CN114088580B - Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol - Google Patents
Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol Download PDFInfo
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- CN114088580B CN114088580B CN202111284208.7A CN202111284208A CN114088580B CN 114088580 B CN114088580 B CN 114088580B CN 202111284208 A CN202111284208 A CN 202111284208A CN 114088580 B CN114088580 B CN 114088580B
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- propylene glycol
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 70
- 239000007788 liquid Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000009792 diffusion process Methods 0.000 title claims abstract description 24
- 241000208125 Nicotiana Species 0.000 claims description 76
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 76
- 229960004063 propylene glycol Drugs 0.000 claims description 61
- 235000013772 propylene glycol Nutrition 0.000 claims description 60
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000004445 quantitative analysis Methods 0.000 claims description 10
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 6
- 238000004817 gas chromatography Methods 0.000 claims description 6
- 238000002386 leaching Methods 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 235000019437 butane-1,3-diol Nutrition 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000779 smoke Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 230000000391 smoking effect Effects 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract description 2
- 238000000265 homogenisation Methods 0.000 abstract description 2
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N2013/003—Diffusion; diffusivity between liquids
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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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The application relates to a method for detecting the diffusion rate of a material liquid applied to a heated cigarette by using propylene glycol. The detection method is convenient, the detection result is accurate and reliable, the detection method can be used for determining the shelf life of the heated cigarettes, improving the smoking experience, determining the homogenization evaluation time of the products and reducing the storage time.
Description
Technical Field
The application belongs to the technical field of heated cigarettes, and particularly relates to a method for detecting the diffusion rate of a material liquid applied in a heated cigarette by using propylene glycol.
Background
With the rise of new tobacco in recent years, the new tobacco is gradually accepted by consumers due to lower hazard, and especially a few consumers in foreign countries, the heated cigarettes rapidly become new consumption hot spots in the cigarette market.
The tobacco rod forming process of orderly heated cigarettes is to continuously unreel special sheet tobacco by an unreeling device through a tobacco leaf base paper or sheet coil with a certain width (100-160 mm) and added with a fuming agent, convey the special sheet to a shredding device through a conveying roller set, cut tobacco into tobacco rods with a certain width, gather the tobacco rods into bundles through a tobacco rod gathering device, wrap the tobacco rods into tobacco rods by using forming paper, divide the tobacco rods into tobacco cores with a certain length through a tobacco rod dividing device, and then combine the tobacco cores with material functional sections into cigarettes.
For enriching smoke or creating heated cigarettes with different styles and tastes, a certain amount of feed liquid is usually applied in a tape casting mode by a feed liquid applying device before tobacco shreds are gathered into a bundle. Therefore, the applied feed liquid is generally arranged at the central position of the tobacco section, and the tobacco shreds which are directly contacted with the feed liquid in the cigarettes only account for about 10% of the total quantity of the tobacco shreds, so that the feed liquid is required to be gradually and uniformly dispersed through natural diffusion of the feed liquid. Because the boiling point of the heated cigarette feed liquid is generally higher, the diffusion speed is slower, and if the heated cigarette feed liquid does not reach a uniform state, the stability of the heated cigarette in mouth-by-mouth smoking can be affected.
Therefore, how to detect the diffusion rate and uniformity of the feed liquid, judge the proper pumping time and determine the shelf life becomes a difficult problem which puzzles the product development, the improvement of the perfuming system and the shelf life.
Disclosure of Invention
The application aims to provide a method for detecting the diffusion rate of a material liquid applied to a heated cigarette by using propylene glycol, so as to solve the problems that the prior art cannot accurately judge and detect the diffusion rate and uniformity of the material liquid, judge proper suction time and determine shelf life.
