CN114088580A - Method for detecting diffusion rate of feed liquid applied in heated cigarette by using propylene glycol - Google Patents
Method for detecting diffusion rate of feed liquid applied in heated cigarette by using propylene glycol Download PDFInfo
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- CN114088580A CN114088580A CN202111284208.7A CN202111284208A CN114088580A CN 114088580 A CN114088580 A CN 114088580A CN 202111284208 A CN202111284208 A CN 202111284208A CN 114088580 A CN114088580 A CN 114088580A
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 title claims abstract description 181
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 59
- 239000007788 liquid Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000009792 diffusion process Methods 0.000 title claims abstract description 24
- 241000208125 Nicotiana Species 0.000 claims abstract description 85
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 85
- 238000000605 extraction Methods 0.000 claims abstract description 5
- 229960004063 propylene glycol Drugs 0.000 claims description 56
- 235000013772 propylene glycol Nutrition 0.000 claims description 55
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000005070 sampling Methods 0.000 claims description 12
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 10
- 238000004445 quantitative analysis Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000004817 gas chromatography Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000001914 filtration 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
- 239000006228 supernatant 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
- PBVNQZNFWRISBX-UHFFFAOYSA-N butane-1,3-diol;methanol Chemical compound OC.CC(O)CCO PBVNQZNFWRISBX-UHFFFAOYSA-N 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000001819 mass spectrum Methods 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 230000000391 smoking effect Effects 0.000 abstract description 4
- 238000005520 cutting process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 238000005144 WAX chromatography Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 230000004075 alteration Effects 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
- 235000019437 butane-1,3-diol Nutrition 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization 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
- 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 invention relates to a method for detecting the diffusion rate of feed liquid applied in a heated cigarette by using propylene glycol, which comprises the steps of selecting reconstituted tobacco cut tobacco used for producing cigarettes and cigarettes produced by using the reconstituted tobacco cut tobacco, respectively detecting the content of propylene glycol in the reconstituted tobacco cut tobacco, the content of propylene glycol on the surface of cut tobacco at the center of the cigarettes and the content of propylene glycol on the surface of cut tobacco at the outer side 1/3 of the cigarettes by adopting an extraction method, and calculating the diffusion rate of the propylene glycol by using a formula. The detection method is convenient and fast, has accurate and reliable detection results, can be used for determining the shelf period of the heated cigarettes, improving the smoking experience, determining the time for evaluating the product homogeneity and reducing the storage time.
Description
Technical Field
The invention belongs to the technical field of heated cigarettes, and particularly relates to a method for detecting the diffusion rate of an applied feed liquid in a heated cigarette by using propylene glycol.
Background
With the rise of novel tobacco in recent years, the novel tobacco is gradually accepted by consumers due to lower harmfulness, and particularly, the novel tobacco has a large number of consumers abroad, so that the cigarette heating is a new consumption hotspot in the cigarette market rapidly.
A technology for forming the tobacco strips of orderly heated cigarettes includes such steps as continuously unwinding the raw tobacco leaves or coiled tobacco sheets (100-160 mm) with smoke generating agent, conveying the tobacco sheets to a cutting unit, cutting the tobacco shreds into strips, collecting the tobacco shreds in a bundle, wrapping the strips with paper, cutting to obtain tobacco cores, and combining them with functional material segments.
In order to enrich smoke or create heated cigarettes with different styles and tastes, a certain amount of feed liquid is applied through a feed liquid applying device in a flow casting mode before tobacco shreds are gathered into bundles. Therefore, the applied feed liquid is generally in the center of the tobacco section, the cut tobacco in the cigarette directly contacted with the feed liquid only accounts for about 10 percent of the total amount of the cut tobacco, and the feed liquid is required to be gradually uniform through the natural diffusion of the feed liquid. Because the boiling point of the liquid material for heating the cigarette is generally higher and the diffusion speed is slower, if the liquid material does not reach a uniform state, the stability of mouth-to-mouth smoking of the heated cigarette is influenced.
