco products, in particular to a fingerprint spectrum analysis method for aroma components of different aroma-giving cigarette paper.
Background
The cigarette paper (cigrette paper) is a thin-sheet paper specially used for wrapping tobacco to make cigarette, and is compact, soft and exquisite, and has higher longitudinal tensile strength, certain air permeability and proper burning speed. The cigarette paper is used as an important cigarette auxiliary material and is mainly characterized in that the cigarette paper directly participates in combustion during smoking. Therefore, although the mass proportion of the cigarette paper is small, the cigarette paper has great influence on the overall style and quality, the combustion performance and the chemical components of smoke. The cigarette auxiliary material 'three paper one rod' is one of the important means of cigarette perfuming, the perfuming cigarette paper is a functional material with perfuming and sweetening components added in the cigarette paper manufacturing process, and when the cigarette burns, the additive on the cigarette paper releases the fragrant components through volatilization, cracking and other modes to achieve the purpose of endowing the cigarette with certain characteristic fragrance.
In recent years, cigarette paper perfuming technology has been widely applied to high-end cigarette production. The red date essence microcapsule is proposed to achieve the effect of lasting slow release, and can effectively cover the impure gas of cigarettes and reduce the irritation of the cigarettes when being applied to cigarette paper, so that the smoke has sweet feeling and soft and fine smoke. The novel cigarette paper has natural herbaceous plant fragrance, can improve olfactory enjoyment, has the functions of moistening lung for removing phlegm, relieving cough and asthma, and can improve the smoking quality of cigarettes. The cigarette paper contains many substances, complex components and low content of aroma components.
At present, the technological processes of papermaking, perfuming and the like in the production process of the aromatized cigarette paper are basically outsourcing processing, the quality control system of the aromatized cigarette paper is not established, and the problems of difficult source tracing of the raw material of the aromatized cigarette paper, long detection time, insufficient stability monitoring method and the like exist, so that the quality stability of cigarette brands is influenced. And the existing GC/MS method in the national standard has the defects of specificity and insufficient sensitivity for detecting trace aroma compounds. Therefore, how to establish an accurate, efficient and convenient method for detecting the aroma components of the aromatized cigarette paper is a problem to be solved urgently by cigarette production and processing enterprises.
Therefore, a fingerprint spectrum analysis method for the aroma components of different aroma-giving cigarette paper is needed.
Disclosure of Invention
The invention aims to provide a fingerprint spectrum analysis method for aroma components of different aromatized cigarette papers, which solves the problems in the prior art, can analyze the difference of aroma substances among different aromatized cigarette papers, and provides theoretical basis and technical support for quality stability maintenance and identification of the aromatized cigarette paper products processed in different places.
The invention provides a fingerprint spectrum analysis method for aroma components of different aromatized cigarette paper, which comprises the following steps:
carrying out headspace sample injection treatment on different batches of aromatized cigarette paper samples produced by different paper mills, and then carrying out gas chromatography-ion mobility spectrometry to obtain multi-angle GC-IMS spectrograms of the aroma components of the aromatized cigarette paper samples;
performing qualitative analysis on volatile aroma substances in different aroma-giving cigarette paper samples according to gas chromatography retention time and ion migration time of aroma components of different aroma-giving cigarette paper in multi-angle GC-IMS spectrograms of the aroma components of the different aroma-giving cigarette paper samples;
performing GC-IMS fingerprint analysis on the aroma components of different batches of aroma-giving cigarette paper samples produced by different paper mills according to the qualitative analysis result of the volatile aroma-giving substances, and determining the characteristic peak areas of the aroma-giving cigarette paper samples produced by different paper mills;
according to the GC-IMS fingerprint analysis results of different aromatizing cigarette paper samples, carrying out stoichiometric analysis on the aroma components of the different aromatizing cigarette paper samples so as to distinguish the aromatizing cigarette paper samples of different paper mills.
The fingerprint analysis method for the aroma components of different aromatized cigarette paper as described above, wherein preferably, after the headspace sampling treatment is performed on different batches of aromatized cigarette paper samples produced by different paper mills, the gas chromatography-ion mobility spectrometry analysis is performed to obtain the multi-angle GC-IMS spectrogram of the aroma components of different aromatized cigarette paper samples, specifically comprising:
pre-treating a sample, namely accurately weighing 0.500g of an aromatized cigarette paper sample at room temperature, placing the aromatized cigarette paper sample in a 20mL screw-top empty bottle, incubating at 90 ℃ for 20min, and then introducing the sample, wherein each sample is subjected to parallel test for 3 times;
carrying out headspace sampling treatment by an automatic headspace sampler carried by a GC-IMS flavor analyzer;
detecting different cigarette paper samples by adopting a GC-IMS flavor analyzer, and repeatedly carrying out sample injection measurement on each sample for 3 times to obtain gas chromatography series ion mobility spectrums of aroma components of the different cigarette paper samples;
and analyzing the gas chromatography series ion mobility spectrometry of the aroma components of different aroma-endowing cigarette paper samples by using LAV software to obtain multi-angle GC-IMS spectrograms of the aroma components of the different aroma-endowing cigarette paper samples.
