CN117783324A - Tobacco extract quality discriminating method based on characteristic component relative index - Google Patents
Tobacco extract quality discriminating method based on characteristic component relative index Download PDFInfo
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- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 118
- 239000000284 extract Substances 0.000 title claims abstract description 100
- 238000000034 method Methods 0.000 title claims abstract description 24
- 244000061176 Nicotiana tabacum Species 0.000 title 1
- 241000208125 Nicotiana Species 0.000 claims abstract description 117
- IGJQUJNPMOYEJY-UHFFFAOYSA-N 2-acetylpyrrole Chemical compound CC(=O)C1=CC=CN1 IGJQUJNPMOYEJY-UHFFFAOYSA-N 0.000 claims abstract description 30
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- DMHADBQKVWXPPM-PDDCSNRZSA-N (1e,3z,6e,10z,14s)-3,7,11-trimethyl-14-propan-2-ylcyclotetradeca-1,3,6,10-tetraene Chemical compound CC(C)[C@@H]\1CC\C(C)=C/CC\C(C)=C\C\C=C(\C)/C=C/1 DMHADBQKVWXPPM-PDDCSNRZSA-N 0.000 claims description 2
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- MTXSIJUGVMTTMU-UHFFFAOYSA-N Neonicotine Natural products N1CCCCC1C1=CC=CN=C1 MTXSIJUGVMTTMU-UHFFFAOYSA-N 0.000 claims description 2
- DMHADBQKVWXPPM-SBHJBAJOSA-N cembrene Natural products CC(C)C1CCC(=C/CCC(=CCC=C(C)/C=C/1)C)C DMHADBQKVWXPPM-SBHJBAJOSA-N 0.000 claims description 2
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Abstract
The invention discloses a tobacco extract quality judging method based on characteristic component relative indexes, which judges whether a tobacco extract to be detected meets the following standard: detecting nicotine and common characteristic components in the tobacco extract, wherein the nicotine and common characteristic components at least comprise five components of farnesylacetone, 2-acetyl pyrrole, dihydro-beta-ionol, damascenone and 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one, and judging that relative indexes of all substances are not more than 0.25, 0.05 and 0.05 respectively according to detection results; the relative index is the ratio of the content of the common characteristic components of the corresponding tobacco extracts to the content of nicotine; the tobacco extract to be tested is qualified. The invention takes the relative index as the basis, does not need to accurately quantify the absolute content of each index, and eliminates the influence of the production place, the product form and the preparation process of the raw material of the tobacco extract while taking the quality characteristics and the style characteristics into consideration.
Description
Technical Field
The invention relates to a tobacco extract quality judging method based on characteristic component relative indexes, and belongs to the technical field of tobacco essence and spice.
Background
The tobacco flavor has the effects of endowing or strengthening the style characteristics of a cigarette product, improving the quality of tobacco leaves, improving the comfort level and the like, wherein the tobacco extract is derived from the tobacco, has natural and harmonious aroma, can strengthen the herbal aroma of the tobacco, makes up the aroma loss caused by the shortage of partial tobacco leaves, and is an irreplaceable aroma raw material for flavoring the cigarette and developing novel tobacco products.
The preparation method of the tobacco extract is various, but in the production application, the production process of the tobacco extract is mainly a solvent extraction method in consideration of a plurality of factors such as equipment energy consumption, cost and the like, the tobacco essential oil is mainly steam distillation, and the tobacco absolute oil is mostly obtained by solvent extraction or supercritical extraction of the extract, ethanol dissolution and freeze dewaxing. Thus, there is a large difference in chemical composition between the different forms of the product. In addition, even if tobacco materials are produced in different places in the same production area, the tobacco materials themselves have a difference in aroma-generating components. Therefore, the raw materials, the preparation process and the product forms of various manufacturers are different, so that the commercial tobacco extracts have large chemical composition difference and different quality, and certain difficulty is brought to the quality evaluation of the tobacco extracts. In recent years, studies on tobacco extracts have focused mainly on preparation methods and sensory evaluation, conventional chemical components, characteristic aroma component analysis, production regions, and the like. For example: zhang Hua and the like, screening characteristic components which can be used for characterizing tobacco extracts of different producing areas by combining solid-phase support liquid-liquid extraction-GC-MS with chemometrics, and identifying Yunnan and Zimbabwe tobacco extracts.
