NL2036104A - Method for tracking release pattern of volatile substance in tobacco - Google Patents

Method for tracking release pattern of volatile substance in tobacco Download PDF

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Publication number
NL2036104A
NL2036104A NL2036104A NL2036104A NL2036104A NL 2036104 A NL2036104 A NL 2036104A NL 2036104 A NL2036104 A NL 2036104A NL 2036104 A NL2036104 A NL 2036104A NL 2036104 A NL2036104 A NL 2036104A
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tobacco
release pattern
volatile substance
smoke
monitoring
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NL2036104A
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Dutch (nl)
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Li Dan
Li Chao
Liu Yang
Li Weixue
Wang Huiping
Cai Jieyun
Zhang Xiaowei
Gu Jianlong
Gu Lili
Gao Li
Long Jie
Yang Farong
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Univ Kunming Science & Technology
Yunnan Tobacco Quality Supervision And Testing Station
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Publication of NL2036104A publication Critical patent/NL2036104A/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/067Preparation by reaction, e.g. derivatising the sample
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N30/14Preparation by elimination of some components
    • G01N2030/143Preparation by elimination of some components selective absorption
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The present disclosure relates to the field of capture and detection of volatile substances in tobacco, and in particular to a method for tracking a release pattern of a volatile substance in tobacco. The method includes: introducing, by gas blowing, smoke into an absorption container holding an absorbent to generate an absorption solution, and subjecting the absorption solution to gas chromatography - mass spectrometry (GC-MS). Compared to the method for capturing smoke by a smoking machine and a Cambridge filter, the present disclosure has the advantages of low cost and simple operation. In the present disclosure, the environmental atmosphere, heating program, gas blowing time, and absorbent volume of the capture process are all controllable. In addition, diversif1ed pre-treatment conditions can be provided as needed, such as specific purif1cation treatment, to reduce interference from non-target substances. Therefore, the present disclosure provides an effective approach for analyzing the release pattern of tobacco smoke.

Description

METHOD FOR TRACKING RELEASE PATTERN OF VOLATILE
SUBSTANCE IN TOBACCO
TECHNICAL FIELD
The present disclosure relates to the field of capture and detection of volatile substances in tobacco, and in particular to a method for tracking a release pattern of a volatile substance in tobacco.
BACKGROUND
The smoke generated by heated tobacco includes various volatile substances, and multi-dimensional acquisition and detection of these volatile substances can provide data support for the analysis of tobacco aroma and taste. Common methods for capturing the volatile components in tobacco include Cambridge filter capture, electrostatic precipitation capture, cold trap capture, and adsorption tube capture. Cambridge filter capture has good repeatability, but it has high cost and complex analysis, limiting its large-scale promotion. Electrostatic precipitation capture has good test repeatability and low background interference during analysis, but it is prone to the formation of ozone and artificial products, resulting in inaccurate analysis results. Cold trap capture can reduce the occurrence of side reactions and has high accuracy, but it requires no moisture in the sample, which limits its application. In adsorption tube capture, the adsorption tube has a simple structure and is easy to operate, but if the adsorption material is broken, it will lead to inaccurate test results. In order to comprehensively understand the release pattern of the volatile substance in tobacco, the capture method must maximize the acquisition efficiency of the volatile substance from the device to the process, and must be able to specifically acquire a certain type of substance.
Therefore, there is a need for a method for tracking a release pattern of a volatile substance in tobacco.
SUMMARY
An objective of the present disclosure is to propose a method for tracking a release pattern of a volatile substance in tobacco. The present disclosure achieves release and capture of smoke at gradient temperatures under different atmospheres.
To solve the above technical problem, the present disclosure adopts the following technical solution.
The method for tracking a release pattern of a volatile substance in tobacco includes the following steps: blowing smoke, generated by heating a tobacco sample by a gradient smoke release device, into an absorption container holding an absorbent to generate an absorption solution, and subjecting the absorption solution to gas chromatography - mass spectrometry (GC-MS).