In the above method for analyzing fingerprint patterns of aroma components of different aroma-providing cigarette papers, preferably, during the headspace sample injection treatment, the conditions of the automatic headspace sample injector are as follows: incubating the headspace bottle with the sample for 20 min; the incubation temperature is 90 ℃; the sample injection volume is 200 mu l; the temperature of a sample injection needle is 95 ℃; the incubation speed was 500 rpm.
In the method for analyzing the fingerprint spectrum of the aroma components of the different aromatized cigarette papers, preferably, when the GC-IMS flavor analyzer is used for detecting different aromatized cigarette paper samples, the analysis conditions of the gas chromatography are that the analysis time is as follows: 20min, column type: FS-SE-54-CB-1, the column length is 15m, the inner diameter ID is-0.53 mm, the film thickness is 1 μm, and the chromatographic column temperature is 60 ℃;
the gas chromatography gradient program was: when the sample introduction time is 0-2min, the flow rate of the carrier gas is 2 mL/min; when the sample introduction time is 2-20min, the flow rate of the carrier gas is 10 mL/min; when the sample injection time is 20-30min, the carrier gas flow rate is 100mL/min, and the drift gas flow rate of each sample injection time is 150 mL/min;
the ion mobility spectrometry conditions are as follows: the length of the drift tube is 98 mm; linear voltage in the tube is 500V/cm; the drift tube temperature is 45 ℃; the carrier/drift gas is nitrogen; drift gas flow rate 150 mL/min; a radioactive source: beta rays; ionization mode: a positive ion.
The fingerprint spectrum analysis method for the aroma components of different cigarette paper with different aromatizing properties, as described above, preferably, the LAV software is used to analyze the gas chromatography tandem ion mobility spectrometry of the aroma components of different cigarette paper samples with different aromatizing properties to obtain the multi-angle GC-IMS spectrogram of the aroma components of different cigarette paper samples, which specifically includes:
analyzing gas chromatography series ion mobility spectrometry of the aroma components of different aroma-added cigarette paper samples by using LAV software to obtain GC-IMS three-dimensional comparison spectrograms of the aroma components of the different aroma-added cigarette paper samples;
reducing the dimension of GC-IMS three-dimensional comparison spectrograms of different aromatized cigarette paper samples by using LAV software to obtain two-dimensional spectrogram top views of the different aromatized cigarette paper samples;
and (3) applying LAV software, taking the spectrogram of one sample as a reference, and comparing the top views of the two-dimensional spectrograms of different aromatizing cigarette paper samples by adopting a difference comparison mode so as to compare the difference in the content of the aroma substances among different samples.
The fingerprint analysis method for the aroma components of different aromatized cigarette papers as described above, wherein preferably, the qualitative analysis of the volatile aroma substances in different aromatized cigarette paper samples is performed according to the gas chromatography retention time and the ion migration time of the aroma components of different aromatized cigarette papers in the multi-angle GC-IMS spectrogram of the aroma components of different aromatized cigarette paper samples, which specifically comprises:
and carrying out qualitative analysis on volatile aroma components in different aroma-giving cigarette paper samples by adopting GC-IMS Library Search V2.2.1 qualitative analysis software and utilizing a built-in NIST database and an IMS database according to the gas chromatography retention time and the ion migration time of the aroma components of different aroma-giving cigarette paper in gas phase ion migration spectrograms of different aroma-giving cigarette paper samples.
In the fingerprint analysis method of the aroma components of different aroma-providing cigarette papers as described above, preferably, in the qualitative analysis of the volatile aroma-providing substances in the samples of different aroma-providing cigarette papers, common aroma-providing substances are detected from different aroma-providing cigarette papers, and the identified common aroma-providing substances include alcohol compounds, ketone compounds, aldehyde compounds and ester compounds.
The method for analyzing the fingerprint of the aromatic components of different aromatic cigarette paper as described above, wherein preferably, the GC-IMS fingerprint analysis is performed on the aromatic components of different batches of aromatic cigarette paper samples produced by different paper mills according to the qualitative analysis result of the volatile aromatic substance, so as to determine the characteristic peak areas of the aromatic cigarette paper samples produced by different paper mills, specifically comprising:
and analyzing GC-IMS two-dimensional spectrograms of different aromatizing cigarette paper samples in a Gallery plot view mode of LAV software, repeating each experiment for 3 times to obtain a fingerprint spectrum automatically generated by all detectable signal peaks in the GC-IMS two-dimensional spectrogram so as to compare the change conditions of aromatizing component compounds of aromatizing cigarette paper of different batches produced by different paper mills.
The fingerprint analysis method for the aroma components of different aromatized cigarette paper as described above, wherein preferably, the method for performing chemometric analysis on the aroma components of different aromatized cigarette paper samples according to the GC-IMS fingerprint analysis results of the different aromatized cigarette paper samples to distinguish the aromatized cigarette paper samples of different paper mills, specifically comprises:
and (3) analyzing the aromatized cigarette paper samples produced by different paper mills by adopting a principal component analysis method and a partial least squares regression analysis method to obtain the distribution rule of corresponding areas of the aromatized cigarette paper samples of different batches of the same manufacturer and the aromatized cigarette paper samples of different manufacturers so as to distinguish the cigarette paper samples produced by different paper mills.
The fingerprint analysis method of the aroma components of different aromatized cigarette papers is preferably characterized in that the data preprocessing method corresponding to the principal component analysis is UV scaling; and (3) performing partial least square discriminant analysis on the number of corresponding reserved latent variables: 5; and (3) cross validation: leaving one method; data preprocessing: UV scaling.