Therefore, how to detect the diffusion rate and uniformity of the feed liquid, judge the appropriate pumping time and determine the shelf life becomes a difficult problem which troubles the product development, the flavoring system modification and the shelf life.
Disclosure of Invention
The invention aims to provide a method for detecting the diffusion rate of feed liquid applied in a heated cigarette by using propylene glycol, so as to solve the problems that the diffusion rate and uniformity of the feed liquid cannot be accurately judged and detected, the proper suction time cannot be judged, and the shelf life cannot be determined in the prior art.
In order to realize the purpose, the invention 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 comprises the following steps:
s1 sampling reconstituted tobacco
After the reconstituted tobacco is shredded, randomly selecting cut tobaccos with set weight as reconstituted tobacco samples;
s2 sampling the middle tobacco
Randomly sampling at the circle center of the cigarette and the outer side 1/3 of the cigarette respectively to obtain a chip sample at the circle center of the cigarette and a chip sample at the outer side 1/3 of the cigarette, and sealing the chip samples for later use;
s3 method for extracting propylene glycol from tobacco flakes
(1) Method for extracting propylene glycol from feed liquid on surface of tobacco slice sample
Respectively weighing a sheet tobacco sample at the center of the cigarette in the step S2 and a sheet tobacco sample at the outer side 1/3 of the cigarette with set weights, respectively placing the sheet tobacco samples in beakers, immersing the sheet tobacco samples with methanol, controlling the extraction time to be within +/-2S of a first set time, filtering out the sheet tobacco samples, shaking up the filtrate, taking 20.0 mu L of 1, 3-butanediol methanol solution with the concentration of 30.0g/L, using the supernatant of the filtrate to fix the volume to 1mL, shaking up the filtrate, carrying out quantitative analysis by GC-MS, and determining the content of propylene glycol in the feed liquid on the surface of the sheet tobacco sample;
(2) method for extracting propylene glycol from total amount of feed liquid of tobacco flake sample
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 determining the content of propylene glycol in the reconstituted tobacco and the content of propylene glycol in the total amount of the feed liquid of the sheet tobacco sample;
s4 and calculation method of diffusion rate of feed liquid
And e is (a-x)/(b-x) x 100%, wherein e is the diffusion rate and is the unit, a is the content of propylene glycol at 1/3 positions on the outer side of the cigarette and is the unit of mg/ml, b is the content of propylene glycol at the central position after the feed liquid is applied and is the unit of mg/ml, and x is the content of propylene glycol in the reconstituted tobacco and is the unit of mg/ml.
Further, in step S2, each sampling of a single cigarette does not exceed 20 mg.
Further, the column 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, injection port temperature: 200 ℃; sample introduction amount: 2 mu L of the solution; no flow diversion; carrier gas: he, constant flow rate: 1.0 mL/min; temperature programming: 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 3 min; the scanning mode is as follows: scan mode.
Further, mass spectrometry conditions for quantitative analysis by GC-MS were, ionization: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450 amu.
The invention has the beneficial effects that:
the detection method is convenient and fast, has accurate and reliable detection results, can be used for determining the shelf period of the heated cigarettes, improving the smoking experience, determining the time for evaluating the product homogeneity and reducing the storage time.
Drawings
FIG. 1 is a graph showing the change of propylene glycol content in a cigarette at different positions with respect to storage time.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and explaining the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
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 propylene glycol applied to the tobacco sheet raw material has the effect of bringing out aroma substances to form aerosol through vaporization and fogging, so that the smoking experience is met. In actual production, the content of 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% to 50% of the total amount of the feed liquid, so that the diffusion rate of the applied feed liquid in the heated cigarette is proved by detecting the content of the propylene glycol through the technical scheme.
The technical scheme of the application is that the method for detecting the diffusion rate of the feed liquid applied in the heated cigarette by using the propylene glycol comprises the following steps:
s1 sampling reconstituted tobacco
After the reconstituted tobacco (also called as tobacco sheet raw material) is subjected to a shredding process, randomly selecting cut tobaccos with set weight as reconstituted tobacco samples, and determining the content of propylene glycol in the reconstituted tobacco samples through analysis of the reconstituted tobacco samples.
