CN114544805A - Method for measuring mouth-to-mouth stability of heated cigarette by electronic nose - Google Patents
Method for measuring mouth-to-mouth stability of heated cigarette by electronic nose Download PDFInfo
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- CN114544805A CN114544805A CN202210114695.0A CN202210114695A CN114544805A CN 114544805 A CN114544805 A CN 114544805A CN 202210114695 A CN202210114695 A CN 202210114695A CN 114544805 A CN114544805 A CN 114544805A
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000443 aerosol Substances 0.000 claims abstract description 16
- 230000000391 smoking effect Effects 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000000779 smoke Substances 0.000 claims abstract description 12
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- 229920006221 acetate fiber Polymers 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 15
- 239000002131 composite material Substances 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000002390 rotary evaporation Methods 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 4
- 238000011156 evaluation Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000004587 chromatography analysis Methods 0.000 claims description 3
- 239000013618 particulate matter Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 230000010358 mechanical oscillation Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 4
- 239000012141 concentrate Substances 0.000 abstract 1
- 239000000284 extract Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 239000000796 flavoring agent Substances 0.000 description 6
- 235000019634 flavors Nutrition 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 241000208125 Nicotiana Species 0.000 description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 230000001953 sensory effect Effects 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003909 pattern recognition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F42/00—Simulated smoking devices other than electrically operated; Component parts thereof; Manufacture or testing thereof
- A24F42/90—Testing
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Library & Information Science (AREA)
- Engineering & Computer Science (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a method for measuring mouth-to-mouth stability of a heated cigarette by an electronic nose, which takes a self-made heated cigarette as an object, uses a mouth-to-mouth smoking machine to smoke, collects aerosol of each mouth of the heated cigarette, extracts and concentrates the aerosol by a solvent, samples obtained from a concentrated solution sample are injected and analyzed by the electronic nose, and the similarity of spectrograms of each sample is determined by comparing the smell fingerprint information of each mouth-to-mouth sample and calculating, thereby measuring the mouth-to-mouth stability of the heated cigarette. The method for determining the mouth-to-mouth stability of the heated cigarette by means of the electronic nose has the advantages of high detection speed, low detection limit, more types of determined substance components, good reproducibility and the like, is an objective, accurate and efficient analysis method, and has good potential application value.
Description
Technical Field
The invention relates to the field of novel tobacco heating cigarettes, in particular to a method for measuring the mouth-to-mouth stability of a heating cigarette by an electronic nose.
Background
The electric heating cigarette is composed of an electric heating cigarette smoking tool and an electric heating cigarette, a non-combustion heating mode is adopted to replace the traditional combustion thermal cracking to release smoke, the heating temperature is about 200-350 ℃, and an inhalable aerosol system is generated. Therefore, the heating cigarette has the advantages and characteristics of less harm, high safety, capability of better meeting physiological and psychological needs of smokers and the like, attracts a plurality of tobacco product consumers, and shows good development momentum in the international market.
At present, the most direct and effective evaluation method is through sensory effect, but the differences of description and judgment of the smoking result among smokers are caused by the influence of different sensory organ sensitivities and capturing degrees of various indexes, different physiological and psychological conditions, different environmental conditions and other factors, which fully explains that the sensory smoking method has great limitations. When one or more flavors pass through the electronic nose, the smell fingerprints of the flavors can be sensed by the sensor and extracted through a special intelligent pattern recognition algorithm. Different gas samples can be distinguished and identified by using different 'smell fingerprint' information of different flavor substances, so that the electronic nose can distinguish and identify the collected flavor substances, and the stability of the instrument of the same type is the best at present.
Disclosure of Invention
The invention aims to provide a method for measuring mouth-to-mouth stability of a heated cigarette by an electronic nose so as to solve the limitation problem of a sensory evaluation method.