Further, the method includes: treating, if a target analyte is not nicotine, the absorption solution with a molecularly imprinted solid-phase extraction column or through derivatization to reduce a high-content nicotine component; and filtering, by a 0.22 pum organic-phase microporous filter membrane, the absorption solution after nicotine reduction treatment for GC-MS.
Further, the gradient smoke release device includes a quartz tube; the quartz tube is provided therein with a quartz boat; the quartz boat is heated by a tube furnace; and the tube furnace is connected to a thermocouple and a temperature controller; one end of the quartz tube is provided with a gas connector; the gas connector is provided with a push rod; the gas connector is connected to two gas tubes through a three-way tube; and the two gas tubes are respectively connected to gas supply devices, and each are provided with a pressure reducing valve and a rotameter; the other end of the quartz tube forms an outlet end connected to multiple first outlet tubes and provided with a temperature sensor; the first outlet tubes each are provided with a solenoid valve; the thermocouple, the temperature controller, the temperature sensor, and the solenoid valve are connected to an external controller; and the controller is connected to a visual operation screen; and a tail end of each of the first outlet tubes is connected to a first absorption container; the first absorption container is placed in a cooling tank; and the first absorption container is provided with a second outlet tube.
Further, the gas supply devices include an air supply device and a nitrogen supply device.
Further, the tobacco sample heated has a mass of 0.1-12 g.
Further, the blowing is gas blowing carried out at 0.1-100 mL/min, preferably 10 mL/min.
Further, the tobacco sample is heated at 0.1-30°C/min, preferably 15°C/min, to 15-
1,200°C, preferably 250°C.
Further, the absorbent has a volume of 0.1-150 mL, preferably 60 mL.
Further, the absorbent is at -10-25°C, preferably 0°C.
Further, all electrical components are powered by an external power source.
Further, the thermocouple, the temperature controller, the solenoid valve, the temperature sensor, the controller, the tube furnace, and the visual operation screen are all commercially available, and their internal structures and circuit connections are well - known in this art.
Further, the smoke is analyzed by GC-MS.
GC conditions: Agilent DB-5MS chromatographic column (30 m = 0.25 mm x 0.25 um); injection port temperature: 250°C; splitless injection; injection volume: 0.1 pL; carrier gas: high-purity helium (99.999%)};, and temperature programming for chromatographic column: holding 80°C for 2 min, rising to 110°C at 10°C/min, holding for 1 min, rising to 240°C at 3°C/min, and holding for 5 min.
MS conditions: ion source (electron impact (ED); full scan mode (Scan); scanning range: 45-500 amu; total ion chromatogram (TIC); ion source temperature: 230°C; and quadrupole temperature: 150°C.
Further, the volatile substance in the tobacco includes nicotine, organic acids, aldehydes, ketones, and alcohols.
Further, the tobacco sample includes a flue-cured tobacco product and a heated tobacco product.
Compared with the prior art, the present disclosure has at least one of the following beneficial effects. 1. Compared to the method for capturing smoke by a smoking machine and a
Cambridge filter, the present disclosure has the advantages of low cost and simple operation. In the present disclosure, the environmental atmosphere, heating program, gas blowing time, and absorbent volume of the capture process are all controllable. In addition, diversified pre-treatment conditions can be provided as needed, such as specific purification treatment, to reduce interference from non-target substances. Therefore, the present disclosure provides an effective approach for analyzing the release pattern of tobacco smoke. 2. The present disclosure controls the environmental atmosphere of volatile substances released from tobacco through a capture device. The present disclosure can dilute the environmental atmosphere through air and nitrogen, and can also provide atmospheres with different oxygen contents, such as 5% or 10%. 3. The present disclosure can set the heating program of the tube furnace to control the heating rate of different temperature ranges, thereby acquiring the continuous release pattern of volatile substances under different heating programs or the volatile substance composition of tobacco at various temperatures. Therefore, the present disclosure can explore the migration patterns of different substances with heating temperature, providing basic data for setting the appropriate temperature for tobacco smoke or heated cigarettes. 4. The present disclosure captures all the smoke components of tobacco in the absorption container through the capture device. Compared to traditional capture methods, the present disclosure simplifies the operation steps and reduces smoke loss. 5. The present disclosure utilizes the molecularly imprinted solid-phase extraction column or derivatization method to treats the absorption solution of tobacco smoke generated through heating and absorption, so as to reduce the high-content nicotine component, facilitating accurate detection of other volatile components.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a structural diagram of a method for tracking a release pattern of a volatile substance in tobacco according to the present disclosure;
FIG. 2 is a connection diagram of a quartz tube and first outlet tubes according to the present disclosure;
FIG. 3 is a total ion chromatograph (TIC) of Hongda C3F flue-cured tobacco from
Mile City, Honghe Hani and Yi Autonomous Prefecture, Yunnan Province, China; and
FIG. 4 is a TIC of Hongda C3F flue-cured tobacco after derivatization.