In order to achieve the above purpose, the application is realized by the following technical scheme:
a method for detecting the diffusion rate of an applied feed liquid in a heated cigarette by using propylene glycol, comprising the following steps:
s1, sampling reconstituted tobacco
Randomly selecting cut tobacco with set weight as a reconstituted tobacco sample after shredding the reconstituted tobacco;
s2, sampling the middle piece of cigarettes
Randomly sampling at the center of the cigarette and 1/3 of the outside of the cigarette respectively to obtain a sheet cigarette sample at the center of the cigarette and a sheet cigarette sample at 1/3 of the outside of the cigarette, and sealing the sheet cigarette samples for later use;
s3, extraction method of propylene glycol in tobacco flakes
(1) Method for leaching propylene glycol from feed liquid on surface of sheet smoke sample
Respectively weighing a piece of tobacco sample at the center of a cigarette in the step S2 and a piece of tobacco sample at 1/3 of the outer side of the cigarette, respectively placing the pieces of tobacco sample in a beaker, immersing the pieces of tobacco sample in methanol, controlling the leaching time to be a first set time +/-2S, filtering the pieces of tobacco sample, shaking up filtrate, taking 20.0 mu L of methanol solution of 1, 3-butanediol with the concentration of 30.0g/L, fixing the volume of the supernatant to 1mL, shaking up, carrying out quantitative analysis by using GC-MS, and measuring the content of propylene glycol in the feed liquid on the surfaces of the pieces of tobacco sample;
(2) Method for extracting propylene glycol from total amount of tobacco flake sample feed liquid
Determining the content of propylene glycol in the reconstituted tobacco sample in the step S1 and the sheet tobacco sample in the step S2 according to a gas chromatography, namely the content of propylene glycol in the reconstituted tobacco and the content of propylene glycol in the total amount of the sheet tobacco sample liquid;
s4, calculating method of feed liquid diffusion rate
e= (a-x)/(b-x) x 100%, wherein e is diffusion rate, unit is, a is propylene glycol content at 1/3 of the outer side of the cigarette, unit is mg/ml, b is propylene glycol content at the central position after feed liquid is applied, unit is mg/ml, and x is propylene glycol content in reconstituted tobacco, unit is mg/ml.
Further, in step S2, the single cigarette is sampled to not more than 20mg.
Further, the chromatographic column used for quantitative analysis by GC-MS was a 30 m.times.0.25 mm,0.25 μm polar elastic quartz capillary column.
Further, the gas chromatography conditions for quantitative analysis by GC-MS were as follows: 200 ℃; sample injection amount: 2. Mu.L; not split; carrier gas: he, constant flow rate: 1.0mL/min; programming temperature: the initial temperature is 50 ℃, the temperature is kept for 1min, the heating rate is 5 ℃/min to 200 ℃, and the temperature is kept for 3min; scanning mode: scan mode.
Further, mass spectrometry conditions for quantitative analysis by GC-MS were as follows: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450amu.
The beneficial effects of the application are as follows:
the detection method is convenient, the detection result is accurate and reliable, the detection method can be used for determining the shelf life of the heated cigarettes, improving the smoking experience, determining the homogenization evaluation time of the products and reducing the storage time.
Drawings
Figure 1 is a graph showing propylene glycol content at various locations in a cigarette over time.
Detailed Description
The following examples are given by way of illustration only and are not to be construed as limiting the scope of the application.
The principle of the technical scheme is that the characteristic that the tobacco material does not contain propylene glycol or contains less propylene glycol is utilized, in the application, the propylene glycol refers to 1, 2-propylene glycol, and the effect of the propylene glycol applied in the tobacco sheet raw material is that the aroma substances are carried out to form aerosol through vaporization and fogging, so that the smoking experience is satisfied. In actual production, the propylene glycol applied to the tobacco sheet raw material is generally between 2% and 05% of the weight percentage, and the propylene glycol in the applied feed liquid is used as a solvent, and the content of the propylene glycol accounts for 30% -50% of the total amount of the feed liquid, so that the technical scheme is used for detecting the content of the propylene glycol to prove the diffusion rate of the applied feed liquid in the heated cigarettes.