In order to achieve the purpose, the method is realized by the following technical scheme:
a method for measuring the mouth-to-mouth stability of a heated cigarette by an electronic nose comprises the following steps:
s1 collection of aerosol of heated cigarette
Installing the heated cigarette in a mouth-by-mouth smoking machine, installing the cigarette in a multi-channel smoking machine, and installing a Cambridge filter disc in a catcher to catch the aerosol of the heated cigarette;
s2 pretreatment of aerosol
After the suction is finished, placing the Cambridge filter disc containing the same-mouth-order particle phase substances into a conical flask with a plug, adding a dichloromethane extraction solution, mechanically oscillating and standing, transferring the extraction liquid and the filter disc into a sand core funnel, filtering to obtain a filtrate, filtering the filtrate into a rotary evaporation bottle, carrying out reduced pressure rotary evaporation concentration to obtain a concentrated solution, and carrying out electronic nose analysis after the filtration membrane;
s3, electronic nose analysis
Separating, identifying and quantifying the concentrated solution by using a Heracles II ultra-fast gas-phase odor fingerprint analyzer, and performing fast chromatographic analysis to obtain an electronic nose spectrogram;
s4 evaluation of smoke mouth-to-mouth stability
According to the electronic nose spectrogram of the mouth-by-mouth smoke, a similarity model is established by comparing and analyzing the set quantity of the electronic nose spectrograms and the content change of key components, and the content difference of chemical components among the chemical components of the mouth-by-mouth smoke is quantified, so that the mouth-by-mouth stability of the heated cigarette is measured.
Further, before the step S1, the method comprises the preparation of a heated cigarette, wherein the heated cigarette is composed of a thin sheet rod, a hollow acetate fiber rod, a paper cooling rod and an acetate fiber rod, a 2+2 compounding process is adopted, the thin sheet rod and the hollow acetate fiber rod are compounded to form a thin sheet composite rod, the paper base composite rod is compounded with the paper fiber rod to form a paper base composite rod, and the two composite rods are compounded and cut again to form the heated cigarette.
Further, the total length of the heated cigarette is 50mm, wherein the length of the thin slice rod is 15mm, the length of the hollow acetate fiber rod is 10mm, the length of the paper cooling rod is 15mm, and the length of the acetate fiber rod is 10 mm.
Further, the pretreatment of the aerosol in step S2 is specifically that, after the suction is finished, the cambridge filter disc containing the same-mouth-sequence particulate matter is placed in a 100mL conical flask with a plug, 50mL of dichloromethane extraction solution is added, after mechanical oscillation is performed for 30min, standing is performed for 5min, the extraction solution and the filter disc are transferred to a sand core funnel for filtration, and the triangular flask and the sand core funnel are washed with 10mL of dichloromethane to obtain a filtrate; filtering the filtrate with 0.44 μm filter membrane to 100mL rotary evaporation bottle, performing rotary evaporation concentration at 40 deg.C under reduced pressure until the final concentration is 2mL, and performing electronic nose analysis after filtering with 0.44 μm filter membrane.
Further, in step S3, Heracles II comprises two different polarity columns MXT-5 and MXT-1701, wherein MXT-5 is a nonpolar column and MXT-1701 is a weakly polar column having a length of 10m and a column diameter of 18 μm.
Further, in step S4, comparing and analyzing the 10 electronic nose maps and the content variation of the critical component to establish a similarity model.
The invention has the beneficial effects that:
the method determines the mouth-to-mouth stability of the heated cigarette by means of the electronic nose, is an objective, accurate and efficient analysis method, and has good potential application value.
Drawings
FIG. 1 is an electronic nose map of the chemical composition of a first oral smoke;
FIG. 2 is a graph of the mouth-to-mouth release similarity of a heated cigarette.
Detailed Description
The following embodiments are merely exemplary, and can be used to explain and illustrate the technical solutions of the present invention, and should not be construed as limiting the technical solutions of the present invention.
