CN114113368A - Mouth-by-mouth transfer control method for heating sweet and fragrant monomers in cigarettes - Google Patents
Mouth-by-mouth transfer control method for heating sweet and fragrant monomers in cigarettes Download PDFInfo
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 136
- 235000009508 confectionery Nutrition 0.000 title claims abstract description 129
- 239000000178 monomer Substances 0.000 title claims abstract description 72
- 238000012546 transfer Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000010438 heat treatment Methods 0.000 title claims description 13
- 239000000779 smoke Substances 0.000 claims abstract description 33
- 235000013599 spices Nutrition 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims description 40
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 18
- 241000208125 Nicotiana Species 0.000 claims description 15
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 12
- 230000000391 smoking effect Effects 0.000 claims description 11
- PETRWTHZSKVLRE-UHFFFAOYSA-N 2-Methoxy-4-methylphenol Chemical compound COC1=CC(C)=CC=C1O PETRWTHZSKVLRE-UHFFFAOYSA-N 0.000 claims description 10
- WGAVDEVFJDQIMZ-UHFFFAOYSA-N 3,4-dimethyl-1,2-cyclopentanedione Chemical compound CC1CC(=O)C(=O)C1C WGAVDEVFJDQIMZ-UHFFFAOYSA-N 0.000 claims description 10
- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 10
- 238000001212 derivatisation Methods 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 8
- RHDGNLCLDBVESU-UHFFFAOYSA-N but-3-en-4-olide Chemical compound O=C1CC=CO1 RHDGNLCLDBVESU-UHFFFAOYSA-N 0.000 claims description 7
- XCOBLONWWXQEBS-KPKJPENVSA-N N,O-bis(trimethylsilyl)trifluoroacetamide Chemical compound C[Si](C)(C)O\C(C(F)(F)F)=N\[Si](C)(C)C XCOBLONWWXQEBS-KPKJPENVSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 claims description 5
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 claims description 5
- 229940093503 ethyl maltol Drugs 0.000 claims description 5
- 229940043353 maltol Drugs 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002304 perfume Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000000796 flavoring agent Substances 0.000 claims description 3
- 235000019634 flavors Nutrition 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- -1 n-heptadecane dichloromethane Chemical compound 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 4
- CFAKWWQIUFSQFU-UHFFFAOYSA-N 2-hydroxy-3-methylcyclopent-2-en-1-one Chemical compound CC1=C(O)C(=O)CC1 CFAKWWQIUFSQFU-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000006399 behavior Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 231100000041 toxicology testing Toxicity 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture Of Tobacco Products (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
The invention relates to a mouth-by-mouth transfer control method of a baked sweet and fragrant monomer in a heated cigarette, which detects the mouth-by-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomer in the heated cigarette; determining the types of baked sweet and fragrant monomers to be added into the heated cigarettes; and determining the adding amount of the baked sweet and fragrant monomers to be added according to the types of the baked sweet and fragrant monomers to be added, the mouth-to-mouth transfer rate of the baked sweet and fragrant monomers and the total transfer rate. According to the technical scheme, the detection of the mouth-to-mouth release amount of the baked sweet and fragrant monomer spice in the mainstream smoke of the heated cigarette and the detection of the total transfer rate under different addition amounts are established, so that a control basis is provided for the addition amount of the baked sweet and fragrant monomer spice to be added in the heated cigarette.
Description
Technical Field
The invention belongs to the technical field of novel tobacco, and particularly relates to a mouth-by-mouth transfer control method for a sweet and fragrant monomer baked in a heated cigarette.
Background
Compared with the traditional cigarette, the cigarette heating releases smoke by heating the tobacco material, reduces harmful ingredients generated by pyrolysis of tobacco due to high-temperature combustion, but also brings quality defects of insufficient aroma, low satisfaction and the like, and influences the acceptance of consumers on the cigarette heating product. The flavoring and casing are important methods and means for making up for the insufficient quality of the heated cigarette, and as the material basis of the flavoring and casing of the heated cigarette, the release characteristic of the monomer spice in the heated cigarette directly determines the application effect of the flavoring and casing. Currently, the related researches on heating cigarettes at home and abroad mainly focus on the aspects of conventional chemical index analysis, toxicological evaluation and the like of smoke, and the basic technical researches related to the flavoring of the heating cigarettes, such as the release behavior of monomer spices, are rarely reported.