The technical scheme of the application is that the method for detecting the diffusion rate of the applied feed liquid in the heated cigarettes by using propylene glycol comprises the following steps:
s1, sampling reconstituted tobacco
Randomly selecting cut tobacco with set weight as a reconstituted tobacco sample after a shredding process of reconstituted tobacco (also called as a tobacco sheet raw material), and determining the propylene glycol content in the reconstituted tobacco sample through analysis of the reconstituted tobacco sample.
S2, sampling the middle piece of cigarettes
Selecting cigarettes prepared by the processes of feeding liquid and the like of the sliced cigarettes cut in the step S1, randomly sampling (each time a single cigarette is sampled by not more than 20 mg) at the center of the cigarettes and 1/3 of the outer sides of the cigarettes (1/3 of the outer sides of the cigarettes after trisecting from the center of the cigarettes to the outer sides), and sealing for later use.
S3, extracting method of propylene glycol from tobacco surface feed liquid
In the application, propylene glycol in the tobacco flakes is improved by adopting a leaching method, specifically referring to a method established by Severson and the like, and the specific steps are as follows: weighing 15g (accurate to 0.0001 g) of the sheet tobacco sample, placing the sheet tobacco sample in a 500ml beaker, immersing the sheet tobacco sample in 300ml of methanol, and controlling the leaching time to be set value +/-2 s; filtering out the sheet tobacco, shaking the filtrate uniformly, taking 20.0 mu L of 1, 3-butanediol (internal standard) methanol solution with the concentration of 30.0g/L, fixing the volume to 1mL by using the supernatant of the filtrate, shaking the supernatant uniformly, carrying out quantitative analysis by using GC-MS, and measuring the content of 1, 2-propanediol in the surface feed liquid of the sheet tobacco.
Likewise, the extraction of propylene glycol from reconstituted tobacco samples was also performed using the procedure described above.
And determining the content of propylene glycol in the feed liquid of the sheet tobacco sample at the center of the cigarette by a gas chromatography method, wherein the content is the content of the propylene glycol in the total amount of the sheet tobacco feed liquid.
In the application, the quantitative analysis is carried out by using an Agilent7890A-5973GC-MS gas chromatograph-mass spectrometer in the United states. (1) chromatography column: DB-WAX chromatographic column (30 m x 0.25mm,0.25 μm) polar elastic quartz capillary column. (2) gas chromatography conditions: sample inlet temperature: 200 ℃; sample injection amount: 2. Mu.L; not split; carrier gas: he, constant flow rate: 1.0mL/min; programming temperature: the initial temperature is 50 ℃, the temperature is kept for 1min, the heating rate is 5 ℃/min to 200 ℃, and the temperature is kept for 3min; scanning mode: scan mode. (3) Mass Spectrometry conditions: ionization mode: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450amu.
The calculation formula of the feed liquid diffusion rate is e= (a-x)/(b-x) x 100%, wherein e is the diffusion rate, a is the propylene glycol content at 1/3 of the outer side of the cigarette, b is the propylene glycol content at the central position after feed liquid application, x is the propylene glycol content in reconstituted tobacco, and x is mg/ml.
The propylene glycol content of the cigarette at the center of the cigarette is 1.12mg/mL, the propylene glycol content of the cigarette at the 1/3 position at the outer side of the cigarette is 1.14mg/mL, and the propylene glycol content of the reconstituted tobacco is 0.84mg/mL. As shown in figure 1, the propylene glycol content at different positions in a cigarette of a certain brand is shown as a histogram of change of the propylene glycol content along with the storage time, as can be seen from figure 1, the propylene glycol content at different positions in the cigarette is close to the propylene glycol content at the time of 14 days in storage, the propylene glycol content at different positions is basically unchanged after 17 days, and the time of more than 3 days is required for heating the cigarettes to start delivery to the tobacco company to sell to retailers and then to the consumers at the highest time, so that the storage time can be determined as the storage time plus the transfer time is more than or equal to 10 days, if the time to the consumers is 14 days, the propylene glycol content at different positions in the cigarette can be delivered on the production day, if the time to the consumers is 3 days, the propylene glycol content at different positions can be delivered after the storage time is 7 days, and warehouse occupation is reduced.