S2 sampling the middle tobacco
Selecting the cigarettes prepared by the process of adding the feed liquid and the like to the cut tobacco sheets in the step S1, randomly sampling (each sampling of a single cigarette is not more than 20mg) at the circle center of each cigarette and the outer side 1/3 of each cigarette (which means 1/3 which is divided into three parts from the circle center to the outer side and is close to the outer side of each cigarette), and sealing for later use.
S3 method for extracting propylene glycol from tobacco lamina surface material liquid
In the application, the 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 method comprises the following specific steps: weighing 15g (accurate to 0.0001g) of the tobacco flake sample, placing the tobacco flake sample in a 500ml beaker, immersing the tobacco flake sample in 300ml of methanol, and controlling the extraction time to be a set value +/-2 s; filtering out the tobacco flakes, shaking the filtrate evenly, taking 20.0 mu L of methanol solution of 1, 3-butanediol (internal standard) with the concentration of 30.0g/L, fixing the volume to 1mL by using the supernatant of the filtrate, shaking the filtrate evenly, carrying out quantitative analysis by GC-MS, and determining the content of 1, 2-propanediol in the feed liquid on the surface of the tobacco flakes.
Similarly, the extraction of the propylene glycol in the reconstituted tobacco sample is also carried out by adopting the steps.
And (3) determining the content of propylene glycol in the feed liquid of the tobacco slice sample at the circle center of the cigarette according to the gas chromatography, wherein the content of propylene glycol is the total amount of the tobacco slice feed liquid.
In this application, quantitative analysis was performed using an Agilent7890A-5973 GC-MS. (1) A chromatographic column: DB-WAX chromatography column (30m x 0.25mm, 0.25 μm) polar elastic quartz capillary column. (2) Gas chromatography conditions: sample inlet temperature: 200 ℃; sample introduction amount: 2 mu L of the solution; no flow diversion; carrier gas: he, constant flow rate: 1.0 mL/min; temperature programming: 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 3 min; the scanning mode is as follows: scan mode. (3) Mass spectrum conditions: an ionization mode: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450 amu.
The calculation formula of the diffusion rate of the feed liquid is that e is (a-x)/(b-x) x 100 percent, wherein e is the diffusion rate and the unit is percent, a is the content of propylene glycol at 1/3 positions outside the cigarettes and the unit is mg/ml, b is the content of the propylene glycol at the central position after the feed liquid is applied and the unit is mg/ml, and x is the content of the propylene glycol in the reconstituted tobacco and the unit is mg/ml.
The content of propylene glycol in the center of a certain brand of cigarette is 1.12mg/mL, the content of propylene glycol in the outer side 1/3 of the cigarette is 1.14mg/mL, and the content of propylene glycol in the reconstituted tobacco is 0.84mg/mL through gas chromatography detection. As shown in figure 1, the bar chart shows the change of the content of propylene glycol at different positions in a certain brand of cigarette along with the storage time, as can be seen from figure 1, the content of the propylene glycol at different positions in the cigarette is close to that at 14 days of storage, the content of the propylene glycol at different positions basically does not change after 17 days, the heated cigarette is considered to be sold from the beginning to a tobacco company to a retailer, and then needs more than 3 days at the fastest speed in the hands of a consumer, so that the storage time and the transportation time are determined to be more than or equal to 10 days, if the time in the hands of the consumer is 14 days, the heated cigarette can be delivered on the same production day, if the time in the hands of the consumer is 3 days, the heated cigarette can be delivered after 7 days, and the warehouse occupation is reduced.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A method for detecting the diffusion rate of an applied feed liquid in a heated cigarette by using propylene glycol is characterized by comprising the following steps:
s1 sampling reconstituted tobacco
After the reconstituted tobacco is shredded, randomly selecting cut tobaccos with set weight as reconstituted tobacco samples;
s2 sampling the middle tobacco