Reference Numerals: 1. gas supply device; 2. pressure reducing valve; 3. rotameter; 4. push rod; 5. gas connector; 6. quartz tube; 7. tube furnace; 8. quartz boat; 9. thermocouple; 10. temperature controller; 11. first absorption container; 12. cooling tank; 16. first outlet tube; 17. solenoid valve; and 18. second outlet tube.
DETAILED DESCRIPTION OF THE EMBODIMENTS
To make the objectives, technical solutions, and advantages of the present disclosure clearer, the present disclosure is described in further detail below with reference to the drawings (FIGS. 1 to 4) and examples. It should be understood that the specific examples are merely intended to explain the present disclosure, rather than to limit the present disclosure.
In an example, a gradient smoke release device includes quartz tube 6. The quartz tube 6 is provided therein with quartz boat 8, and the quartz boat is heated by tube furnace 7. The tube furnace 7 is connected to thermocouple 9 and temperature controller 10.
One end of the quartz tube 6 is provided with gas connector 5. The gas connector 5 is provided with push rod 4, and the gas connector 5 is connected to two gas tubes through a three-way tube. The two gas tubes are respectively connected to gas supply devices 1. The gas tubes each are provided with pressure reducing valve 2 and rotameter 3.
The other end of the quartz tube 6 forms an outlet end connected to multiple first outlet tubes 16 and provided with a temperature sensor. The first outlet tubes 16 each are provided with solenoid valve 17. The thermocouple 9, the temperature controller 10, the temperature sensor, and the solenoid valve 17 are connected to an external controller.
The controller is connected to a visual operation screen.
A tail end of each of the first outlet tubes 16 is connected to first absorption container 11. The first absorption container 11 is placed in cooling tank 12. The first absorption container 11 is provided with second outlet tube 18.
When in use, the quartz boat 8 with a tobacco sample is put into the quartz tube 6, and the tube furnace 7 is turned on for heating. Thus, the tube furnace 7 heats the tobacco sample in the quartz boat 8 to generate smoke.
Instruments, Reagents, and Materials:
GC-MS instrument: Agilent 7890B-5977A (Agilent Technologies (Shanghai) Co.,
Ltd.); BTF-1200C-S tube furnace (Anhui BEQ Equipment Technology Co., Ltd.); digital thermostatic water bath (Jintan Chengdong Xinrui Instrument Plant); dichloromethane (chromatographically pure, Oceanpak), n,o-bis(trimethylsilyl)trifluoroacetamide (BSTFA) (Tan-Mo Technology Co., Ltd.); and Hongda C3F flue-cured tobacco planted in Mile City, Honghe Hani and Yi Autonomous Prefecture, Yunnan Province, China, provided by Yunnan Tobacco Quality Supervision and Test Station.
GC-MS conditions: GC conditions: Agilent DB-5M-UI chromatographic column (30 m x 0.25 mm ~ 0.25 um); injection port temperature: 250°C; splitless injection;
injection volume: 0.1 pL; carrier gas: high-purity helium (99.999%); and temperature programming for chromatographic column: holding 80°C for 2 min, rising to 110°C at 10°C/min, holding for 1 min, rising to 240°C at 3°C/min, and holding for 5 min.