The invention provides a fingerprint analysis method for aroma components of different aromatized cigarette paper, the HS-GC-IMS technology is combined with a chemometrics method to analyze the difference of aroma substances among different aromatized cigarette paper, and theoretical basis and technical support are provided for the quality stability maintenance and identification of the aromatized cigarette paper products processed in different places; the differences of the aroma components of 23 different manufacturers of the same variety and different batches of aroma-providing cigarette paper samples are researched by adopting a headspace-gas chromatography-ion mobility spectrometry combined method; taking 23 different batches of flavored cigarette paper samples produced by 3 different cigarette paper processing enterprises of the same variety as experimental objects, acquiring and trace analyzing the fragrant substances in the cigarette paper by adopting an HS-GC-IMS technology, comparing the difference of the content of the fragrant substances among different cigarette paper by establishing a fingerprint, evaluating the product stability among different production plants of a multi-point processing variety in a data visualization mode by utilizing principal component analysis and partial least squares regression analysis, and providing theoretical basis and data support for monitoring the change of the fragrant components of the flavored cigarette paper and tracing identification; 65 common aroma substances are detected from different aroma cigarette paper, identified dimer aroma substances of 29 monomers and partial substances are identified, but the contents of different compounds have certain difference; the research of data visualization form is carried out through fingerprint analysis, so that the components of the aroma substances of cigarette paper samples of different batches are approximately the same, but the content of the characteristic aroma components of the samples of different manufacturers is different; through principal component analysis and partial least squares regression analysis and evaluation, cigarette paper samples of different manufacturers can be well separated, and traceability identification of products of different processing manufacturers is facilitated; the method has the advantages of high sensitivity, less sample loss, convenient operation and high analysis efficiency; the HS-GC-IMS technology is combined with a chemometrics method, so that the defects of the existing detection means can be made up, the difference of aroma substances among complex systems of the aromatized cigarette paper can be analyzed, and the method has a positive promoting effect on the quality stability maintenance and new product development of the aromatized cigarette paper products of multi-point processing varieties.
Drawings
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described with reference to the accompanying drawings, in which:
FIG. 1 is a flow chart of an embodiment of a fingerprint analysis method for the aroma components of different aromatized cigarette papers provided by the present invention;
FIG. 2 is a three-dimensional GC-IMS spectrogram of the aroma components of different aromatized cigarette paper;
FIG. 3 is a gas phase ion mobility spectrum of different flavored cigarette paper samples;
FIG. 4 is a difference diagram of gas phase ion mobility spectra with cigarette paper sample FXJYZ10-03 as reference;
FIG. 5 is a qualitative result of the volatile components of the cigarette paper sample;
FIG. 6 is a GC-IMS fingerprint of the aroma component of the aromatized cigarette paper;
FIG. 7 is a graph of PCA analysis of GC-IMS data for an aromatized cigarette paper sample;
FIG. 8 is a plot of PLS-DA pattern recognition scores for GC-IMS data for an aromatized cigarette paper sample.
Detailed Description
Various exemplary embodiments of the present disclosure will now be described in detail with reference to the accompanying drawings. The description of the exemplary embodiments is merely illustrative and is in no way intended to limit the disclosure, its application, or uses. The present disclosure may be embodied in many different forms and is not limited to the embodiments described herein. These embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. It should be noted that: the relative arrangement of parts and steps, the composition of materials, numerical expressions and numerical values set forth in these embodiments are to be construed as merely illustrative, and not as limitative, unless specifically stated otherwise.
As used in this disclosure, "first", "second": and the like, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element preceding the word covers the element listed after the word, and does not exclude the possibility that other elements are also covered. "upper", "lower", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
In the present disclosure, when a specific component is described as being located between a first component and a second component, there may or may not be intervening components between the specific component and the first component or the second component. When it is described that a specific component is connected to other components, the specific component may be directly connected to the other components without having an intervening component, or may be directly connected to the other components without having an intervening component.
All terms (including technical or scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs unless specifically defined otherwise. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate.
As shown in fig. 1, the fingerprint analysis method for the aroma components of different aromatized cigarette papers provided in this embodiment specifically includes, in an actual implementation process:
and S1, performing headspace sample injection treatment on different batches of aromatized cigarette paper samples produced by different paper mills, and performing gas chromatography-ion mobility spectrometry to obtain multi-angle GC-IMS spectrograms of the aroma components of the aromatized cigarette paper samples.
In one embodiment, 8 batches of flavored cigarette paper samples (FXJYZ 10-01-08) produced by a paper mill A, 10 batches of flavored cigarette paper samples (FXJYZ 11-01-10) produced by a paper mill B and 5 batches of flavored cigarette paper samples (FXJYZ 14-01-05) produced by a paper mill C are selected for gas chromatography-ion mobility spectrometry.
In an embodiment of the method for analyzing fingerprint spectrums of aroma components of different aromatized cigarette papers of the present invention, the step S1 may specifically include:
step S11, preprocessing the sample, accurately weighing 0.500g (accurate to 0.001g) of the aromatized cigarette paper sample at room temperature, placing the aromatized cigarette paper sample in a 20mL screw-top empty bottle, incubating for 20min at 90 ℃, then injecting samples, and simultaneously performing 3 parallel tests on each sample.