The technical scheme takes a self-made (tobacco flavor) heated cigarette as an object, the heated cigarette is inserted into a heated cigarette smoking set, a mouth-by-mouth smoking machine is used for smoking, aerosol of each mouth of the heated cigarette is collected, solvent extraction and concentration are carried out, samples of obtained concentrated solution are subjected to sample injection analysis through an electronic nose, the similarity of spectrograms of all samples is determined through comparison of smell fingerprint information of each mouth-by-mouth sample, and therefore the mouth-by-mouth stability of the heated cigarette is determined. In the aspect of separation and identification of compounds, the main component analysis of Heracles II (electronic nose) is to search related information of a sample under a certain visual angle by carrying out linear transformation on an original data vector on the premise of not knowing the measured sample, repeatedly change a coordinate axis to achieve the purpose of distinguishing the sample, simultaneously calibrate by adopting an n-alkane standard solution (nC6-nC16), convert retention time into a retention index, and then carry out qualitative analysis on the compounds by using an Arochem Bals database. The technology has the advantages of high detection speed, low detection limit, more types of measured substance components, good reproducibility and the like.
Referring to fig. 1 and 2, the present application provides a method for measuring the mouth-to-mouth stability of a heated cigarette by an electronic nose, which comprises the following steps:
step (1), self-making a heating cigarette:
the cigarette consists of four sections of material, including thin sheet rod, hollow acetate fiber rod, paper cooling rod and acetate fiber rod. The total length of the cigarette is 50mm, wherein the length of the thin slice rod is 15mm, the length of the hollow acetate fiber rod is 10mm, the length of the paper cooling rod is 15mm, and the length of the acetate fiber rod is 10 mm. The '2 + 2' composite process is adopted, the thin sheet rod and the hollow acetate fiber rod are compounded to form a thin sheet composite rod, the paper rod and the acetate fiber rod are compounded to form a paper-based composite rod, and the two composite rods are compounded and cut again to form the heated cigarette.
Step (2), collecting aerosol of the heated cigarette:
the self-made (tobacco flavor) heated cigarette is arranged in a mouth-by-mouth smoking machine and a multi-pore channel smoking machine, and the Cambridge filter disc is arranged in a catcher to catch the heated cigarette aerosol. Starting the smoking set, starting the suction of the 1 st channel immediately after preheating, sucking each channel one by one, and taking down the smoking set and replacing cigarettes after the suction of the 10 th channel is finished. The aerosol of each mouth of the heated cigarette was collected for 20 cigarettes.
Step (3), pretreatment of aerosol:
after the suction is finished, placing the Cambridge filter disc containing the same-mouth-sequence particulate matter into a 100mL conical flask with a plug, adding 50mL dichloromethane extraction solution, mechanically oscillating for 30min, standing for 5min, transferring the extraction liquid and the filter disc into a sand core funnel, filtering, and washing the triangular flask and the sand core funnel with 10mL dichloromethane to obtain filtrate. Filtering the filtrate with 0.44 μm filter membrane to 100mL rotary evaporation bottle, performing rotary evaporation concentration at 40 deg.C under reduced pressure until the final concentration is 2mL, and performing electronic nose analysis after filtering with 0.44 μm filter membrane.
Step (4), analyzing the electronic nose:
and (3) separating, identifying and quantifying the compound by using a Heracles II ultra-fast gas-phase odor fingerprint analyzer (electronic nose), and performing fast chromatographic analysis to obtain an electronic nose spectrogram. Heracles II comprises two columns of different polarity MXT-5 and MXT-1701, wherein MXT-5 is a non-polar column and MXT-1701 is a less polar column, 10m in length and 18 μm in column diameter.