MS conditions: ion source (electron impact (EI)); full scan mode (Scan); scanning range: 45-500 amu; total ion chromatogram (TIC); ion source temperature: 230°C; and quadrupole temperature: 150°C.
Example 1
A temperature programming method was adopted. That is, a temperature was raised to 150°C at 15°C/min, the temperature was then held for 10 min, and then air blew at 10 mL/min for 75 min, thereby acquiring smoke at 0-150°C. In this way, 0.1 g of Hongda
C3F tobacco powder was gradually heated to 150°C, 200°C, 250°C, 300°C, 350°C, and 400°C. Specifically, during heating, smoke at different temperatures was controlled by the controller to enter different first outlet tubes 16, and then enter different first absorption containers 11 for absorption. For example, 0-150°C smoke entered first- position first outlet tube 16, and 151-200°C smoke entered a second-position first outlet tube 16. When the smoke was at 0-150°C, the temperature sensor detected and transmitted a temperature signal to the controller. Thus, the controller enabled the solenoid valve of the first-position first outlet tube 16 to open, allowing smoke to enter a first absorption container for absorption. When the smoke was at 151-200°C, the temperature sensor detected and transmitted a temperature signal to the controller. Thus, the controller enabled the solenoid valve of the second-position first outlet tube 16 to open, allowing the smoke to enter a second absorption container for absorption.
The absorption containers held 60 mL of 0°C dichloromethane for capturing the smoke at different temperatures for GC-MS. Through the GC-MS, peak areas and relative contents of nicotine, organic acids, ketones, alcohols, esters, hydrocarbons, and phenols at different temperatures were derived, as shown in Table 1.
Table 1 Peak areas and relative contents of various substances at different temperatures
Temperature | Substance Relative
Substances Peak Area (°C) Type Content (%) 200 1 472693840 28.745 1 1827654152 64.770
Nicotine 446022126 51.683 200 6 100004332 6.081 250 7 95915756 3.399
Organic acids 300 2 15110724 1.751 350 2 85418968 1.454 400 2 5417150 1.943
Cw ee
Ketones 300 4 13228670 3 14099236 0.500
Alcohols 2 3803097 0.441 2 245869835 41.965
Cw 0
Esters 300 2 3434187 0.398
(°C) Type Content (%)
Ee
Hydrocarbons sa
Example 2 0.1 g of a Hongda C3F flue-cured tobacco sample was spread flat in the 60 mm x 30 mm quartz boat, and the quartz boat with the tobacco sample was placed at a center of the furnace tube. After device connection was completed, a heating program (refer to
Example 1) was set. The temperature was raised at 25°C/min to 250°C, and held for 10 min. Air was introduced into the device at 20 mL/min and blew for 75 min. In the condition of freezing saturated salt water bath, the smoke was absorbed through the absorption container holding 150 mL of 0°C dichloromethane. After the absorption,
GC/MS was carried out, and the results are shown in Table 2.
Table 2 Composition analysis of smoke absorption solution
S Retention Time Relative Content
0.
cyclopentadiene eT Eee | 0 en x x :
one methylphenyl)ethenone 5 1,1,5-Trimethyl-1,2- dihydronaphthalene : 5 @ wes | wees | er
Octadecanoic acid
Example 3 0.1 g of a Hongda C3F flue-cured tobacco sample was spread flat in the 60 mm x 30 mm quartz boat, and the quartz boat with the tobacco sample was placed at a center of the furnace tube. After device connection was completed, a heating program was set.
The temperature was raised at 30°C/min to 250°C, and held for 10 min. Air was introduced into the device at 50 mL/min and blew for 75 min. In the condition of freezing saturated salt water bath, the smoke was absorbed through the absorption container holding 150 mL of 25°C dichloromethane. 200 uL of BSTFA was added into the absorption solution for derivatization in a water bath at 60°C for 50 min. Then GC/MS was carried out, and the results are shown in Table 3.