Wherein the screw top hollow bottle is a precise dark brown screw top hollow bottle with the model of 22.5 multiplied by 75.5mm produced by HAMAG company in China.
And step S12, performing headspace sampling treatment by an automatic headspace sampler carried by the GC-IMS flavor analyzer.
Wherein, when the headspace advances a kind and handles, automatic headspace injector condition is: incubating the headspace bottle with the sample for 20 min; the incubation temperature is 90 ℃; the sample injection volume is 200 mu l; the temperature of a sample injection needle is 95 ℃; the incubation speed was 500 rpm.
And S13, respectively detecting different aromatized cigarette paper samples by adopting a GC-IMS flavor analyzer, and repeatedly injecting and measuring each sample for 3 times to obtain gas chromatography series ion mobility (GC-IMS) spectrums of the aroma components of the different aromatized cigarette paper samples.
Illustratively, detection can be performed using a FlavourSpec GC-IMS flavor analyzer from g.a.s. germany, with a CTC autostop injector. The invention does not specifically limit the manufacturer and model of the GC-IMS flavor analyzer.
The GC-IMS combines the advantages of high separation degree of gas chromatography and high sensitivity of ion mobility spectrometry, can quickly detect trace volatile organic compounds in a sample without any special sample pretreatment, and is used for measuring volatile headspace components in a solid or liquid sample.
The Ion Mobility Spectrometry (IMS) technology has good qualitative and semi-quantitative analysis capability, can provide more qualitative and quantitative information than a spectrum, and can be used as a tool for developing basic research, stability analysis and fingerprint analysis of flavor and fragrance chemicals. The headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) combines the advantages of high separation efficiency of gas chromatography and high sensitivity of ion mobility spectrometry, is simple and convenient to operate without any special sample pretreatment, can quickly measure trace volatile components in solid or liquid samples, can perform qualitative analysis on substances by combining an NIST database and an IMS database, and has high visualization degree. The method is suitable for trace analysis and detection of volatile and semi-volatile substances.
When the GC-IMS flavor analyzer is adopted to detect different aromatized cigarette paper samples, the gas chromatography analysis conditions are analysis time: 20min, column type: FS-SE-54-CB-1, wherein the column length is 15m, the inner diameter ID is-0.53 mm, the film thickness is 1 mu m, and the chromatographic column temperature is 60 ℃;
the gas chromatography gradient program was: when the sample introduction time is 0-2min, the flow rate of the carrier gas is 2 mL/min; when the sample introduction time is 2-20min, the flow rate of the carrier gas is 10 mL/min; when the sample introduction time is 20-30min, the flow rate of the carrier gas is 100mL/min, and the drift gas flow rate of each sample introduction time is 150 mL/min;
the ion mobility spectrometry conditions are as follows: the length of the drift tube is 98 mm; linear voltage in the tube is 500V/cm; the drift tube temperature is 45 ℃; the carrier/drift gas is nitrogen; drift gas flow rate 150 mL/min; a radioactive source: beta rays; ionization mode: a positive ion.
Step S14, analyzing the gas chromatography tandem ion mobility spectrometry of the aroma components of different aroma-providing cigarette paper samples by using LAV (laboratory analytical viewer) software to obtain multi-angle GC-IMS spectrograms of the aroma components of the different aroma-providing cigarette paper samples.
In an embodiment of the method for analyzing fingerprint spectrums of aroma components of different aromatized cigarette papers of the present invention, the step S14 may specifically include:
and step S141, analyzing the gas chromatography tandem ion mobility spectrometry of the aroma components of different aroma-endowing cigarette paper samples by using LAV software to obtain GC-IMS three-dimensional comparison spectrograms of the aroma components of the different aroma-endowing cigarette paper samples.
8 different cigarette paper samples are selected to be subjected to rapid analysis of gas chromatography tandem ion mobility spectrometry (GC-IMS), and FIG. 2 is a GC-IMS three-dimensional comparison spectrogram of aroma components of the different cigarette paper samples obtained according to LAV software analysis. From fig. 2, it can be observed visually that: the types of volatile organic compounds are relatively close among different samples.
And S142, performing dimension reduction treatment on GC-IMS three-dimensional comparison spectrograms of different aromatized cigarette paper samples by using LAV software to obtain two-dimensional spectrogram top views of the different aromatized cigarette paper samples.
In order to facilitate the transverse comparison and analysis among the samples, the three-dimensional spectrogram of each sample is subjected to dimension reduction treatment to obtain a two-dimensional spectrogram top view shown in fig. 3 for difference comparison. In fig. 3, the abscissa represents the migration time of the fragrant substance with respect to the reactive ion peak at IMS separation, the ordinate represents the retention time of the fragrant substance at GC separation, the vertical line at 1.0 of the abscissa represents the Reactive Ion Peak (RIP) peak, and each point on both sides of the RIP peak represents a fragrant substance. The concentration of the substance is represented by color, with light colors indicating lower concentrations, dark colors indicating higher concentrations, and darker colors indicating higher concentrations of the aroma-forming substance. The results show that: the normalized migration time was 4.48ms, where the majority of organic material had completed efficient migration at 200-.