Step (5), evaluating the mouth-by-mouth stability of the smoke:
according to the electronic nose spectrogram of the mouth-by-mouth smoke, 10 electronic nose spectrograms and the content change of key components are contrastively analyzed to establish a similarity model, and the content difference of chemical components among the chemical components of the mouth-by-mouth smoke is quantified, so that the purpose of measuring the mouth-by-mouth stability of the heated cigarette is realized.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A method for measuring mouth-to-mouth stability of a heated cigarette by an electronic nose is characterized by comprising the following steps:
s1 collection of aerosol of heated cigarette
Installing the heated cigarette in a mouth-by-mouth smoking machine, installing the cigarette in a multi-channel smoking machine, and installing a Cambridge filter disc in a catcher to catch the aerosol of the heated cigarette;
s2 pretreatment of aerosol
After the suction is finished, placing the Cambridge filter disc containing the same-mouth-order particle phase substances into a conical flask with a plug, adding a dichloromethane extraction solution, mechanically oscillating and standing, transferring the extraction liquid and the filter disc into a sand core funnel, filtering to obtain a filtrate, filtering the filtrate into a rotary evaporation bottle, carrying out reduced pressure rotary evaporation concentration to obtain a concentrated solution, and carrying out electronic nose analysis after the filtration membrane;
s3, electronic nose analysis
Separating, identifying and quantifying the concentrated solution by using a Heracles II ultra-fast gas-phase odor fingerprint analyzer, and performing fast chromatographic analysis to obtain an electronic nose spectrogram;
s4 evaluation of smoke mouth-to-mouth stability
According to the electronic nose spectrogram of the mouth-by-mouth smoke, a similarity model is established by comparing and analyzing the set quantity of the electronic nose spectrograms and the content change of key components, and the content difference of chemical components among the chemical components of the mouth-by-mouth smoke is quantified, so that the mouth-by-mouth stability of the heated cigarette is measured.
2. The method for measuring the mouth-to-mouth stability of the heated cigarette by the electronic nose according to claim 1, wherein the step S1 is preceded by preparing the heated cigarette, the heated cigarette is composed of four sections of materials, namely a thin sheet rod, a hollow acetate fiber rod, a paper cooling rod and an acetate fiber rod, by adopting a 2+2 composite process, the thin sheet rod and the hollow acetate fiber rod are compounded to form the thin sheet composite rod, the paper rod and the acetate fiber rod are compounded to form the paper-based composite rod, and the two composite rods are compounded and cut again to form the heated cigarette.
3. The method for measuring the mouth-to-mouth stability of the heated cigarette by the electronic nose according to claim 2, wherein the total length of the cigarette is 50mm, wherein the length of the thin slice rod is 15mm, the length of the hollow acetate fiber rod is 10mm, the length of the paper cooling rod is 15mm, and the length of the acetate fiber rod is 10 mm.
4. The method for determining the mouth-to-mouth stability of the heated cigarette by the electronic nose according to claim 1, wherein the pretreatment of the aerosol in the step S2 is specifically that after the smoking is finished, the Cambridge filter containing the same-mouth-sequence particulate matter is placed in a 100mL conical flask with a plug, 50mL of dichloromethane extraction solution is added, after mechanical oscillation is carried out for 30min, standing is carried out for 5min, the extraction liquid and the filter are transferred to a sand core funnel for filtration, and the triangular flask and the sand core funnel are washed by 10mL of dichloromethane to obtain filtrate; filtering the filtrate with 0.44 μm filter membrane to 100mL rotary evaporation bottle, performing rotary evaporation concentration at 40 deg.C under reduced pressure until the final concentration is 2mL, and performing electronic nose analysis after filtering with 0.44 μm filter membrane.
5. The method for determining the mouth-to-mouth stability of a heated cigarette according to claim 1, wherein in step S3, Heracles II comprises two chromatographic columns of different polarities MXT-5 and MXT-1701, wherein MXT-5 is a non-polar chromatographic column and MXT-1701 is a less polar chromatographic column, wherein the length of the column is 10m, and the diameter of the column is 18 μm.
6. The method for determining the mouth-to-mouth stability of the heated cigarette by the electronic nose according to claim 1, wherein in the step S4, 10 electronic nose spectrograms and content changes of key components are contrastively analyzed to establish a similarity model.
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| CN202210114695.0A CN114544805B (en) | 2022-01-30 | 2022-01-30 | Method for measuring mouth-to-mouth stability of heated cigarettes through electronic nose |
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| CN202210114695.0A CN114544805B (en) | 2022-01-30 | 2022-01-30 | Method for measuring mouth-to-mouth stability of heated cigarettes through electronic nose |
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| CN114544805B (en) | 2024-05-10 |
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