CN113671063A - Method for measuring ester transfer rate in heated cigarette - Google Patents
Method for measuring ester transfer rate in heated cigarette Download PDFInfo
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- CN113671063A CN113671063A CN202110786179.8A CN202110786179A CN113671063A CN 113671063 A CN113671063 A CN 113671063A CN 202110786179 A CN202110786179 A CN 202110786179A CN 113671063 A CN113671063 A CN 113671063A
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 295
- 150000002148 esters Chemical class 0.000 title claims abstract description 79
- 238000012546 transfer Methods 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000779 smoke Substances 0.000 claims abstract description 78
- 239000000178 monomer Substances 0.000 claims abstract description 51
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 34
- 239000002304 perfume Substances 0.000 claims abstract description 24
- 235000013599 spices Nutrition 0.000 claims abstract description 22
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 78
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 66
- 239000007788 liquid Substances 0.000 claims description 55
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- 239000000243 solution Substances 0.000 claims description 50
- 230000000391 smoking effect Effects 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 26
- 238000012417 linear regression Methods 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 24
- 238000005303 weighing Methods 0.000 claims description 24
- 239000013618 particulate matter Substances 0.000 claims description 23
- 241000208125 Nicotiana Species 0.000 claims description 22
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 22
- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 22
- MDHYEMXUFSJLGV-UHFFFAOYSA-N phenethyl acetate Chemical compound CC(=O)OCCC1=CC=CC=C1 MDHYEMXUFSJLGV-UHFFFAOYSA-N 0.000 claims description 18
- SESFRYSPDFLNCH-UHFFFAOYSA-N benzyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1=CC=CC=C1 SESFRYSPDFLNCH-UHFFFAOYSA-N 0.000 claims description 16
- 238000004364 calculation method Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- UWKAYLJWKGQEPM-LBPRGKRZSA-N linalyl acetate Chemical compound CC(C)=CCC[C@](C)(C=C)OC(C)=O UWKAYLJWKGQEPM-LBPRGKRZSA-N 0.000 claims description 14
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 claims description 14
- -1 n-heptadecane dichloromethane Chemical compound 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 13
- ZOZIRNMDEZKZHM-UHFFFAOYSA-N Phenethyl phenylacetate Chemical compound C=1C=CC=CC=1CCOC(=O)CC1=CC=CC=C1 ZOZIRNMDEZKZHM-UHFFFAOYSA-N 0.000 claims description 12
- 238000005086 pumping Methods 0.000 claims description 12
- 239000013068 control sample Substances 0.000 claims description 11
- 238000011010 flushing procedure Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 11
- KBEBGUQPQBELIU-CMDGGOBGSA-N Ethyl cinnamate Chemical compound CCOC(=O)\C=C\C1=CC=CC=C1 KBEBGUQPQBELIU-CMDGGOBGSA-N 0.000 claims description 8
- 229960002903 benzyl benzoate Drugs 0.000 claims description 8
- KBEBGUQPQBELIU-UHFFFAOYSA-N cinnamic acid ethyl ester Natural products CCOC(=O)C=CC1=CC=CC=C1 KBEBGUQPQBELIU-UHFFFAOYSA-N 0.000 claims description 8
- JLIDRDJNLAWIKT-UHFFFAOYSA-N 1,2-dimethyl-3h-benzo[e]indole Chemical compound C1=CC=CC2=C(C(=C(C)N3)C)C3=CC=C21 JLIDRDJNLAWIKT-UHFFFAOYSA-N 0.000 claims description 7
- DULCUDSUACXJJC-UHFFFAOYSA-N benzeneacetic acid ethyl ester Natural products CCOC(=O)CC1=CC=CC=C1 DULCUDSUACXJJC-UHFFFAOYSA-N 0.000 claims description 7
- CCRCUPLGCSFEDV-UHFFFAOYSA-N cinnamic acid methyl ester Natural products COC(=O)C=CC1=CC=CC=C1 CCRCUPLGCSFEDV-UHFFFAOYSA-N 0.000 claims description 7