And S143, using LAV software, taking a spectrogram of one sample as a reference, and comparing two-dimensional spectrogram top views of different aromatizing cigarette paper samples by adopting a difference comparison mode to compare the difference in the content of the aroma substances among different samples.
In order to more clearly compare the difference in the content of the fragrant substance between the different samples, a difference comparison mode was used, and fig. 4 was obtained. And selecting the spectrogram of the FXJYZ10-03 sample as a reference, deducting the reference from the spectrograms of other 7 samples, wherein if the two volatile organic compounds are consistent, the background after deducting is faded to be white, the dark color represents that the concentration of the substance is higher than that of the reference sample, and the light color represents that the concentration of the substance is lower than that of the reference sample. As can be seen from fig. 4: different aroma substances in 8 cigarette paper samples have different GC-IMS spectral characteristic information. Wherein the samples FXJYZ10-05 and FXJYZ10-07 of the same manufacturer A are relatively similar to the reference sample FXJYZ10-03 in whole; the species and contents of the aroma compounds of the 3 samples FXJYZ11-06, FXJYZ11-04 and FXJYZ11-08 of the manufacturer B are relatively similar, and the color of the aroma compounds drifting in the vicinity of the retention time of 200s compared with the reference sample FXJYZ10-03 is remarkably changed. The aroma-forming compounds of the samples FXJYZ14-01 and FXJYZ14-04 of manufacturer C were similar to the 3 samples of manufacturer B, and were also significantly different from the aroma-forming compounds of the reference sample FXJYZ10-03 in the vicinity of the retention time of 200 s.
And step S2, carrying out qualitative analysis on volatile aroma substances in different aroma-endowing cigarette paper samples according to the gas chromatography retention time and the ion migration time of the aroma components of different aroma-endowing cigarette paper in the multi-angle GC-IMS spectrograms of the aroma components of different aroma-endowing cigarette paper samples.
Specifically, GC-IMS Library Search V2.2.1 qualitative analysis software is adopted, a built-in NIST database and an IMS database are utilized, and according to the gas chromatography retention time and the ion migration time of aroma components of different aromatized cigarette paper in gas phase ion migration spectrograms of different aromatized cigarette paper samples, the volatile aroma components in different aromatized cigarette paper samples are subjected to qualitative analysis.
Specifically, according to the retention time and the ion migration time of the gas chromatography of the aroma components of the aromatized cigarette paper, the volatile aroma substances in 23 different aromatized cigarette paper samples are qualitatively analyzed by combining an IMS database matched with an instrument. As shown in fig. 5, each point marked with a number represents a substance that is characterized. The qualitative analysis results of the fragrant substances are shown in table 1, and the numbers in fig. 5 correspond to the fragrant substances in table 1 one to one.
TABLE 1 qualitative analysis of gas phase ion mobility spectrogram of cigarette paper sample
In the qualitative analysis of volatile aroma substances in different cigarette paper samples, common aroma substances are detected from different cigarette paper, and the identified common aroma substances can be identified to comprise alcohol compounds, ketone compounds, aldehyde compounds and ester compounds.
From the qualitative analysis results of fig. 5 and table 1, it can be seen that: a total of 65 odoriferous substances were detected in each of the cigarette papers, and among them, 29 monomers and a dimer of partial substances were identified. The 29 kinds of fragrant substances are mainly compounds such as alcohols, ketones, aldehydes and esters. These substances are important aroma components in the aromatized cigarette paper and impart different style characteristics to the cigarette paper. The 29 compounds were subjected to a categorical statistical analysis. The results show that: the most various aroma substances are alcohols and ketones, and there are 7 kinds of aroma substances. The alcohol has the effects of moistening and improving the fragrance of tobacco in the smoking process of the cigarette, so that the mainstream smoke of the cigarette is fine, soft and rich in concentration. The ketone substances have strong influence on the smoking taste, aroma and satisfaction of the cigarettes, and can coordinate the cigarette aroma, cover up miscellaneous gas and endow the cigarettes with different characteristic aroma. In addition, the cigarette paper also contains 5 aldehydes, 4 esters, 1 acid and 5 dimers. The substances are main sources for forming the aroma characteristics of the aromatized cigarette paper, and the content difference of the substances has important influence on the style characteristics of the aroma of the aromatized cigarette paper and is an important index for controlling the internal quality of the aromatized cigarette paper. Among them, butyl acetate has a pleasant fruity odor. The furoic acid methyl ester has strong fruit fragrance and baking fragrance, is coordinated with the tobacco fragrance, and can enhance the fullness of the smoke and cover up miscellaneous gas. Benzaldehyde has the aroma of almonds, cherries and nuts. Octanal has a light, fresh, sweet orange peel odor. Nonanal, also known as geranial, is naturally present in rose oil, citrus oil, lime oil and clary sage oil, with a rose-like, citrus-like aroma. The 1-hexanol has fruity fragrance and is used for preparing coconut and berry essences. The beta-damascenone can generate cool and pleasant green fragrance and strong rose fragrance, has soft fragrance, is light and transparent, and has an important effect on improving the fragrance of cigarettes.
And step S3, performing GC-IMS fingerprint analysis on the aroma components of different batches of aroma-giving cigarette paper samples produced by different paper mills according to the qualitative analysis result of the volatile aroma-giving substances, and determining the characteristic peak areas of the aroma-giving cigarette paper samples produced by different paper mills.