The roasted sweet aroma is a compound aroma characteristic with the roasted aroma, the sweet aroma and the burnt sweet aroma and is an important component of the aroma style characteristic of the cigarettes. For the heated cigarette, the aroma style characteristics of the cigarette can be enhanced by adding the roasted sweet aroma spice, and an effective aroma compensation effect can be achieved. However, no report is found on the mouth-to-mouth transfer behavior of the monomer aroma of roasted sweet in the heated cigarette.
Disclosure of Invention
The invention aims to provide a mouth-to-mouth transfer control method of a baked sweet monomer in a heated cigarette, which takes the baked sweet monomer spice as an object, establishes a mouth-to-mouth release amount analysis method in main stream smoke of the heated cigarette, and measures the mouth-to-mouth release amount of the baked sweet monomer spice under different addition amounts so as to realize the control of the baked sweet monomer spice in the heated cigarette.
In order to realize the purpose, the invention is realized by the following technical scheme:
a mouth-by-mouth transfer control method for sweet and fragrant monomers baked in a heated cigarette comprises the following steps:
s1, detecting the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomers in the heated cigarette;
s2, determining the types of baked sweet and fragrant monomers to be added into the heated cigarette;
s3, determining the adding amount of the baking sweet and fragrant monomers to be added according to the types of the baking sweet and fragrant monomers to be added and the mouth-to-mouth transfer rate and the total transfer rate of the baking sweet and fragrant monomers.
Further, the roasted sweet monomers comprise at least furanone, 3, 4-dimethyl-1, 2-cyclopentadione, methyl cyclopentenolone, maltol, 4-methyl guaiacol or ethyl maltol.
Further, the method for detecting the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomer in the heated cigarette in the step S1 includes the following steps:
step 1, preparation of flavoring solution
Weighing a set weight of roasted sweet and fragrant monomer perfume, and fixing the volume to a first set volume by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2 to serve as a first flavoring solution; transferring the first flavoring solution with a second set volume, and fixing the volume to the first set volume by using the mixed solution of the ethanol and the propylene glycol to be used as a second flavoring solution;
step 2, preparation of flavored and heated cigarettes
Respectively adding the first flavoring solution and the second flavoring solution prepared in the step 1 into blank heated cigarettes to prepare heated cigarettes with different addition amounts of the baked sweet and fragrant monomers, and respectively marking the heated cigarettes as a first heated cigarette and a second heated cigarette;
step 3, determining the roasted sweet and fragrant components in the cut tobacco of the blank heated cigarette
And (3) determination of neutral roasted sweet components: taking out tobacco shreds of blank heated cigarettes, crushing and sieving by a 40-mesh sieve to obtain tobacco powder, weighing 2g of tobacco powder into 100mL of conical bottles with plugs, adding 50mL of extraction solution containing 5 mu g/mL of n-heptadecane-containing dichloromethane solution, carrying out ultrasonic treatment for 30min, shaking uniformly, taking 5mL of supernate, sieving by a 0.44 mu m filter membrane, and carrying out GC-MS analysis on the filtrate;
and (3) determining the acid roasted sweet components: measurement of ingredients with neutral roasted sweet flavor except that before GC-MS analysis, 1ml of supernatant is taken to be put into a chromatographic bottle, 300 mu L of BSTFA is added, and derivatization treatment is carried out for 40min in water bath at 60 ℃;
step 4, quantitatively measuring the roasted sweet and fragrant components in the smoke mouth by mouth
1) Respectively inserting the first heated cigarette and the second heated cigarette in the step 2 into a heated cigarette smoking set, and then installing the heated cigarette smoking set on a mouth-by-mouth smoking machine
The Cambridge filter sheet is used for collecting and heating particulate matters in the mainstream smoke of the cigarettes;
2) determination of roasted sweet component
And (3) determination of neutral roasted sweet components: placing 2 filter discs containing the same-mouth particle phase substances in the step (1) into a 100mL conical flask with a plug, adding 50mL of extraction solution containing 5 mu g/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extraction liquid and the filter discs into a sand core funnel, carrying out primary filtration, and flushing 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, concentrating at 45 deg.C under normal pressure to 2mL, filtering with 0.44 μm filter membrane, and performing GC-MS analysis;
and (3) determining the acid roasted sweet components: the same conditions as those in step (2) but requiring derivatization treatment before GC-MS analysis, specifically, 1ml of the concentrated solution is taken into a chromatographic bottle, 300. mu.L of BSTFA is added, and water bath at 60 ℃ is used for derivatization for 40 min.