Table 3 Composition analysis of smoke absorption solution after silanization derivatization
S Retention Time Relative Content 3
K
B) 3% 1-Hexanol, TMS derivative isopropylcyclohexyl ester 4.265 Benzfuran
Ei
Benzyl alcohol, tert-butyldimethylsilyl (TBDMS) derivative 1-Trimethylsilyloxy-n-octene 3-Aminophenol, TMS derivative 0.688
Ee a 3,5-Dimethylphenol, TMS derivative a 3-Ethylphenol, TMS derivative 3,5-Dimethylphenol, TMS derivative en
Phenylacetic acid, TMS derivative 12.818 Azelaic acid, TMS derivative
Pimelic acid, TMS derivative
Oleic acid, TMS derivative 0.268 8-Methylheptane
According to Table 2 and Table 3, the relative content of nicotine in the smoke absorption solution without derivatization was 32.984%, while the relative content of nicotine in the absorption solution after silanization derivatization was 19.819%. This 5 shows that the silanization treatment reduced the high-content nicotine component, facilitating the detection of other volatile components.
Example 4 0.1 g of a Hongda C3F flue-cured tobacco sample was spread flat in the 60 mm x 30 mm quartz boat, and the quartz boat with the tobacco sample was placed at a center of the furnace tube. After device connection was completed, a heating program was set.
The temperature was raised at 15°C/min to 250°C, and held for 10 min. Air was introduced into the device at 10 mL/min and blew for 75 min. In the condition of freezing saturated salt water bath, the smoke was absorbed through the absorption container holding 60 mL of 0°C dichloromethane. After the absorption, the smoke absorption solution was divided into two parts. One part of the smoke absorption solution was directly subjected to GC/MS. For the other part of the smoke absorption solution, 200 uL of BSTFA was added for derivatization in a water bath at 60°C for 50 min, and then
GC/MS was carried out. The contents of the substances before and after derivation were compared, and the results are shown in Table 4.
Table 4 Contents of various substances before and after derivatization
Before Derivatization
Substances Substance Total Relative Substance Total Relative
Nicotine 1 19.819
Alcohols 1 3.416
Example 5 0.1 g of a Hongda C3F flue-cured tobacco sample was spread flat in the 60 mm x 30 mm quartz boat, and the quartz boat with the tobacco sample was placed at a center of the furnace tube. After device connection was completed, a heating program was set.
The temperature was raised at 15°C/min to 250°C, and held for 10 min. Air was introduced into the device at 10 mL/min and blew for 75 min. In the condition of freezing saturated salt water bath, the smoke was absorbed through 30 mL, 40 mL, 50 mL, 60 mL, 70 mL, and 80 mL of 0°C dichloromethane. 200 uL of BSTFA was added into the absorption solution for derivatization in a water bath at 60°C for 50 min. Then GC/MS was carried out, and the results in the case of using 50 mL of dichloromethane as the absorbent are shown in Table 5.