- UWKAYLJWKGQEPM-UHFFFAOYSA-N linalool acetate Natural products CC(C)=CCCC(C)(C=C)OC(C)=O UWKAYLJWKGQEPM-UHFFFAOYSA-N 0.000 claims description 7
- 229940095102 methyl benzoate Drugs 0.000 claims description 7
- CCRCUPLGCSFEDV-BQYQJAHWSA-N methyl trans-cinnamate Chemical compound COC(=O)\C=C\C1=CC=CC=C1 CCRCUPLGCSFEDV-BQYQJAHWSA-N 0.000 claims description 7
- 239000000523 sample Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- UFLHIIWVXFIJGU-ARJAWSKDSA-N (Z)-hex-3-en-1-ol Chemical compound CC\C=C/CCO UFLHIIWVXFIJGU-ARJAWSKDSA-N 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 239000000796 flavoring agent Substances 0.000 claims description 2
- 235000019634 flavors Nutrition 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 238000005809 transesterification reaction Methods 0.000 claims 1
- 238000007865 diluting Methods 0.000 description 9
- 238000011068 loading method Methods 0.000 description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- MIYFJEKZLFWKLZ-UHFFFAOYSA-N Phenylmethyl benzeneacetate Chemical compound C=1C=CC=CC=1COC(=O)CC1=CC=CC=C1 MIYFJEKZLFWKLZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention relates to a method for measuring the ester transfer rate in a heated cigarette, which utilizes a GC-MS analysis method to measure the mass fraction of 9 ester aroma components in a cigarette sheet and the mouth-to-mouth release amount in main stream smoke under two addition amounts, and explores the transfer behavior of 9 ester monomer spices in the heated cigarette. The result shows that with the increase of the number of the suction openings, the gradually released amounts of the 9 ester monomer spices in the particulate matters in the main stream smoke of the heated cigarette tend to increase firstly and then decrease, and the sum of the gradually released amounts has good linear positive correlation with the number of the suction openings; the mouth-to-mouth transfer rate of 9 ester monomer perfumes is concentrated on the 3 rd to 4 th mouths and the total transfer, and the transfer rate is measured by utilizing a function of a linear relation. The method can accurately measure the esters in the heated cigarette, can quickly analyze the transfer rate of the esters in the heated cigarette, and provides data support for the application of the ester monomer spice in the heated cigarette.
Description
Technical Field
The invention belongs to the technical field of cigarette performance measurement, and particularly relates to a method for measuring ester transfer rate in a heated cigarette.
Background
The ester monomer spice is a common cigarette spice, generally has sweet aroma, fruit aroma or flower aroma, is coordinated with cigarette aroma, and is widely used in cigarette blending. For heating cigarettes, the fruity sweet style characteristics can be endowed by adding the ester monomer spice, and an effective fragrance compensation effect can be achieved.
However, no report is found on the mouth-to-mouth transfer behavior study of the ester monomer perfume in the heated cigarette so far. Therefore, 9 ester monomer spices are taken as objects, the release amount of the ester monomer spices in the mainstream smoke of the heated cigarette is analyzed, the transfer behavior of the ester monomer spices in the mainstream smoke of the heated cigarette is researched, and the data support is provided for the application of the ester monomer spices in the heated cigarette.
Disclosure of Invention
The invention aims to provide a method for measuring the ester transfer rate in a heated cigarette, so as to solve the problem that no clear detection data exists in the mouth-to-mouth transfer of ester monomer spices in the heated cigarette.