Step 5, the calculation formula of the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomer spice in the mainstream smoke of the cigarette is as follows:
mouth-to-mouth transfer rate: t isN＝(RAN-R0N)/(CmA-Cm0)×100％ (1)
The total transfer rate: t ═ RA-R0)/(CmA-Cm0)×100％ (2)
Wherein: rANThe release amount of the roasted sweet and fragrant components in the particle phase substances of the main stream smoke of the Nth opening of the flavored cigarette is mu g/piece;
R0Nthe release amount of the baked sweet components in the particle phase substances of the main stream smoke of the Nth mouth of the blank cigarette is mu g/cigarette;
CmA-the content of roasted sweet components in the flavored cigarette slices, μ g per cigarette;
Cm0-the content of roasted sweet components in the blank cigarette sheet, μ g/cigarette;
RAthe total release amount of the roasted sweet components in the main stream smoke particle phase substances of the flavored cigarettes is mu g/cigarette;
R0the total release amount of the baked sweet components in the particulate matters of the main stream smoke of the blank cigarette is mu g/cigarette.
Furthermore, in the step 2, the addition amount of the roasted sweet components in the first heated cigarette is 0.1 per mill, and the addition amount of the roasted sweet components in the second heated cigarette is 0.5 per mill.
The invention has the beneficial effects that:
according to the technical scheme, the detection of the mouth-to-mouth release amount of the baked sweet and fragrant monomer spice in the mainstream smoke of the heated cigarette and the detection of the total transfer rate under different addition amounts are established, so that a control basis is provided for the addition amount of the baked sweet and fragrant monomer spice to be added in the heated cigarette.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and explaining the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
In the following examples of the present application, examples 2 to 6 are all the same as the technique of example 1, except that the differences are only the roasted sweet monomer, wherein the roasted sweet monomer of example 1 is furanone, the roasted sweet monomer of example 2 is 3, 4-dimethyl-1, 2-cyclopentadione, the roasted sweet monomer of example 3 is methyl cyclopentenolone, the roasted sweet monomer of example 4 is maltol, the roasted sweet monomer of example 5 is 4-methyl guaiacol, and the roasted sweet monomer of example 6 is ethyl maltol.
Example 1
A mouth-by-mouth transfer control method for sweet and fragrant monomers baked in a heated cigarette comprises the following steps:
s1, detecting the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomers in the heated cigarette;
s2, determining the types of baked sweet and fragrant monomers to be added into the heated cigarette;
s3, determining the adding amount of the baking sweet and fragrant monomers to be added according to the types of the baking sweet and fragrant monomers to be added and the mouth-to-mouth transfer rate and the total transfer rate of the baking sweet and fragrant monomers.
In the present application, the roasted sweet monomers are six roasted sweet monomers of furanone, 3, 4-dimethyl-1, 2-cyclopentadione, methyl cyclopentenolone, maltol, 4-methyl guaiacol or ethyl maltol.
The method for detecting the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomer in the heated cigarette comprises the following steps:
step 1, preparation of flavoring solution
About 0.25g of furanone monomer perfume is accurately weighed to be accurate to 0.0001 g, the volume is determined to be 10mL by using ethanol/propylene glycol (v: v ═ 1:2), and the furanone monomer perfume is shaken up to be used as a first perfuming solution for standby. Accurately transferring 2mL of the first flavoring solution, diluting to 10mL with the ethanol/propylene glycol solution, and shaking to obtain a second flavoring solution.
Step 2, preparation of flavored and heated cigarettes
Respectively injecting 0.48 mu L of the first flavoring solution and the second flavoring solution into an unflavored heated cigarette (hereinafter referred to as blank cigarette) by using an essence injection machine to prepare each heated cigarette with the addition of the sweet and fragrant baking component of 0.1 per thousand and 0.5 per thousand, and respectively marking as a first heated cigarette A and a second heated cigarette B.
Step 3, determining the roasted sweet and fragrant components in the cut tobacco of the blank heated cigarette
Extraction solution: a dichloromethane solution containing 5. mu.g/mL n-heptadecane (internal standard) was prepared.