Randomly sampling at the circle center of the cigarette and the outer side 1/3 of the cigarette respectively to obtain a chip sample at the circle center of the cigarette and a chip sample at the outer side 1/3 of the cigarette, and sealing the chip samples for later use;
s3 method for extracting propylene glycol from tobacco flakes
(1) Method for extracting propylene glycol from feed liquid on surface of tobacco slice sample
Respectively weighing a sheet tobacco sample at the center of the cigarette in the step S2 and a sheet tobacco sample at the outer side 1/3 of the cigarette with set weights, respectively placing the sheet tobacco samples in beakers, immersing the sheet tobacco samples with methanol, controlling the extraction time to be within +/-2S of a first set time, filtering out the sheet tobacco samples, shaking up filtrate, taking 20.0 mu L of 1, 3-butanediol methanol solution with the concentration of 30.0g/L, using the supernatant of the filtrate to fix the volume to 1mL, shaking up, carrying out quantitative analysis by GC-MS, and determining the content of 1, 2-propanediol in feed liquid on the surface of the sheet tobacco sample;
(2) method for extracting propylene glycol from total amount of feed liquid of tobacco flake sample
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 determining the content of propylene glycol in the reconstituted tobacco and the content of propylene glycol in the total amount of the feed liquid of the sheet tobacco sample;
s4 and calculation method of diffusion rate of feed liquid
And e is (a-x)/(b-x) x 100%, wherein e is the diffusion rate and is the unit, a is the content of propylene glycol at 1/3 positions on the outer side of the cigarette and is the unit of mg/ml, b is the content of propylene glycol at the central position after the feed liquid is applied and is the unit of mg/ml, and x is the content of propylene glycol in the reconstituted tobacco and is the unit of mg/ml.
2. The method for detecting the diffusion rate of an applied liquid in the heated cigarette by using the propylene glycol as claimed in claim 1, wherein in the step S2, each sampling of a single cigarette is not more than 20 mg.
3. The method for detecting the diffusion rate of an applied liquid in 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 the feed liquid applied in the heated cigarette by using the propylene glycol as claimed in claim 3, wherein the gas chromatography conditions in the quantitative analysis by the GC-MS are that the injection port temperature is: 200 ℃; sample introduction amount: 2 mu L of the solution; no flow diversion; carrier gas: he, constant flow rate: 1.0 mL/min; temperature programming: 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 3 min; the scanning mode is as follows: scan mode.
5. The method for detecting the diffusion rate of an applied feed liquid in a heated cigarette by using propylene glycol according to claim 1, wherein the mass spectrum conditions in the quantitative analysis by GC-MS are ionization mode: EI; ion source temperature: 230 ℃; transmission line temperature: 230 ℃; scanning range: 33-450 amu.
6. The method of claim 1, wherein each sample of a single cigarette does not exceed 20mg per sample.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 rate of tobacco lamina feed liquid |
| EP2617299A1 (en) * | 2012-01-18 | 2013-07-24 | Delfortgroup AG | Paper filled with tobacco particles |
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| WO2020232970A1 (en) * | 2019-05-17 | 2020-11-26 | 江南大学 | Method for determining short chain fatty acid content in intestinal contents or excrement |
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2021
- 2021-11-01 CN CN202111284208.7A patent/CN114088580B/en active Active
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| EP2617299A1 (en) * | 2012-01-18 | 2013-07-24 | Delfortgroup AG | Paper filled with tobacco particles |
| 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 rate of tobacco lamina feed liquid |
| CN103983705A (en) * | 2014-04-17 | 2014-08-13 | 江苏中烟工业有限责任公司 | Method for determination of material liquid retention ratio in cut cigarette tobacco preparation |
| WO2020232970A1 (en) * | 2019-05-17 | 2020-11-26 | 江南大学 | Method for determining short chain fatty acid content in intestinal contents or excrement |
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Non-Patent Citations (2)
| Title |
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| 刘菲;赵明月;余祥英;曾世通;胡军;: "超声提取-GC/MS法测定烟叶中的烷烃", 烟草科技, no. 01 * |
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