In order to realize the purpose, the invention is realized by the following technical scheme:
a method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing any one of 9 ester monomer perfumes to a first set mass, and using a mixed solution of ethanol and propylene glycol to fix the volume to a first set volume to serve as a first perfuming solution of each ester monomer;
weighing the first flavoring liquid with a second set volume, and fixing the volume to a third set volume by using a mixed solution of ethanol and propylene glycol to serve as the second flavoring liquid of each ester monomer;
2) preparation of flavored cigarette
Placing the blank cigarettes in a constant temperature and humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for a first set time, and respectively injecting the first flavoring liquid and the second flavoring liquid into different blank cigarettes according to the fourth set volume to obtain flavored cigarettes which are respectively marked as flavored cigarettes A and flavored cigarettes B; placing the flavored cigarette in a constant temperature and humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for balancing for at least a second set time;
3) mainstream smoke total particulate matter collection
After the flavored cigarette is inserted into a heating cigarette smoking set, the flavored cigarette is installed in a single-channel smoking machine, a Cambridge filter disc is installed in a catcher, and the mouth-by-mouth mainstream smoke particle phase components of the flavored cigarette are respectively caught under a set smoking mode;
4) pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; filtering the filtrate with 0.44 μm needle filter to 100mL rotary evaporation bottle, concentrating to 2mL under 45 deg.C and normal pressure, filtering with 0.44 μm filter membrane, and performing GC-MS analysis;
5) pretreatment of control sample
Taking out thin shreds from blank cigarette branches, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, performing ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and performing GC-MS analysis;
6) calculation of transfer Rate
Respectively detecting the mass fractions of 9 ester aroma components in a cigarette sheet and the mouth-to-mouth release amount in main stream smoke aiming at a blank cigarette, a flavored cigarette A and a flavored cigarette B, and respectively calculating the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of the 9 ester monomer spices in a cigarette main stream smoke particle phase object according to formulas (1) to (3);
oral release amount ═ C1N-C0N (1)
Oral transfer rate ═ C1N-C0N)/(Cm1-Cm0)×100％ (2)
Total transfer rate ═ C1-C0)/(Cm1-Cm0)×100％ (3)
Wherein: c1NRepresents the per-mouth release amount of the particulate matters in the main stream smoke of the flavored cigarettes, namely mu g/per cigarette;
C0Nindicating the mouth-to-mouth release amount of particulate matters in the main stream smoke of the blank cigarette, namely mu g/cigarette;
Cm1represents the mass fraction in the sheet of flavoured cigarettes, μ g/count;
Cm0represents the mass fraction in the flakes of the blank cigarette, μ g/cigarette;
C1represents the total release amount of particulate matters in the main stream smoke of the flavored cigarette, and the content is mu g/cigarette;
C0the total release amount of particulate matters in the main stream smoke of the blank cigarette is expressed, and the content is microgram/cigarette;
7) taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Preferably, the 9 ester monomer perfumes are respectively ethyl acetate, methyl benzoate, ethyl phenylacetate, linalyl acetate, phenethyl acetate, methyl cinnamate, ethyl cinnamate, benzyl benzoate and phenethyl phenylacetate.
Preferably, the volume ratio of ethanol to propylene glycol in the mixed solution of ethanol and propylene glycol is 1: 2.
Preferably, the first set time and the second set time are both 48 hours.
Preferably, in step 3), the suction mode is set to 55mL per suction volume, 2s duration and 30s suction interval.
Preferably, in step 3), 20 cigarettes of the mouth of the heated cigarette are collected by each cambridge filter, and 40 cigarettes of the mouth of the heated cigarette are collected by each mouth of the heated cigarette.
Preferably, the chromatographic conditions of the GC-MS analysis are that the injection port temperature is: 290 ℃; temperature rising procedure:
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 scan mode acquisition mass number range: 40 to 350.
The invention has the beneficial effects that:
the method can accurately measure the esters in the heated cigarette, can quickly analyze the mouth-to-mouth transfer rate of the esters in the heated cigarette, and provides data support for the application of ester monomer spices in the heated cigarette.
Drawings
Fig. 1 to 9 are graphs of transfer rates of leaf alcohol acetate, methyl benzoate, ethyl phenylacetate, linalyl acetate, phenethyl acetate, methyl cinnamate, ethyl cinnamate, benzyl benzoate and phenethyl phenylacetate in particulate matters of mainstream smoke of a heated cigarette.
Detailed Description
The technical solution is described in detail by the following embodiments, which are only exemplary and can be used to explain and illustrate the technical solution of the present invention, but not to be construed as limiting the technical solution of the present invention.
The technical scheme aims at the analysis of 9 ester monomer spices as detection objects, and the 9 ester monomer spices are respectively acetic acid leaf alcohol ester, methyl benzoate, ethyl phenylacetate, linalyl acetate, phenethyl acetate, methyl cinnamate, ethyl cinnamate, benzyl benzoate and phenethyl phenylacetate.
In the following examples 1 to 9, the detection methods and procedures were the same, except that the ester-based monomer perfumes were the above-mentioned 9 types. And the calculation formulas of the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of the ester monomer spices in the particulate matters of the main stream smoke of the cigarettes are calculated according to the formula in the embodiment 1, so the description in the embodiments 2 to 9 is not repeated.
