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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
propylene glycol
cigarette
tobacco
sample
feed liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202111284208.7A
Other languages
Chinese (zh)
Other versions
CN114088580A (en
Inventor
宋伟民
尹献忠
王帝
芦昶彤
张喆
桂鹏
张孟伟
朱琦
郑峰洋
王宏伟
杨志强
郑凯
赵永振
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Tobacco Henan Industrial Co Ltd
Original Assignee
China Tobacco Henan Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Tobacco Henan Industrial Co Ltd filed Critical China Tobacco Henan Industrial Co Ltd
Priority to CN202111284208.7A priority Critical patent/CN114088580B/en
Publication of CN114088580A publication Critical patent/CN114088580A/en
Application granted granted Critical
Publication of CN114088580B publication Critical patent/CN114088580B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N2013/003Diffusion; diffusivity between liquids

Landscapes

  • 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

Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol
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.
CN202111284208.7A 2021-11-01 2021-11-01 Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol Active CN114088580B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111284208.7A CN114088580B (en) 2021-11-01 2021-11-01 Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111284208.7A CN114088580B (en) 2021-11-01 2021-11-01 Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol

Publications (2)

Publication Number Publication Date
CN114088580A CN114088580A (en) 2022-02-25
CN114088580B true CN114088580B (en) 2023-12-15

Family

ID=80298551

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111284208.7A Active CN114088580B (en) 2021-11-01 2021-11-01 Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol

Country Status (1)

Country Link
CN (1) CN114088580B (en)

Citations (5)

* Cited by examiner, † Cited by third party
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 ratio of feed liquid of flue-cured tobacco lamina
EP2617299A1 (en) * 2012-01-18 2013-07-24 Delfortgroup AG Paper filled with tobacco particles
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
CN110726648A (en) * 2019-10-25 2020-01-24 中国烟草总公司郑州烟草研究院 Method for characterizing diffusion rate of glycerol solution system in tobacco sheet
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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 ratio of feed liquid of flue-cured tobacco lamina
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
CN110726648A (en) * 2019-10-25 2020-01-24 中国烟草总公司郑州烟草研究院 Method for characterizing diffusion rate of glycerol solution system in tobacco sheet

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
章平泉 ; 徐光忠 ; 陆斌 ; .卷烟烟丝中1,2-丙二醇和丙三醇含量测试方法的改进.辽宁化工.2020,(第04期),全文. *
超声提取-GC/MS法测定烟叶中的烷烃;刘菲;赵明月;余祥英;曾世通;胡军;;烟草科技(第01期);全文 *

Also Published As

Publication number Publication date
CN114088580A (en) 2022-02-25

Similar Documents

Publication Publication Date Title
AU2015341517B2 (en) Container containing a nicotine solution
RU2672027C2 (en) Solution containing nicotine in unprotonated form and protonated form
Borgerding et al. The chemical composition of smokeless tobacco: a survey of products sold in the United States in 2006 and 2007
Peace et al. Evaluation of nicotine and the components of e-liquids generated from e-cigarette aerosols
EP2434913B1 (en) Tobacco smoke filter
WO2005041151A2 (en) Tobacco product labeling system
Stepanov et al. Levels of (S)-N′-nitrosonornicotine in US tobacco products
EP3804534A1 (en) Apparatus and method for manufacturing cut reconstituted tobaccos
CN114062537B (en) Method for accurately detecting diffusion rate of applied feed liquid in heated cigarettes
CN114088580B (en) Method for detecting diffusion rate of applied feed liquid in heated cigarettes by using propylene glycol
Koszowski et al. Nicotine content and physical properties of large cigars and cigarillos in the United States
Cheng et al. Harmful and potentially harmful constituents in the filler and smoke of tobacco-containing tobacco products
CN108936800B (en) Tobacco hollow particle, preparation method thereof and cigarette filter stick
CN114088581B (en) Method for detecting diffusion rate of applied feed liquid in heated cigarettes
Rehder Silinski et al. Analysis of Nicotine and Non-nicotine Tobacco Constituents in Aqueous Smoke/Aerosol Extracts by UHPLC and Ultraperformance Convergence Chromatography–Tandem Mass Spectrometry
Li et al. Direct Determination of Free Nicotine Content in Tobacco
CN114088584B (en) Detection and correction method for diffusion rate of applied feed liquid in heating cigarette
CN105823839B (en) Piece cigarette absorbs the evaluation method of feed liquid effect during a kind of leaves storage
Jeong et al. Comparison of the content of tobacco alkaloids and tobacco-specific nitrosamines in ‘heat-not-burn’tobacco products before and after aerosol generation
CN114088583B (en) Method for establishing diffusion model of applied feed liquid in heating cigarette
CN114088582B (en) Method for stabilizing diffusion rate of applied feed liquid in heating cigarette
Edwards et al. Quantitative measurement of harmful and potentially harmful constituents, pH, and moisture content in 16 commercial smokeless tobacco products
Azeez et al. Assessment of Cr, Cd and Pb levels in tobacco leaves and selected cigarette samples from Ilorin Metropolis Kwara State, Nigeria
Borgerding et al. Determination of nicotine in tobacco, tobacco processing environments and tobacco products
Fischer et al. Improved method for the determination of tobacco-specific nitrosamines (TSNA) in tobacco smoke

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right

Effective date of registration: 20230802

Address after: No.16 Yulin South Road, Zhengdong New District, Zhengzhou City, Henan Province

Applicant after: CHINA TOBACCO HENAN INDUSTRIAL Co.,Ltd.

Address before: No.16 Yulin South Road, Zhengdong New District, Zhengzhou City, Henan Province

Applicant before: CHINA TOBACCO HENAN INDUSTRIAL Co.,Ltd.

Applicant before: HENAN AGRICULTURAL University

TA01 Transfer of patent application right
GR01 Patent grant
GR01 Patent grant