Specifically, GC-IMS two-dimensional spectrograms of different aromatized cigarette paper samples are analyzed in a Gallery plot mode of LAV software, each experiment is repeated for 3 times, and fingerprint spectrums automatically generated by all detectable signal peaks in the GC-IMS two-dimensional spectrograms are obtained so as to compare the change conditions of aromatized component compounds of different batches of aromatized cigarette paper produced by different paper mills.
In order to further comprehensively compare the change conditions of aroma component compounds of different manufacturers and different batches of aroma-giving cigarette paper, 23 aroma-giving cigarette paper samples are analyzed in a Gallery plot mode of LAV software, each experiment is repeated for 3 times, and all fingerprint spectrums automatically generated by detectable signal peaks in a GC-IMS two-dimensional spectrum are obtained, and the result is shown in figure 6. In the figure, the abscissa is a detection signal peak of the fragrant substance in the sample, and the ordinate is the sample number. As can be seen from the fingerprint spectrum of FIG. 6, the samples of the aromatized cigarette paper of different batches of the same manufacturer have obvious similarity, and the main difference is the concentration. The cigarette paper samples of different manufacturers show obvious difference, and the aroma substances of the samples have respective characteristic peak areas and also have common similar areas. Wherein 18 aroma components in the area A are rich in cigarette paper samples produced by the manufacturer A, the characteristic compounds are more prominent and are different from other two samples, and the area A can be used as a characteristic peak area of the cigarette paper samples produced by the manufacturer A. The 24 components in the area B are relatively higher in the cigarette paper sample produced by the manufacturer B and can be used as the characteristic aroma marker of the aromatized cigarette paper of the manufacturer B. The 14 aroma components in the area C are obviously increased and can be used as the characteristic aroma marker of the aromatized cigarette paper of a C manufacturer.
And S4, performing chemometric analysis on aroma components of different aroma-giving cigarette paper samples according to GC-IMS fingerprint analysis results of the different aroma-giving cigarette paper samples so as to distinguish the aroma-giving cigarette paper samples of different paper mills.
The data were subjected to principal component analysis and partial least squares regression analysis using model lab Matman general chemometrics solution software. The GC-IMS fingerprint data of different aromatized cigarette paper samples are led into ModelLab Matman software for chemometric analysis, and in the invention, the chemometric modeling analysis software can be, for example, ModelLab Matman scientific big data system solution software 2021 version of Chinese Chemmind Technologies.
Specifically, the main component analysis (PCA) and partial least squares regression (PLS) are adopted to analyze the cigarette paper samples produced by different paper mills, so as to obtain the distribution rules of the corresponding areas of the cigarette paper samples of different batches of the same manufacturer and the cigarette paper samples of different manufacturers, so as to distinguish the cigarette paper samples produced by different paper mills, and thus, the difference of the aroma components of the cigarette paper of different manufacturers can be analyzed and compared more intuitively.
Wherein, the data preprocessing method corresponding to the principal component analysis is UV scaling; and (3) performing partial least square discriminant analysis on the number of corresponding reserved latent variables: 5; and (3) cross validation: leaving one method; data preprocessing: UV scaling.
In the specific implementation, the result of distinguishing the aromatized cigarette paper samples of 3 manufacturers by adopting Principal Component Analysis (PCA) is shown in fig. 7, and 2 principal components are selected for analysis after the software system is automatically fitted, wherein the contribution rate of the 1 st principal component is 51.29%, the contribution rate of the 2 nd principal component is 15.86%, and the cumulative contribution rate of the 2 principal components reaches 67.15%, which indicates that the different aromatized cigarette paper samples are well classified. After the characteristic variables in the cigarette paper sample are processed by PCA, the characteristic variables can be directly observed through a two-dimensional plane data point distribution diagram: the cigarette paper samples of the same manufacturer and different batches basically show aggregation distribution, and have better area attribute, and the areas of the samples of different manufacturers do not overlap, which shows that the cigarette paper samples of different manufacturers can be well separated, and the characteristic aroma substances of the samples have certain difference.
The class 3 samples were further analyzed using Partial Least Squares Discriminant Analysis (PLSDA) algorithm. As can be seen from figure 8, the PLS-DA score plots suggest significant differences in the volatile compound composition of the wrapper and show that the 3 samples were well differentiated without exceeding the tolling's T295% confidence interval (shown by the oval) with a recognition rate of between 99% and 100%. The method shows that different cigarette paper samples with different aromatizing functions are well clustered, and can be used for remarkably distinguishing cigarette paper samples of different manufacturers.
The invention adopts GC-IMS Library Search V2.2.1 qualitative analysis software, and carries out qualitative analysis on the aroma substances in the samples by utilizing a built-in NIST database and an IMS database. Combining a Gallery Plot plug-in and a Reporter plug-in, applying LA software to analyze and process data in multiple angles to obtain two-dimensional and three-dimensional spectrograms, and comparing and analyzing aroma component differences among different samples according to the fingerprint spectrogram.