Example 1
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of folic acetate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P1;
accurately transferring 2ml of the first flavoring liquid P1, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H1.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P1 and the second flavoring liquid H1 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A1 and a flavored cigarette B1; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Cambridge filter is loaded into the trap and under a set suction mode (55 mL of suction volume per port, 2s duration, between suctions)Every 30 seconds, a bell-shaped curve) to respectively capture the grain phase components of the main stream smoke one by one (8 mouths) of the flavored cigarette; each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
GC-MS analysis of chromatographic conditions
A chromatographic column: j. the design is a square&W122-5563 (60 m.times.0.25 mm. times.1 μm); sample inlet temperature: 290 ℃; temperature rising procedure:
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 to 350.
6) Calculation of transfer Rate
Aiming at a blank cigarette, a flavored cigarette A1 and a flavored cigarette B1, the mass fraction of the folic alcohol acetate in the cigarette sheet and the mouth-to-mouth release amount in the mainstream smoke are respectively detected, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of the folic alcohol acetate in the mainstream smoke particulate matters of the cigarettes are respectively calculated according to formulas (1) to (3) in example 1, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 2
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of methyl benzoate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P2;
accurately transferring 2ml of the first flavoring liquid P2, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H2.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P2 and the second flavoring liquid H2 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A2 and a flavored cigarette B2; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each Cambridge filter sheet collects 20 cigarettes, and each filter sheet collects 40 cigarettesAnd (4) phase material.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
For a blank cigarette, a flavored cigarette A2 and a flavored cigarette B2, the mass fraction of methyl benzoate in a cigarette sheet and the mouth-to-mouth release amount in main stream smoke are respectively detected, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of methyl benzoate in a cigarette main stream smoke particle phase are respectively calculated according to formulas (1) to (3) in example 1, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 3
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of ethyl phenylacetate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P3;
accurately transferring 2ml of the first flavoring liquid P3, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H3.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P3 and the second flavoring liquid H3 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A3 and a flavored cigarette B3; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
Aiming at a blank cigarette, a flavored cigarette A3 and a flavored cigarette B3, the mass fraction of ethyl phenylacetate in a cigarette sheet and the mouth-to-mouth release amount in main stream smoke are respectively detected, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of ethyl phenylacetate in a cigarette main stream smoke particle phase substance are respectively calculated according to formulas (1) to (3) in example 1, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 4
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of linalyl acetate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P4;
accurately transferring 2ml of the first flavoring liquid P4, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H4.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P4 and the second flavoring liquid H4 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A4 and a flavored cigarette B4; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
Aiming at a blank cigarette, a flavored cigarette A4 and a flavored cigarette B4, the mass fraction of the linalyl acetate in the cigarette sheet and the mouth-to-mouth release amount in the main stream smoke are respectively detected, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of the linalyl acetate in the main stream smoke particle phase of the cigarette are respectively calculated according to formulas (1) to (3) in example 1, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 5
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of phenethyl acetate, fixing the volume to 10ml by using a mixed solution of ethanol and propylene glycol with the volume ratio of 1:2, and shaking up to obtain a first flavoring solution P5;
accurately transferring 2ml of the first flavoring liquid P5, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H5.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P5 and the second flavoring liquid H5 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A5 and a flavored cigarette B5; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
The mass fraction of phenethyl acetate in the cigarette sheet and the mouth-to-mouth release amount in the mainstream smoke of the cigarette were respectively detected for a blank cigarette, a flavored cigarette A5 and a flavored cigarette B5, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of phenethyl acetate in the particulate matters of the mainstream smoke of the cigarette were respectively calculated according to the formulas (1) to (3) in example 1, as shown in Table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 6
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of methyl cinnamate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P6;