And (3) determination of neutral roasted sweet components: taking out the thin cut tobacco from the blank cigarette, crushing, and sieving by a 40-mesh sieve to obtain thin tobacco powder. About 2g (exactly to 0.0001 g) of flake tobacco was weighed into a 100mL conical flask with a stopper, 50mL of the extraction solution was added, after sonication for 30min, shaking was carried out, 5mL of the solution was filtered through a 0.44 μm filter, and the filtrate was subjected to GC-MS analysis.
A chromatographic column: j & W122-5563 (60 m.times.0.25 mm. times.1 μm); sample inlet temperature: 200 ℃; temperature rising procedure: keeping the temperature at 40 ℃ for 3min, increasing the temperature to 250 ℃ at the heating rate of 3 ℃/min, and increasing the temperature to 290 ℃ at the heating rate of 5 ℃/min for 20 min; sample introduction mode: no-flow sampling, sample injection amount: 1 mu L of the solution; carrier gas: he gas, flow rate: 1.5 mL/min. Transmission line temperature: 290 ℃; an ionization mode: EI; ionization energy: 70 eV; and (3) monitoring mode: a full scan mode and a selective ion scan mode; full-sweep collection mass number range: 40-350 parts of; the retention time and mass spectrum parameters of the fragrance component and the internal standard are shown in table 1, and the serial numbers 1 to 6 in table 1 are furanone, 3, 4-dimethyl-1, 2-cyclopentanedione, methyl cyclopentenolone, maltol, 4-methyl guaiacol and ethyl maltol in sequence.
And (3) determining the acid roasted sweet components: determination of ingredients with neutral roast sweet flavor except that before GC-MS analysis, 1ml of supernatant was put into a chromatographic flask, and 300. mu.L of BSTFA was added thereto and subjected to derivatization treatment in a water bath at 60 ℃ for 40 min.
TABLE 1 Retention time and Mass Spectrometry parameters for target Compounds and internal standards
Step 4, quantitatively measuring the roasted sweet and fragrant components in the smoke mouth by mouth
1) Respectively inserting the first heated cigarette and the second heated cigarette in the step 2 into a heated cigarette smoking set, and then installing the heated cigarette smoking set on a mouth-by-mouth smoking machine
The Cambridge filter sheet is used for collecting and heating particulate matters in the mainstream smoke of the cigarettes; starting the smoking set, starting the suction of the 1 st port immediately after preheating, and gradually sucking 8 channels until the first portAfter the suction of 8 channels is finished, the smoking set is taken down and the cigarettes are replaced. The pumping parameters were: aspiration volume 55mL, duration 2s, aspiration frequency 30 s. And (3) collecting 20 particles of the main stream smoke of the same mouth of the heated cigarette per 1 Cambridge filter, and collecting 40 particles of the main stream smoke of the same mouth of the cigarette per one mouth of the cigarette.
2) Determination of roasted sweet component
And (3) determination of neutral roasted sweet components: placing 2 filter discs containing the same-mouth particle phase substances into a 100mL conical flask with a plug, adding 50mL of extraction solution (the same extraction solution in the step 3), mechanically oscillating for 30min, standing for 5min, transferring the extract and the filter discs into a sand core funnel, carrying out primary filtration, and washing the triangular flask and the sand core funnel with 10mL of dichloromethane to obtain filtrate. Filtering the filtrate with 0.44 μm filter membrane to 100mL rotary evaporation bottle, concentrating to 2mL at 45 deg.C under normal pressure, filtering with 0.44 μm filter membrane, and performing GC-MS analysis under the same analysis conditions as in step 3.
And (3) determining the acid roasted sweet components: the same conditions as those in step (2) but requiring derivatization treatment before GC-MS analysis, specifically, 1ml of the concentrated solution is taken into a chromatographic bottle, 300. mu.L of BSTFA is added, and water bath at 60 ℃ is used for derivatization for 40 min.
Step 5, calculating formulas of the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomer spice in the mainstream smoke of the cigarette
Aiming at blank cigarettes and flavored cigarettes, the mass fractions of 6 baked sweet components in the cigarette slices and the mouth-to-mouth release amount of the baked sweet components in main stream smoke are respectively detected. The quantification was performed by an internal standard calibration method, i.e., the amount of the target compound (peak area of the target compound/peak area of the internal standard) × (mass of the internal standard/number of cigarettes).
The calculation formulas of the mouth-to-mouth transfer rate and the total transfer rate of the 6 kinds of baked sweet and fragrant monomer spices in the mainstream smoke of the cigarettes are shown in the formulas (1) and (2).