Although there is necessarily a large difference between different kinds of tobacco extracts, tobacco materials have some common characteristics, such as nicotine and other alkaloids, neophytadiene, 4,7, 9-megastigmatrien-3-one, damascone, etc., and how to use the common characteristics to realize quality discrimination of tobacco extracts has not been reported yet.
Disclosure of Invention
The invention aims to provide a tobacco extract quality judging method based on characteristic component relative indexes, which aims to solve the problem that the common characteristics of the tobacco extract quality judging method are not utilized to realize the tobacco extract quality judgment in the prior art.
In order to achieve the above object, the present invention adopts the technical scheme that the tobacco extract quality discriminating method based on the characteristic component relative index:
a tobacco extract quality judging method based on characteristic component relative indexes judges whether the tobacco extract to be detected meets the following criteria:
(1) Detecting nicotine and common characteristic components in a tobacco extract, wherein the common characteristic components of the tobacco extract at least comprise five components of farnesylacetone, 2-acetyl pyrrole, dihydro-beta-ionol, damascenone and 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one;
(2) Judging that the relative indexes of five characteristic components of farnesylacetone, 2-acetylpyrrole, dihydro-beta-ionol, damascenone and 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one are not more than 0.25, 0.05 and 0.05 respectively according to the detection result of the step (1); the relative index is the ratio of the content of the common characteristic components of the corresponding tobacco extracts to the content of nicotine;
if the tobacco extract to be tested meets the (1) and (2) items at the same time, the tobacco extract to be tested is qualified; otherwise, the tobacco extract to be tested is unqualified.
The beneficial effect of above-mentioned scheme lies in: the invention introduces the concept of relative index, namely the ratio (peak area, relative content or absolute content) of chemical components to nicotine for the first time in order to avoid the interference of product morphology (tincture, absolute oil, essential oil, extract and the like) on analysis results. Nicotine not only can provide satisfaction, but also is one of key influencing factors of tobacco quality, and usually sugar-nitrogen ratio, sugar-alkali ratio and the like are often used for tobacco quality judgment and analysis. For tobacco extract products, the quality characteristics and the style characteristics are equally important, and the characteristic aroma components are closely related to the flavor style characteristics of cigarettes, so that the influence of the nicotine content on quality indexes such as taste and the like is large. Therefore, the relative index is taken as a discrimination standard, and the influence of the production place, the product form and the preparation process of the raw material of the tobacco extract is eliminated while the quality characteristics and the style characteristics are considered. Furthermore, the invention uses the common characteristic components of the tobacco extract as the judgment standard through analysis and discovery, and has the advantages of accurate and reliable result and simple and quick operation. The quality judging method lays a theoretical foundation for evaluating the tobacco extract products with good quality in the market, and is beneficial to promoting the benign development of the tobacco extract products in the market.
Specifically, the qualification of the invention means that the sample has the characteristics of tobacco extract.
In order to simplify the complex operation flow, it is preferable that the relative index is a ratio of the peak area or the relative content or the absolute content of the common characteristic component of the corresponding tobacco extract to the nicotine on the premise of ensuring the evaluation accuracy. Specifically, the common characteristic components of the corresponding tobacco extracts are farnesylacetone, 2-acetyl pyrrole, dihydro-beta-ionol, damascenone or 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one.