accurately transferring 2ml of the first flavoring liquid P6, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H6.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P6 and the second flavoring liquid H6 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A6 and a flavored cigarette B6; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
Aiming at a blank cigarette, a flavored cigarette A6 and a flavored cigarette B6, the mass fraction of methyl cinnamate in a cigarette slice and the mouth-to-mouth release amount in main stream smoke are respectively detected, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of methyl cinnamate in cigarette main stream smoke particulate matters are respectively calculated according to formulas (1) to (3) in the embodiments, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 7
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of ethyl cinnamate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P7;
accurately transferring 2ml of the first flavoring liquid P7, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H7.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P7 and the second flavoring liquid H7 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A7 and a flavored cigarette B7; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
Aiming at a blank cigarette, a flavored cigarette A7 and a flavored cigarette B7, the mass fraction of ethyl cinnamate in a cigarette slice and the mouth-to-mouth release amount in main stream smoke are respectively detected, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of ethyl cinnamate in cigarette main stream smoke particle phase substances are respectively calculated according to formulas (1) to (3) in example 1, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 8
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of benzyl benzoate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P8;
accurately transferring 2ml of the first flavoring liquid P8, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H8.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P8 and the second flavoring liquid H8 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A8 and a flavored cigarette B8; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
Aiming at a blank cigarette, a flavored cigarette A8 and a flavored cigarette B8, the mass fraction of the benzyl benzoate in the cigarette sheet and the mouth-to-mouth release amount in the mainstream smoke are respectively detected, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of the benzyl benzoate in the cigarette mainstream smoke particle phase are respectively calculated according to formulas (1) to (3) in example 1, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
Example 9
A method for measuring the ester transfer rate in a heated cigarette comprises the following steps:
1) preparation of perfuming solutions
Weighing 0.25g (accurate to 0.0001g) of phenethyl phenylacetate, metering to 10ml by using a mixed solution of ethanol and propylene glycol in a volume ratio of 1:2, and shaking up to obtain a first flavoring solution P9;
accurately transferring 2ml of the first flavoring liquid P9, and diluting to 10ml with a mixed solution of ethanol and propylene glycol at a volume ratio of 1:2 to obtain a second flavoring liquid H9.
2) Preparation of flavored cigarette
Placing blank cigarettes in a constant-temperature and constant-humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for 48 hours, and respectively injecting the first flavoring liquid P9 and the second flavoring liquid H9 into different blank cigarettes in an amount of 0.48 mu L, wherein 40 blank cigarettes are respectively injected for later use to obtain flavored cigarettes which are respectively marked as a flavored cigarette A9 and a flavored cigarette B9; the flavored cigarette is put in a constant temperature and humidity box with the temperature of 22 plus or minus 2 ℃ and the relative humidity of 60 plus or minus 5 percent to be balanced for at least 48 hours.
3) Mainstream smoke total particulate matter collection
Inserting the flavored cigarette into a heating cigarette smoking set, and installing the flavored cigarette in a single-channel smoking machine
Loading the Cambridge filter into a catcher, and respectively catching grain phase components (8 mouths) of the mainstream smoke one by one of flavored cigarettes under a set suction mode (the suction volume per mouth is 55mL, the duration is 2s, the suction interval is 30s, and a bell-shaped curve); each cambridge filter sheet collects 20 cigarettes, and each cambridge filter sheet collects 40 cigarettes.
4) Pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; the filtrate was filtered through a 0.44 μm needle filter into a 100mL rotary evaporator, concentrated to 2mL at 45 ℃ under normal pressure, filtered through a 0.44 μm filter, and subjected to GC-MS analysis.
5) Pretreatment of control sample
Taking out the thin shreds from the blank cigarette, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, carrying out ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and carrying out GC-MS analysis.
The GC-MS analysis chromatographic conditions were the same as in example 1.
6) Calculation of transfer Rate
The mass fraction of phenethyl acetate in the cigarette sheet and the mouth-to-mouth release amount in the main stream smoke are respectively detected aiming at a blank cigarette, a flavored cigarette A9 and a flavored cigarette B9, and the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of the phenethyl acetate in the cigarette main stream smoke particle phase are respectively calculated according to formulas (1) to (3) in example 1, which is shown in the table I.
7) Taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
TABLE retention time and Mass Spectrometry parameters for 9 ester Compounds and internal standards
TABLE II standard deviation of 9 ester compounds
Calculating according to the formula (1), and obtaining the mouth-to-mouth release amount of the 9 ester monomer spices in the particulate matters of the main stream smoke of the heated cigarette, wherein the results are shown in the third table and the fourth table.