Mouth-to-mouth transfer rate: t isN＝(RAN-R0N)/(CmA-Cm0)×100％ (1)
The total transfer rate: t ═ RA-R0)/(CmA-Cm0)×100％ (2)
Wherein: rANThe release amount of the roasted sweet and fragrant components in the particle phase substances of the main stream smoke of the Nth opening of the flavored cigarette is mu g/piece;
R0Nthe release amount of the baked sweet components in the particle phase substances of the main stream smoke of the Nth mouth of the blank cigarette is mu g/cigarette;
CmA-the content of roasted sweet components in the flavored cigarette slices, μ g per cigarette;
Cm0-the content of roasted sweet components in the blank cigarette sheet, μ g/cigarette;
RAthe total release amount of the roasted sweet components in the main stream smoke particle phase substances of the flavored cigarettes is mu g/cigarette;
R0the total release amount of the baked sweet components in the particulate matters of the main stream smoke of the blank cigarette is mu g/cigarette.
The results of the measurement of the release amount of the roasted sweet monomers are shown in Table 2:
TABLE 2 mass fractions of 6 roasted sweet and fragrant components in heated cigarette flakes
After the mouth-to-mouth quantitative determination by the above roasted sweet and fragrant monomer components, the results are shown in tables 3 to 5 below.
TABLE 3 gradual release of 6 roasted sweet components in the mainstream smoke of blank cigarette
Note: -not detected
TABLE 4 gradual release of 6 roasted sweet components in mainstream Smoke of first heated cigarette
TABLE 5 gradual release of 6 roasted sweet components in mainstream of second heated cigarette
As can be seen from tables 3-5: the 6 baked sweet components are unevenly released when the cigarette is heated and smoked, and the total release amount of the baked sweet components shows a tendency of increasing firstly and then decreasing. In the first heated cigarette, the extreme value of the mouth-to-mouth release amount of the roasted sweet components except the methyl cyclopentenolone appears in the 3 rd mouth; in the second heated cigarette, the release amount of 6 baked sweet components appears to be extreme in the 4 th opening.
In sum, as the suction sequence becomes larger, the mouth-to-mouth transfer rate of the 6 roasted sweet and fragrant monomer spices in the mainstream smoke of the heated cigarette generally shows a trend of increasing first and then decreasing. When the addition amount is 0.1 per mill, the maximum value of the mouth-to-mouth transfer rate of the methylcyclopentadienyl alcohol ketone appears at the 4 th mouth, the maximum values of the mouth-to-mouth transfer rates of the other 5 roasted sweet monomer spices appear at the 3 rd mouth, and the maximum mouth-to-mouth transfer rate range is 5.4% -11.3%; when the addition amount is 0.5 per mill, the maximum value of the transfer rate of 6 roasted sweet monomer spices is shown in the 4 th mouth, and the maximum transfer rate of the roasted sweet monomer spices is 2.1-9.3 percent. Comparing the transfer rate per mouth of the same roasted sweet and fragrant monomer spice under two addition levels, the stability of the transfer rate per mouth under the addition level of 0.5 per mill is obviously superior to that under the addition level of 0.1 per mill. The adding amount of the baked sweet and fragrant monomer spice in the heated cigarette is controlled according to the range.
While there have been shown and described what are at present considered the preferred embodiments of the invention, the basic principles of the invention and the advantages thereof, it will be understood by those skilled in the art that the invention is not limited by the foregoing embodiments, which are merely illustrative of the principles of the invention, but various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (4)
1. A mouth-by-mouth transfer control method for heating sweet and fragrant monomers in cigarettes is characterized by comprising the following steps:
s1, detecting the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomers in the heated cigarette;
s2, determining the types of baked sweet and fragrant monomers to be added into the heated cigarette;
s3, determining the adding amount of the baking sweet and fragrant monomers to be added according to the types of the baking sweet and fragrant monomers to be added and the mouth-to-mouth transfer rate and the total transfer rate of the baking sweet and fragrant monomers.
2. The method of claim 1, wherein the monomer roasted sweet is at least one of furanone, 3, 4-dimethyl-1, 2-cyclopentadione, methylcyclopentadienolone, maltol, 4-methyl guaiacol, and ethyl maltol.