According to the fingerprint spectrum analysis method for the aroma components of different aromatized cigarette papers provided by the embodiment of the invention, the HS-GC-IMS technology is combined with a chemometrics method to analyze the difference of aroma substances among different aromatized cigarette papers, so that a theoretical basis and a technical support are provided for the quality stability maintenance and identification of the aromatized cigarette paper products processed in different places; the differences of the aroma components of 23 different manufacturers of the same variety and different batches of aroma-providing cigarette paper samples are researched by adopting a headspace-gas chromatography-ion mobility spectrometry combined method; taking 23 different batches of aromatized cigarette paper samples of the same variety produced by 3 different cigarette paper processing enterprises as experimental objects, adopting HS-GC-IMS technology to collect and perform trace analysis on aroma substances in the cigarette paper, comparing the difference of the content of the aroma substances between different cigarette papers by establishing a fingerprint, evaluating the product stability between different production plants of the multi-point processed variety in a data visualization mode by utilizing principal component analysis and partial least squares regression analysis, and providing theoretical basis and data support for monitoring the aroma component change and tracing identification of the aromatized cigarette paper; detecting 65 common aroma substances from different aromatized cigarette paper, and identifying the identified dimer aroma substances of 29 monomers and partial substances, wherein the contents of different compounds have certain difference; data visualization form research is carried out through fingerprint analysis, so that the components of the aroma substances of different batches of cigarette paper samples are approximately the same, but the content of the characteristic aroma components of the samples of different manufacturers has certain difference; through principal component analysis and partial least squares regression analysis and evaluation, cigarette paper samples of different manufacturers can be well separated, and traceability identification of products of different processing manufacturers is facilitated; the method has the advantages of high sensitivity, less sample loss, convenient operation and high analysis efficiency; the HS-GC-IMS technology is combined with a chemometrics method, so that the defects of the existing detection means can be made up, the difference of aroma substances among complex systems of the aroma-providing cigarette paper can be analyzed, and the method has a positive promoting effect on the quality stability maintenance and new product development of the aroma-providing cigarette paper of multi-point processing varieties.
Thus, various embodiments of the present disclosure have been described in detail. Some details that are well known in the art have not been described in order to avoid obscuring the concepts of the present disclosure. It will be fully apparent to those skilled in the art from the foregoing description how to practice the presently disclosed embodiments.
Although some specific embodiments of the present disclosure have been described in detail by way of example, it should be understood by those skilled in the art that the foregoing examples are for purposes of illustration only and are not intended to limit the scope of the present disclosure. It will be understood by those skilled in the art that various changes may be made in the above embodiments or equivalents may be substituted for elements thereof without departing from the scope and spirit of the present disclosure. The scope of the present disclosure is defined by the appended claims.
Claims (10)
1. A fingerprint spectrum analysis method for aroma components of different aromatized cigarette paper is characterized by comprising the following steps:
carrying out headspace sample injection treatment on different batches of aromatized cigarette paper samples produced by different paper mills, and then carrying out gas chromatography-ion mobility spectrometry to obtain multi-angle GC-IMS spectrograms of the aroma components of the aromatized cigarette paper samples;
performing qualitative analysis on volatile aroma substances in different aroma-giving cigarette paper samples according to gas chromatography retention time and ion migration time of aroma components of different aroma-giving cigarette paper in multi-angle GC-IMS spectrograms of the aroma components of the different aroma-giving cigarette paper samples;
performing GC-IMS fingerprint analysis on the aroma components of different batches of aroma-giving cigarette paper samples produced by different paper mills according to the qualitative analysis result of the volatile aroma-giving substances, and determining the characteristic peak areas of the aroma-giving cigarette paper samples produced by different paper mills;
according to the GC-IMS fingerprint analysis results of different aromatizing cigarette paper samples, carrying out stoichiometric analysis on the aroma components of the different aromatizing cigarette paper samples so as to distinguish the aromatizing cigarette paper samples of different paper mills.
2. The fingerprint spectrum analysis method for the aroma components of different aromatized cigarette paper according to claim 1, wherein the multi-angle GC-IMS spectrogram of the aroma components of different aromatized cigarette paper samples is obtained by performing gas chromatography-ion mobility spectrometry after headspace sample injection treatment on different batches of aromatized cigarette paper samples produced by different paper mills, and specifically comprises the following steps:
pre-treating a sample, namely accurately weighing 0.500g of an aromatized cigarette paper sample at room temperature, placing the aromatized cigarette paper sample in a 20mL screw-top empty bottle, incubating at 90 ℃ for 20min, and then introducing the sample, wherein each sample is subjected to parallel test for 3 times;
carrying out headspace sample injection treatment by an automatic headspace sample injector of a GC-IMS flavor analyzer;
detecting different cigarette paper samples by adopting a GC-IMS flavor analyzer, and repeatedly carrying out sample injection measurement on each sample for 3 times to obtain gas chromatography series ion mobility spectrums of aroma components of the different cigarette paper samples;
and analyzing the gas chromatography series ion mobility spectrometry of the aroma components of different aroma-endowing cigarette paper samples by using LAV software to obtain multi-angle GC-IMS spectrograms of the aroma components of the different aroma-endowing cigarette paper samples.
3. The fingerprint analysis method for the aroma components of different aromatized cigarette papers according to claim 2, wherein during headspace sample injection treatment, the conditions of the automatic headspace sample injector are as follows: incubating the headspace bottle with the sample for 20 min; the incubation temperature is 90 ℃; the sample injection volume is 200 mu l; the temperature of a sample injection needle is 95 ℃; the incubation speed was 500 rpm.