Table III perfuming and heating 9 ester monomer perfumes in main stream smoke particle phase substance of cigarette A
TABLE 4 gradual release amount of 9 ester monomer perfumes in main stream smoke particulate matter of four flavored heating cigarettes B
From the third table and the fourth table, it can be known that 9 ester aroma components are non-uniformly released when the cigarette is heated and smoked under the two addition amounts of 0.1 per thousand and 0.5 per thousand, and the release amount per one mouth is increased firstly and then decreased gradually. When the addition amount is 1 per mill, the maximum value of the mouth-by-mouth release amount is concentrated in the 3 rd to 5 th mouths. When the addition amount is 5 per mill, the maximum of the mouth-to-mouth release amount is concentrated in the 3 rd mouth and the 4 th mouth.
And (3) performing linear regression treatment by taking the suction mouth sequence N as an x axis and taking the sum of the mouth-to-mouth release amount as a y axis to obtain a linear regression equation and correlation coefficients of the mouth-to-mouth release amount and the suction mouth number of the 9 ester monomer perfumes, wherein the results are shown in a table five.
Table five 9 linear regression equation and correlation coefficient of mouth-to-mouth release amount and suction mouth number of ester monomer perfume
From Table five, R of the linear regression equation2All of the above-mentioned ingredients are greater than 0.99, which shows that the sum of the mouth-to-mouth release amounts of the 9 ester monomer perfumes with different addition amounts has good linear positive correlation with the number of the pumping openings. The above results indicate that although 9 ester monomer flavors do not migrate uniformly in heated cigarettes, the amount released is between the number of puffsThere is an inherent regularity.
The mouth-to-mouth transfer rate of the 9 ester monomer spices in the particulate matters of the main stream smoke of the heated cigarette is obtained by calculation according to the formula (2), and the results are shown in figures 1 to 9.
As can be seen from fig. 1 to 9, as the number of the smoking openings increases, the mouth-to-mouth transfer rate of particulate matters of the mainstream smoke of the heated cigarette generally shows a trend of increasing and then decreasing, and the mouth-to-mouth transfer rate is less than 10.0%. Under two addition amounts, the single-port transfer rates are respectively 0.7-8.0% and 0.4-7.7%, and the maximum values are mainly concentrated in the 3 rd to 4 th ports.
The calculation is carried out by utilizing the formula (3), the total transfer rate of the 9 ester monomer spices in the particulate matters of the main stream smoke of the heated cigarette is obtained, and the result is shown in the sixth table.
Total transfer rate of 9 ester monomer spices in Table six heated cigarettes
From table six, it can be seen that: under the condition of two addition amounts, the total transfer rates of the 9 ester monomer spices in the particulate matters of the main stream smoke of the heated cigarette are respectively 9.8-52.8% and 4.9-50.2%. Wherein, the total transfer rate of 5 ester monomer perfumes of the ethyl acetate, the ethyl cinnamate, the benzyl benzoate, the benzyl phenylacetate and the phenethyl phenylacetate is greater than 5 thousandths when the addition amount is 1 thousandth, and the balance of 4 ester monomer perfumes is vice versa.