As a further improvement, the tobacco extract of step (1) shares common characteristic components including neophytadiene, myosmine, dienonene, neonicotinoid, 5-methylfuran aldehyde, DL-pantothenolactone, phenylacetaldehyde, 2-acetylpyrrole, maltol, isophorone, 6-ethyl-5, 6-dihydro-2H-pyran-2-one, 5-hydroxymethylfurfural, ethyl phenylacetate, anethole, dihydro- β -ionol, damascenone, β -damascenone, geranylacetone, 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one, 2,3' -bipyridine, 4,7, 9-megastigmatrien-3-one (4), 9-hydroxy-4, 7-megastigmadien-3-one, farnesyl acetone and sibirisone.
The beneficial effect of above-mentioned scheme lies in: the components are characteristic components shared by most tobacco extracts, and can effectively represent the characteristics of the tobacco extracts.
As a further improvement, the information of the common characteristic components of the tobacco extract in the step (1) is obtained by SPME-GC/MS, GC/MS or HPLC-MS method.
The beneficial effect of above-mentioned scheme lies in: SPME-GC/MS, GC/MS and HPLC-MS are effective methods for analyzing the components of substances, and can rapidly and accurately obtain the content of the substances.
Preferably, a total ion flow diagram of the tobacco extract to be detected is obtained through an SPME-GC/MS method and spectrogram processing is carried out; the spectrogram processing includes chromatographic signal baseline correction, peak extraction and annotation and peak alignment.
The beneficial effect of above-mentioned scheme lies in: after the obtained total ion flow diagram of the tobacco extract is subjected to the spectrogram processing, the retention time, peak area and other information of each component in the tobacco extract can be accurately obtained, and a foundation is laid for subsequent analysis modeling.
As a further improvement, the product form of the tobacco extract comprises one or more of extract, absolute, essential oil and tincture.
The beneficial effect of above-mentioned scheme lies in: the tobacco extract quality judging method of the invention focuses on the relative content of characteristic components and nicotine in the tobacco extract, is not influenced by the processing technology and the product form, is suitable for all tobacco extracts, and has strong universality.
As a further improvement, the raw material source of the tobacco extract includes one or more of china (Yunnan, henan), zimbabwe, brazil, U.S. (virginia).
The beneficial effect of above-mentioned scheme lies in: the tobacco extract quality judging method focuses on the relative content of characteristic components and nicotine in the tobacco extract, is not influenced by tobacco types, is suitable for all tobacco extracts, and has strong universality.
As a further improvement, the raw material type of the tobacco extract includes one or more of flue-cured tobacco, burley tobacco, red sun-cured tobacco, cigar.
The beneficial effect of above-mentioned scheme lies in: the tobacco extract quality judging method focuses on the relative content of characteristic components and nicotine in the tobacco extract, is not influenced by the types of tobacco leaves, processing technology and storage conditions, is suitable for all tobacco extracts, and has strong universality.
The preparation method of the tobacco extract comprises, but is not limited to, solvent extraction, subcritical extraction, supercritical extraction, molecular distillation, membrane separation, column chromatography, steam distillation and the like.
Detailed Description
According to the invention, more than 200 commercial tobacco extracts with different product forms, raw material sources and raw material types are analyzed for characteristic component relative indexes, 27 common characteristic components of the tobacco extracts are obtained, and the 27 common characteristic components are as follows: neophytadiene, myosmine, dienoneine, neonicotinoid, 5-methylfuran aldehyde, DL-pantothenolactone, phenylacetaldehyde, 2-acetylpyrrole, maltol, isophorone, 6-ethyl-5, 6-dihydro-2H-pyran-2-one, 5-hydroxymethylfurfural, ethyl phenylacetate, anethole, dihydro- β -ionol, damascenone, β -damascenone, geranylacetone, 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one, 2,3' -bipyridine, 4,7, 9-megastigmatrien-3-one (4), 9-hydroxy-4, 7-megastigmadien-3-one, farnesylacetone and cembrene. Further analyzing the distribution of the 27 common characteristic components relative indexes in more than 200 commercial tobacco extracts, screening out 5 characteristic components of Nicotine acetone, 2-acetyl pyrrole, dihydro-beta-ionol, damascenone and 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one with small variation coefficient (indicating small difference among different samples), and obtaining the tobacco extract quality criterion based on the five characteristic component relative indexes through analysis.