Table 5 Composition analysis using 50 mL of dichloromethane as the absorbent
Retention
SN Compounds Relative Content (%) ay | me cn
2-Furoic acid hydrazide 0.570 3.908 a-Benzylphenylethylamine 0.660
L-(+)-Lactic acid, 2TMS 4 5.077 oo 0.831 derivative
Alloocimene 1.318 6 5.215 N-butyl benzene 0.907 5.323 Propionic acid, TMS derivative 8 5.577 Hexachloroethane 1.117 0 5.678 1,4-Diethylbenzene 0.396 2-Bromo-1-methyl-1- 5.784 1.056 phenylcyclopropane 6.171 Vinyl trans-cinnamate 6.821 3-Pyridine, TMS derivative 0.871 7.12 M-cresol, TMS derivative 0.901 2-Methoxythiophenol, TMS 14 8.68 oo 1.839 derivative 3-Methyl-2-furoic acid, TMS 9.076 oo 1.796 derivative 3,5-Dimethylphenol, TMS 16 9.28 1.597 derivative 2,5-Dimethylphenol, TMS 17 9.594 — 0.699 derivative 2-(1,1-Dimethylethyl)-6-(1- 18 10.185 ( lethyl)-6+ 1.117 methylethyl)phenol
Methylsulfonic acid, TBDMS 19 11.728 oo 2.752 derivative
M-toluenic acid, TMS 21 13 oo 0.494 derivative 13.229 Glycolic acid, 2TMS derivative 0.834 2-Furanacrylic acid, TMS 23 13.436 —_ 0.797 derivative
3-Methylcatechol, 2TMS 24 13.987 oo 2.250 derivative 15.147 1,3-Dimethylnaphthalene 1.013
Trans-2-phenylcyclopropyl 27 17.154 P YIeyeIopTopy 1.805 isocyanate 17.494 M-toluic acid, TMS derivative 18.981 Isovanillin, TMS derivative 1.616 5-Hydroxymethyl-2-furoic 31 19.655 VOS 0.583 acid, 2TMS derivative 20.188 Phthalimide, TMS derivative 7-Butyl-tricyclo- 33 20.494 y 1.003 [4.2.0(2,5)]dec-7-ene
Vanillin methyl ester, TMS 23.169 a 0.505 derivative 23.723 O-isopropylphenol 1.193 2,6-Dihydroxyacetophenone, 37 24.083 a. 0.643 2TMS derivative 26.198 1-Dodecanol 1.647 27.439 Vanilla acid, 2TMS derivative 0.593 28.633 Alizarin, 2TMS derivative 0.223 30.559 Myristic acid, TMS derivative 1.845 (2E,6E,10E)-3,7,11,15- 42 32.44 tetramethylhexadecane- 1.302 2,6,10,14-tetraene-1-yl formate 13-Methyltetradec-9-enoic 44 33.335 | Co 2.228 acid, TMS derivative
Pentadecylic acid, TMS 33.93 a 1.148 derivative
34.75 Cembrene 1.319 36.426 Palmitic acid, TMS derivative 0.447 36.665 Scopolamine, TMS derivative 2.100 1,5-Divinyl-2,3-dimethyl- 49 37.964 0.730 ‚(10,20,30,5B)-cyclohexane (3aR,4R,8R,8aS)-3a,4,8a- trimethyl-7-methylene 38.85 1.943 decahydro-4,8- methylazacyclohexene- 2-Methyl-3-(3-methyl-butan-2- 51 39.4 eny)-2-(4-methyl-penten-3- 0.471 eny)-oxocyclobutane
Heptadecanoic acid, TMS 52 39.442 oo 1.573 derivative 41.199 Phytol, TMS derivative 0.581 9,12-Octadecadienoic acid 54 42.347 oo 10.046 (Z,Z)-, TMS derivative
Oleic acid, (Z)-, TMS 42.798 oo 1.329 derivative a-Linolenic acid, TMS 56 42.896 oo 0.666 derivative 10-Azelaic acid, (Z)-, TMS 57 44.579 oo 0.747 derivative 2-Methyl-3-(3-methyl-butan-2- 58 45.344 eny)-2-(4-methyl-penten-3- 0.111 eny)-oxocyclobutane 45.467 Azelaic acid, TMS derivative 0.228 (2E,6E)-3,7-11- 46.789 trimethyldodecane-2,6-10- 0.968 trienyl propionate
(2E,6E)-3,7,11- 61 47.069 trimethyldodeca-2,6-10-trien-1- 2.349 yl stearate isophthalic acid sulfate derivative 51204 Diethylheptadecyloxy(2- methylbutoxy)-silane 68 51.889 1,14-Tetradecanediol
Example 6 12 g of a Hongda C3F flue-cured tobacco sample was spread flat in the 60 mm * 30 mm quartz boat, and the quartz boat with the tobacco sample was placed at a center of the furnace tube. After device connection was completed, a heating program was set.
The temperature was raised at 30°C/min to 400°C, and held for 10 min. Nitrogen was introduced into the device at 50 mL/min and blew for 75 min (before heating, the nitrogen was introduced at 50 mL/min from a gas inlet for 20 min to exhaust air in the device). In the condition of freezing saturated salt water bath, the smoke was absorbed through 150 mL of 25°C dichloromethane. Then the absorption solution was subjected to GC/MS.