3. The method for controlling the mouth-to-mouth transfer of the baked sweet and fragrant monomers in the heated cigarette according to claim 1, wherein the method for detecting the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomers in the heated cigarette in the step S1 comprises the following steps:
step 1, preparation of flavoring solution
Weighing a set weight of roasted sweet and fragrant monomer perfume, and fixing the volume to a first set volume by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2 to serve as a first flavoring solution; transferring the first flavoring solution with a second set volume, and fixing the volume to the first set volume by using the mixed solution of the ethanol and the propylene glycol to be used as a second flavoring solution;
step 2, preparation of flavored and heated cigarettes
Respectively adding the first flavoring solution and the second flavoring solution prepared in the step 1 into blank heated cigarettes to prepare heated cigarettes with different addition amounts of the baked sweet and fragrant monomers, and respectively marking the heated cigarettes as a first heated cigarette and a second heated cigarette;
step 3, determining the roasted sweet and fragrant components in the cut tobacco of the blank heated cigarette
And (3) determination of neutral roasted sweet components: taking out tobacco shreds of blank heated cigarettes, crushing and sieving by a 40-mesh sieve to obtain tobacco powder, weighing 2g of tobacco powder into 100mL of conical bottles with plugs, adding 50mL of extraction solution containing 5 mu g/mL of n-heptadecane-containing dichloromethane solution, carrying out ultrasonic treatment for 30min, shaking uniformly, taking 5mL of supernate, sieving by a 0.44 mu m filter membrane, and carrying out GC-MS analysis on the filtrate;
and (3) determining the acid roasted sweet components: measurement of ingredients with neutral roasted sweet flavor except that before GC-MS analysis, 1ml of supernatant is taken to be put into a chromatographic bottle, 300 mu L of BSTFA is added, and derivatization treatment is carried out for 40min in water bath at 60 ℃;
step 4, quantitatively measuring the roasted sweet and fragrant components in the smoke mouth by mouth
1) Respectively inserting the first heated cigarette and the second heated cigarette in the step 2 into a heated cigarette smoking set, and then installing the heated cigarette smoking set on a mouth-by-mouth smoking machine
The Cambridge filter sheet is used for collecting and heating particulate matters in the mainstream smoke of the cigarettes;
2) determination of roasted sweet component
And (3) determination of neutral roasted sweet components: placing 2 filter discs containing the same-mouth particle phase substances in the step (1) into a 100mL conical flask with a plug, adding 50mL of extraction solution containing 5 mu g/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extraction liquid and the filter discs into a sand core funnel, carrying out primary filtration, and flushing 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, concentrating at 45 deg.C under normal pressure to 2mL, filtering with 0.44 μm filter membrane, and performing GC-MS analysis;
and (3) determining the acid roasted sweet components: the conditions are the same as those in the step (2), but derivatization treatment is needed before GC-MS analysis, specifically, 1ml of concentrated solution is taken into a chromatographic bottle, 300 mu L of BSTFA is added, and derivatization is carried out in a water bath at 60 ℃ for 40 min;
step 5, the calculation formula of the mouth-to-mouth transfer rate and the total transfer rate of the baked sweet and fragrant monomer spice in the mainstream smoke of the cigarette is as follows:
mouth-to-mouth transfer rate: t isN＝(RAN-R0N)/(CmA-Cm0)×100％ (1)
The total transfer rate: t ═ RA-R0)/(CmA-Cm0)×100％ (2)
Wherein: rANThe release amount of the roasted sweet and fragrant components in the particle phase substances of the main stream smoke of the Nth opening of the flavored cigarette is mu g/piece;
R0Nthe release amount of the baked sweet components in the particle phase substances of the main stream smoke of the Nth mouth of the blank cigarette is mu g/cigarette;
CmA-the content of roasted sweet components in the flavored cigarette slices, μ g per cigarette;
Cm0-the content of roasted sweet components in the blank cigarette sheet, μ g/cigarette;
RAthe total release amount of the roasted sweet components in the main stream smoke particle phase substances of the flavored cigarettes is mu g/cigarette;
R0the total release amount of the baked sweet components in the particulate matters of the main stream smoke of the blank cigarette is mu g/cigarette.
4. The method for controlling transfer of the roasted sweet and fragrant monomers in the heated cigarettes according to claim 3, wherein the addition amount of the roasted sweet and fragrant components in the first heated cigarette in the step 2 is 0.1% o, and the addition amount of the roasted sweet and fragrant components in the second heated cigarette is 0.5% o.
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