The present invention will be described in further detail with reference to specific examples. The equipment and reagents used in the examples, experimental examples and comparative examples were all commercially available, except for the specific descriptions.
Example 1
The tobacco extract quality discriminating method based on the characteristic component relative index of the embodiment is implemented as follows:
the tobacco extract samples with different raw material sources and product forms are prepared for 32 samples. Wherein the product form comprises extract, absolute, tincture and essential oil; the raw material sources comprise flue-cured tobacco, burley tobacco, aromatic tobacco, cigar and the like, and SPME-GC/MS is adopted to analyze characteristic components in the tobacco extract.
Accurately weighing 0.5g of sample, placing in a 20mL headspace bottle, sealing the headspace bottle with an aluminum cap, and carrying out HS-SPME-GC/MS analysis. The solid phase microextraction head (50/30 μm DVB/CAR/PDMS) is aged at 270 ℃ for 20min to remove volatile components residues possibly adsorbed in the head, so as to avoid sample pollution. The aged solid phase microextraction head is kept at a headspace for adsorption for 30min at a temperature of 100 ℃ and is desorbed for 5min at a temperature of 270 ℃.
GC/MS conditions: DB-5ms capillary column (60 m 250 m 0.25 m); sample inlet temperature: 250 ℃; carrier gas: high-purity helium with a flow rate of 1.0mL/min; sample injection amount: 1 μl; split ratio: 15:1, a step of; programming temperature: 50 ℃ (2 min) 8 ℃/min 280 ℃ (25 min). Ionization mode: EI; ion source temperature: 230 ℃; ionization energy: 70eV; quadrupole temperature: 150 ℃; electron multiplier voltage: 1.89kV; mass scan range: 33-500 amu; scanning mode: full scanning; solvent delay: 5min.
And (3) applying MATLAB mass spectrum data analysis kit (AntDAS), carrying out steps of chromatographic signal baseline correction, peak extraction, annotation, peak alignment and the like on the acquired data, finally obtaining retention time, peak area and corresponding MSP files of each component in the sample, and introducing the MSP files into an NIST database for database searching qualitative analysis.
Through analysis, 32 tobacco extracts to be tested all contain neophytadiene, myosmine, dienoneine, neonicotine, 5-methylfuran aldehyde, DL-pantolactone, phenylacetaldehyde, 2-acetylpyrrole, maltol, isophorone, 6-ethyl-5, 6-dihydro-2H-pyran-2-one, 5-hydroxymethylfurfural, ethyl phenylacetate, anethole, dihydro-beta-ionol, damascenone, beta-damascenone, geranylacetone, 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-butene-2-one, 2,3' -bipyridine, 4,7, 9-megastigmatrien-3-one (4), 9-hydroxy-4, 7-megastigmadien-3-one, farnesyl acetone and sibiriene, and 27 tobacco extracts have common characteristic components. And the ratio of the peak area to the nicotine peak area of five components of nisylacetone, 2-acetylpyrrole, dihydro- β -ionol, damascenone and 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one was calculated as the relative index of the components according to the peak pattern obtained by GC/MS, as shown in table 1.