Example 7 6 g of a Hongda C3F flue-cured tobacco sample was spread flat in the 60 mm x 30 mm quartz boat, and the quartz boat with the tobacco sample was placed at a center of the furnace tube. After device connection was completed, a heating program was set.
The temperature was raised at 30°C/min to 1,200°C, and held for 10 min. Nitrogen was introduced into the device at 100 mL/min and blew for 75 min (before heating, the nitrogen was introduced at 100 mL/min from a gas inlet for 20 min to exhaust air in the device). In the condition of freezing saturated salt water bath, the smoke was absorbed through 150 mL of 25°C dichloromethane. Then the absorption solution was subjected to GC/MS.
The present disclosure is described above according to several explanatory examples of the present disclosure. However, it should be understood that those skilled in the art may design various modifications and implementations, and these modifications and implementations should fall within the protection scope and spirit of the present disclosure. More specifically, various modifications and improvements can be made to the components and/or layouts of the theme combination layout within the scope defined by the drawings and claims of the present disclosure. In addition to the modification and improvement of the components and/or layout, other uses will also be apparent to those skilled in the art.

Claims (9)

ConclusiesConclusions 1. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak, die de volgende stappen omvat: het blazen van rook, die gegenereerd is door het verwarmen van een tabaksmonster door een gradiéntrookafgifte-inrichting, in een absorptiehouder die een absorbens vasthoudt om een absorptie-oplossing te genereren, en het onderwerpen van de absorptie-oplossing aan gaschromatografie-massaspectrometrie (GC-MS).A method of monitoring a release pattern of a volatile substance in tobacco, comprising the steps of: blowing smoke generated by heating a tobacco sample through a gradient smoke dispenser into an absorber holding an absorbent to generating an absorption solution, and subjecting the absorption solution to gas chromatography-mass spectrometry (GC-MS). 2. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 1, die verder het volgende omvat: het behandelen, als een doelanalyt geen nicotine is, van de absorptie-oplossing met een moleculair ingeprente vastefase-extractiekolom of door derivatisering om een nicotinecomponent met een hoog gehalte te verminderen; en het filtreren, door een microporeus filtermembraan van 0,22 um, van de absorptie-oplossing na behandeling van nicotinevermindering voor GC-MS.A method for monitoring a release pattern of a volatile in tobacco according to claim 1, further comprising: treating, when a target analyte is other than nicotine, the absorption solution with a molecularly imprinted solid phase extraction column or by derivatization to reduce a high nicotine component; and filtering, through a 0.22 µm microporous filter membrane, the absorption solution after nicotine reduction treatment for GC-MS. 3. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 1, waarbij de gradiëntrookafgifte-inrichting een kwartsbuis (6) omvat; de kwartsbuis (6) daarin voorzien is van een kwartsschuit (8); de kwartsschuit door een buisoven (7) verwarmd wordt; en de buisoven (7) verbonden is met een thermokoppel (9) en een temperatuurbesturing (10); één uiteinde van de kwartsbuis (6) voorzien is van een gasverbindingsstuk (5); het gasverbindingsstuk (5) voorzien is van een duwstang (4); het gasverbindingsstuk (5) via een driewegbuis met twee gasbuizen verbonden is; en de twee gasbuizen respectievelijk verbonden zijn met gastoevoerinrichtingen (1), en elk voorzien zijn van een drukreduceerventiel (2) en een rotameter (3); het andere uiteinde van de kwartsbuis (6) een uitlaateinde vormt dat verbonden is met meerdere eerste uitlaatbuizen (16) en voorzien is van een temperatuursensor; de eerste uitlaatbuizen (16) elk voorzien zijn van een magneetventiel (17); het thermokoppel (9), de temperatuurbesturing (10), de temperatuursensor en het magneetventiel (17) verbonden zijn met een externe besturing, en de besturing verbonden is met een visueel bedieningsscherm; en een staartuiteinde van elk van de eerste uitlaatbuizen (16) verbonden is