The present application is not limited to the above embodiments, but is not limited to the above embodiments, and any person skilled in the art will have obvious modifications and modifications equivalent to those of the equivalent embodiments, and can make various changes and modifications without departing from the scope of the present application.
Claims (6)
1. A method for detecting the diffusion rate of an applied feed liquid in a heated cigarette by using propylene glycol, which is characterized by comprising the following steps:
s1, sampling reconstituted tobacco
Randomly selecting cut tobacco with set weight as a reconstituted tobacco sample after shredding the reconstituted tobacco;
s2, sampling the middle piece of cigarettes
Randomly sampling at the center of the cigarette and 1/3 of the outside of the cigarette respectively to obtain a sheet cigarette sample at the center of the cigarette and a sheet cigarette sample at 1/3 of the outside of the cigarette, and sealing the sheet cigarette samples for later use;
s3, extraction method of propylene glycol in tobacco flakes
(1) Method for leaching propylene glycol from feed liquid on surface of sheet smoke sample
Respectively weighing a piece of tobacco sample at the center of a cigarette in the step S2 and a piece of tobacco sample at 1/3 of the outer side of the cigarette, respectively placing the pieces of tobacco sample in a beaker, immersing the pieces of tobacco sample in methanol, controlling the leaching time to be a first set time +/-2S, filtering the pieces of tobacco sample, shaking up filtrate, taking 20.0 mu L of methanol solution of 1, 3-butanediol with the concentration of 30.0g/L, fixing the volume of the supernatant to 1mL, shaking up, carrying out quantitative analysis by using GC-MS, and measuring the content of 1, 2-propanediol in the feed liquid on the surfaces of the pieces of tobacco sample;
(2) Method for extracting propylene glycol from total amount of tobacco flake sample feed liquid
Determining the content of propylene glycol in the reconstituted tobacco sample in the step S1 and the sheet tobacco sample in the step S2 according to a gas chromatography, namely the content of propylene glycol in the reconstituted tobacco and the content of propylene glycol in the total amount of the sheet tobacco sample liquid;
s4, calculating method of feed liquid diffusion rate
e= (a-x)/(b-x) x 100%, wherein e is diffusion rate, unit is, a is propylene glycol content at 1/3 of the outer side of the cigarette, unit is mg/ml, b is propylene glycol content at the central position after feed liquid is applied, unit is mg/ml, and x is propylene glycol content in reconstituted tobacco, unit is mg/ml.
2. The method for detecting a diffusion rate of an applied liquid in a heated cigarette using propylene glycol according to claim 1, wherein in step S2, each sample of a single cigarette is not more than 20mg.
3. The method for detecting the diffusion rate of a liquid applied to a heated cigarette by using propylene glycol according to claim 1, wherein the chromatographic column for quantitative analysis by GC-MS is a 30m x 0.25mm,0.25 μm polar elastic quartz capillary column.
4. The method for detecting the diffusion rate of a liquid applied to a heated cigarette by using propylene glycol according to claim 3, wherein the gas chromatography conditions for quantitative analysis by GC-MS are as follows: 200 ℃; sample injection amount: 2. Mu.L; not split; carrier gas: he, constant flow rate: 1.0mL/min; programming temperature: the initial temperature is 50 ℃, the temperature is kept for 1min, the heating rate is 5 ℃/min to 200 ℃, and the temperature is kept for 3min; scanning mode: scan mode.
5. The method for detecting the diffusion rate of a feed liquid applied to a heated cigarette by using propylene glycol according to claim 1, wherein the mass spectrometry conditions for quantitative analysis by GC-MS are as follows: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450amu.
6. The method for detecting the rate of diffusion of an applied liquid in a heated cigarette using propylene glycol according to claim 1, wherein the single cigarette is sampled no more than 20mg per sample.
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2021
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CN103063755A (en) * | 2012-11-16 | 2013-04-24 | 红云红河烟草(集团)有限责任公司 | Method for measuring absorption rate and effective absorption ratio of feed liquid of flue-cured tobacco lamina |
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