Table 1 results of analysis of 5 indices of 32 tobacco extracts in example 1
Through the above experiments, the inventors found that the relative index of farnesyl acetone, 2-acetylpyrrole, dihydro- β -ionol, damascenone or 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one in a part of the samples was abnormal, and judged as a failed sample. Meanwhile, by analyzing non-common components in characteristic components of an abnormal sample, the sample is found to contain non-tobacco aroma components, which indicates that the product cannot represent real information of tobacco extract. For example: the No. 25 Yunyan extract contains theobromine, the component is a characteristic component of the cocoa extract, and the component is not present in tobacco raw materials; the Zimbabwe extract No. 29 and No. 30 and the tobacco extract respectively contain ethyl vanillin and ethyl maltol, which are synthetic flavors, and are not present in natural plants.
The invention uses the relative index for extracting the common characteristic of the tobacco extract, and 27 common characteristic components of the tobacco extract are obtained. Further, five components of farnesylacetone, 2-acetylpyrrole, dihydro- β -ionol, damascenone, or 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one were selected from 27 common components, and their relative indices were used for quality judgment of tobacco extracts. When the tobacco extract is subjected to characteristic component analysis, 27 common components are contained, and when the relative indexes of farnesylacetone, 2-acetyl pyrrole, dihydro-beta-ionol, damascenone or 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one are not more than 0.25, 0.05 and 0.05 respectively, the sample is judged to be qualified; conversely, if any of the above is not satisfied, the product is judged to be a defective product, and is not suitable for use in the related study or application.
The last explanation is: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (6)
1. A tobacco extract quality discriminating method based on characteristic component relative indexes is characterized in that: judging whether the tobacco extract to be tested meets the following criteria:
(1) Detecting nicotine and common characteristic components in a tobacco extract, wherein the common characteristic components of the tobacco extract at least comprise five components of farnesylacetone, 2-acetyl pyrrole, dihydro-beta-ionol, damascenone and 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one;
(2) Judging that the relative indexes of five characteristic components of farnesylacetone, 2-acetylpyrrole, dihydro-beta-ionol, damascenone and 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one are not more than 0.25, 0.05 and 0.05 respectively according to the detection result of the step (1); the relative index is the ratio of the content of the common characteristic components of the corresponding tobacco extracts to the content of nicotine;
if the tobacco extract to be tested meets the (1) and (2) items at the same time, the tobacco extract to be tested is qualified; otherwise, the tobacco extract to be tested is unqualified.
2. The tobacco extract quality discriminating method based on characteristic component relative index according to claim 1 wherein: the tobacco extract in the step (1) has common characteristic components including neophytadiene, myosmine, dienonenicotine, neonicotine, 5-methylfuran aldehyde, DL-pantothenolactone, phenylacetaldehyde, 2-acetyl pyrrole, maltol, isophorone, 6-ethyl-5, 6-dihydro-2H-pyran-2-one, 5-hydroxymethylfurfural, ethyl phenylacetate, anethole, dihydro-beta-ionol, damascenone, beta-damascenone, geranylacetone, 4- (2, 6-trimethyl-1, 3-cyclohexadien-1-yl) -3-buten-2-one, 2,3' -bipyridine, 4,7, 9-megastigmatrien-3-one (4 species), 9-hydroxy-4, 7-megastigmadien-3-one, farnesyl acetone and cembrene.
3. The tobacco extract quality discriminating method based on characteristic component relative index according to claim 1 wherein: the information of the common characteristic components of the tobacco extract in the step (1) is obtained by an SPME-GC/MS, GC/MS or HPLC-MS method.
4. A tobacco extract quality discriminating method based on characteristic component relative index according to any one of claims 1 to 3 wherein: the product form of the tobacco extract comprises one or more of extract, absolute oil, essential oil and tincture.
5. A tobacco extract quality discriminating method based on a characteristic component relative index according to any one of claims 1 to 3, characterized by: the tobacco extract is prepared from one or more of China (Yunnan, henan), zimbabwe, brazil and America (Virginia).
6. A tobacco extract quality discriminating method based on characteristic component relative index according to any one of claims 1 to 3 wherein: the raw material type of the tobacco extract comprises one or more of flue-cured tobacco, burley tobacco, sun-cured red tobacco and cigar.
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