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 (7)
1. A method for measuring the ester transfer rate in a heated cigarette is characterized by comprising the following steps:
1) preparation of perfuming solutions
Weighing any one of 9 ester monomer perfumes to a first set mass, and using a mixed solution of ethanol and propylene glycol to fix the volume to a first set volume to serve as a first perfuming solution of each ester monomer;
weighing the first flavoring liquid with a second set volume, and fixing the volume to a third set volume by using a mixed solution of ethanol and propylene glycol to serve as the second flavoring liquid of each ester monomer;
2) preparation of flavored cigarette
Placing the blank cigarettes in a constant temperature and humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for a first set time, and respectively injecting the first flavoring liquid and the second flavoring liquid into different blank cigarettes according to the fourth set volume to obtain flavored cigarettes which are respectively marked as flavored cigarettes A and flavored cigarettes B; placing the flavored cigarette in a constant temperature and humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5% for balancing for at least a second set time;
3) mainstream smoke total particulate matter collection
After the flavored cigarette is inserted into a heating cigarette smoking set, the flavored cigarette is installed in a single-channel smoking machine, a Cambridge filter disc is installed in a catcher, and the mouth-by-mouth mainstream smoke particle phase components of the flavored cigarette are respectively caught under a set smoking mode;
4) pretreatment of total particulate matter in mainstream smoke
After the pumping is finished, placing the Cambridge filter disc into a 100mL conical flask with a plug, adding 50mL of a5 mu G/mL n-heptadecane dichloromethane solution, mechanically oscillating for 30min, standing for 5min, transferring the extract liquid and the filter disc into a G3 sand core funnel for filtering, and flushing the conical flask and the sand core funnel with 10mL of dichloromethane to obtain a filtrate; filtering the filtrate with 0.44 μm needle filter to 100mL rotary evaporation bottle, concentrating to 2mL under 45 deg.C and normal pressure, filtering with 0.44 μm filter membrane, and performing GC-MS analysis;
5) pretreatment of control sample
Taking out thin shreds from blank cigarette branches, crushing and sieving by a 40-mesh sieve to obtain thin pieces of tobacco powder, weighing the second set mass of thin pieces of tobacco powder into a 100mL conical flask with a plug, adding 50mL dichloromethane solution containing 5 mu g/mL n-heptadecane, performing ultrasonic treatment for 30min, shaking up, taking 5mL, filtering by a 0.44 mu m filter membrane, and performing GC-MS analysis;
6) calculation of transfer Rate
Respectively detecting the mass fractions of 9 ester aroma components in a cigarette sheet and the mouth-to-mouth release amount in main stream smoke aiming at a blank cigarette, a flavored cigarette A and a flavored cigarette B, and respectively calculating the mouth-to-mouth release amount, the mouth-to-mouth transfer rate and the total transfer rate of the 9 ester monomer spices in a cigarette main stream smoke particle phase object according to formulas (1) to (3);
oral release amount ═ C1N-C0N (1)
Oral transfer rate ═ C1N-C0N)/(Cm1-Cm0)×100％ (2)
Total transfer rate ═ C1-C0)/(Cm1-Cm0)×100％ (3)
Wherein: c1NRepresents the per-mouth release amount of the particulate matters in the main stream smoke of the flavored cigarettes, namely mu g/per cigarette;
C0Nindicating the mouth-to-mouth release amount of particulate matters in the main stream smoke of the blank cigarette, namely mu g/cigarette;
Cm1represents the mass fraction in the sheet of flavoured cigarettes, μ g/count;
Cm0represents the mass fraction in the flakes of the blank cigarette, μ g/cigarette;
C1represents the total release amount of particulate matters in the main stream smoke of the flavored cigarette, and the content is mu g/cigarette;
C0the total release amount of particulate matters in the main stream smoke of the blank cigarette is expressed, and the content is microgram/cigarette;
7) taking the number of suction openings as an x axis and the sum of the mouth-to-mouth release amount as a y axis, and performing linear regression treatment to obtain a linear regression equation and a correlation coefficient of the mouth-to-mouth release amount and the number of the suction openings of the ester monomer perfume:
y-bx + a, where a is a constant and b is a coefficient.
2. The method for determining the ester transfer rate in the heated cigarette according to claim 1, wherein the 9 ester monomer flavors are folic alcohol acetate, methyl benzoate, ethyl phenylacetate, linalyl acetate, phenethyl acetate, methyl cinnamate, ethyl cinnamate, benzyl benzoate, and phenethyl phenylacetate, respectively.
3. The method for measuring the ester transfer rate in the heated cigarette according to claim 1, wherein the volume ratio of ethanol to propylene glycol in the mixed solution of ethanol and propylene glycol is 1: 2.
4. The method of claim 1, wherein the first set time and the second set time are both 48 hours.
5. The method for measuring the transesterification rate in the heated cigarette according to claim 1, wherein in the step 3), the smoking mode is set to 55mL per puff volume, 2s duration and 30s smoking interval.
6. The method for determining the ester transfer rate of the heated cigarette according to claim 1, wherein in the step 3), 20 mainstream smoke particulate matters of the mouth of the heated cigarette are collected by each Cambridge filter, and 40 mainstream smoke particulate matters of the mouth of the heated cigarette are collected by each mouth.
7. The method for determining the ester transfer rate in the heated cigarette according to claim 1, wherein the chromatographic conditions of GC-MS analysis are that the injection port temperature is: 290 ℃; 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 scan mode acquisition mass number range: 40 to 350.
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