met een eerste absorptiehouder (11); de eerste absorptiehouder (11) in een koeltank (12) geplaatst is; en de eerste absorptiehouder (11) voorzien is van een tweede uitlaatbuis.A method of monitoring a volatile substance release pattern in tobacco according to claim 1, wherein the gradient smoke delivery device comprises a quartz tube (6); the quartz tube (6) is provided therein with a quartz boat (8); the quartz barge is heated by a tube furnace (7); and the tube furnace (7) is connected to a thermocouple (9) and a temperature controller (10); one end of the quartz tube (6) is provided with a gas connecting piece (5); the gas connecting piece (5) is provided with a push rod (4); the gas connecting piece (5) is connected to two gas pipes via a three-way pipe; and the two gas pipes are respectively connected to gas supply devices (1), and are each provided with a pressure reducing valve (2) and a rotameter (3); the other end of the quartz tube (6) forms an outlet end connected to a plurality of first outlet tubes (16) and provided with a temperature sensor; the first exhaust pipes (16) are each provided with a solenoid valve (17); the thermocouple (9), the temperature control (10), the temperature sensor and the solenoid valve (17) are connected to an external control, and the control is connected to a visual control screen; and a tail end of each of the first exhaust tubes (16) is connected to a first absorption container (11); the first absorption container (11) is placed in a cooling tank (12); and the first absorption container (11) is provided with a second outlet tube. 4. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 3, waarbij de gastoevoerinrichtingen een luchttoevoerinrichting en een stikstoftoevoerinrichting omvatten.A method for monitoring a release pattern of a volatile substance in tobacco according to claim 3, wherein the gas supply devices comprise an air supply device and a nitrogen supply device. 5. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 1, waarbij het verwarmde tabaksmonster een massa van 0,1-12 g heeft.A method for monitoring a volatile substance release pattern in tobacco according to claim 1, wherein the heated tobacco sample has a mass of 0.1-12 g. 6. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 1, waarbij het blazen gasblazen is dat uitgevoerd wordt met 0,1- 100 mL/min.A method for monitoring a release pattern of a volatile substance in tobacco according to claim 1, wherein the blowing is gas blowing performed at 0.1-100 mL/min. 7. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 1, waarbij het tabaksmonster verwarmd wordt met 0,1- 30°C/min tot 15-1.200°C.A method for monitoring a volatile substance release pattern in tobacco according to claim 1, wherein the tobacco sample is heated at 0.1-30°C/min to 15-1,200°C. 8. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 1, waarbij de absorbens een volume van 0,1-150 mL heeft.A method for monitoring a release pattern of a volatile substance in tobacco according to claim 1, wherein the absorbent has a volume of 0.1-150 mL. 9. Werkwijze voor het volgen van een afgiftepatroon van een vluchtige stof in tabak volgens conclusie 1, waarbij de absorbens bij -10-25°C is.A method for monitoring a volatile substance release pattern in tobacco according to claim 1, wherein the absorbent is at -10-25°C.
NL2036104A 2023-05-19 2023-10-24 Method for tracking release pattern of volatile substance in tobacco NL2036104A (en)

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CN108375637A (en) * 2018-02-06 2018-08-07 陕西中烟工业有限责任公司 A kind of heating of large capacity is not burnt tobacco product simulated experiment analytical equipment and method
CN110568090A (en) * 2019-08-06 2019-12-13 河南中烟工业有限责任公司 Method for collecting and detecting acidic aroma components in cigarette mainstream smoke
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CN107422051A (en) * 2017-05-26 2017-12-01 上海烟草集团有限责任公司 A kind of method that gas phase composition is cracked under on-line checking tobacco additive agent or smoking material different temperatures
CN108375637A (en) * 2018-02-06 2018-08-07 陕西中烟工业有限责任公司 A kind of heating of large capacity is not burnt tobacco product simulated experiment analytical equipment and method
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