4. The fingerprint analysis method for the aroma components of different aromatized cigarette paper according to claim 2, wherein when the GC-IMS flavor analyzer is adopted to detect different aromatized cigarette paper samples, the gas chromatography analysis conditions are analysis time: 20min, column type: FS-SE-54-CB-1, the column length is 15m, the inner diameter ID is-0.53 mm, the film thickness is 1 μm, and the chromatographic column temperature is 60 ℃;
the gas chromatography gradient program was: when the sample introduction time is 0-2min, the flow rate of the carrier gas is 2 mL/min; when the sample introduction time is 2-20min, the flow rate of the carrier gas is 10 mL/min; when the sample introduction time is 20-30min, the flow rate of the carrier gas is 100mL/min, and the drift gas flow rate of each sample introduction time is 150 mL/min;
the ion mobility spectrometry conditions are as follows: the length of the drift tube is 98 mm; linear voltage in the tube is 500V/cm; the drift tube temperature is 45 ℃; the carrier/drift gas is nitrogen; drift gas flow rate 150 mL/min; the radioactive source: beta rays; ionization mode: a positive ion.
5. The fingerprint analysis method of the aroma components of different aromatized cigarette paper according to claim 2, wherein the LAV software is used for analyzing the gas chromatography tandem ion mobility spectrometry of the aroma components of different aromatized cigarette paper samples to obtain multi-angle GC-IMS spectrograms of the aroma components of the different aromatized cigarette paper samples, which specifically comprises the following steps:
analyzing gas chromatography series ion mobility spectrometry of the aroma components of different aroma-endowing cigarette paper samples by using LAV software to obtain GC-IMS three-dimensional comparison spectrograms of the aroma components of the different aroma-endowing cigarette paper samples;
reducing the dimension of GC-IMS three-dimensional comparison spectrograms of different aromatized cigarette paper samples by using LAV software to obtain two-dimensional spectrogram top views of the different aromatized cigarette paper samples;
and (3) applying LAV software, taking the spectrogram of one sample as a reference, and comparing the top views of the two-dimensional spectrograms of different aromatizing cigarette paper samples by adopting a difference comparison mode so as to compare the difference in the content of the aroma substances among different samples.
6. The fingerprint analysis method for the aroma components of different aromatized cigarette papers according to claim 1, wherein the qualitative analysis of the volatile aroma substances in different aromatized cigarette paper samples is carried out according to the gas chromatography retention time and the ion migration time of the aroma components of different aromatized cigarette papers in the multi-angle GC-IMS spectrogram of the aroma components of different aromatized cigarette paper samples, which specifically comprises the following steps:
and carrying out qualitative analysis on volatile aroma components in different aromatized cigarette paper samples by adopting GC-IMS Library Search V2.2.1 qualitative analysis software and utilizing a built-in NIST database and an IMS database according to the gas chromatography retention time and the ion migration time of the aroma components of different aromatized cigarette paper in gas phase ion migration spectrograms of different aromatized cigarette paper samples.
7. The fingerprint analysis method for the aroma components of the different aromatized cigarette papers according to claim 6, wherein in the qualitative analysis of the volatile aroma components in the different aromatized cigarette paper samples, common aroma components are detected from the different aromatized cigarette papers, and the identifiable and identified common aroma components comprise alcohol compounds, ketone compounds, aldehyde compounds and ester compounds.
8. The fingerprint analysis method for the aroma components of different aromatized cigarette papers according to claim 5, wherein the GC-IMS fingerprint analysis is performed on the aroma components of different batches of aromatized cigarette paper samples produced by different paper mills according to the qualitative analysis result of the volatile aroma components, so as to determine the characteristic peak areas of the aromatized cigarette paper samples produced by different paper mills, and the method specifically comprises the following steps:
and analyzing GC-IMS two-dimensional spectrograms of different aromatizing cigarette paper samples in a Gallery plot view mode of LAV software, repeating each experiment for 3 times to obtain a fingerprint spectrum automatically generated by all detectable signal peaks in the GC-IMS two-dimensional spectrogram so as to compare the change conditions of aromatizing component compounds of aromatizing cigarette paper of different batches produced by different paper mills.
9. The fingerprint analysis method for the aroma components of different aromatized cigarette papers according to claim 1, wherein the chemometric analysis is performed on the aroma components of different aromatized cigarette paper samples according to the GC-IMS fingerprint analysis results of the different aromatized cigarette paper samples so as to distinguish the aromatized cigarette paper samples of different paper mills, which specifically comprises the following steps:
and (3) analyzing the aromatized cigarette paper samples produced by different paper mills by adopting a principal component analysis method and a partial least squares regression analysis method to obtain the distribution rule of corresponding areas of the aromatized cigarette paper samples of different batches of the same manufacturer and the aromatized cigarette paper samples of different manufacturers so as to distinguish the cigarette paper samples produced by different paper mills.
10. The fingerprint analysis method of the aroma components of different aromatized cigarette papers according to claim 9, wherein the data preprocessing method corresponding to the principal component analysis is UV scaling; and (3) performing partial least square discriminant analysis on the number of corresponding reserved latent variables: 5; and (3) cross validation: leaving one method; data preprocessing: UV scaling.
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