CN105510090B - The lower Volatile infochemicals capturing device of tobacco heating, detecting system and method - Google Patents

Abstract

The invention relates to a collection device, detection system and method for volatile aroma substances under heating of tobacco. The collection device includes: a pyrolysis reaction tube (12), a heating module and a gas collection module (5). Around the pyrolysis reaction tube (12), it is used to heat the tobacco sample (8) placed in the pyrolysis reaction tube (12) to carry out the pyrolysis reaction. One end of the pyrolysis reaction tube (12) is fed with reaction gas, and the other One end is connected with the gas capture module (5), and the gas capture module (5) is used to collect volatile aroma substances after pyrolysis reaction. The trapping device of the present invention can place more tobacco samples in the pyrolysis reaction tube, so as to trap a large amount of aroma substances in the heated non-combustion state of the tobacco samples, so as to facilitate the detection of various trace components in the aroma substances; the present invention The detection method adopts gas chromatography/mass spectrometry, which can make the qualitative detection of each component in the aroma substances have higher accuracy.

Description

Device, detection system and method for capturing volatile aroma substances under heating of tobacco

technical field

The invention relates to the technical field of chemical detection of tobacco aroma components, in particular to a device, detection system and method for collecting volatile aroma substances in a heated and non-combusted state of tobacco.

Background technique

In order to analyze the components of the volatile aroma substances produced by heating or burning tobacco, it is necessary to capture the aroma substances during the heating or burning process. At present, there are mainly two methods of capture commonly used, which will be introduced separately below.

One is the online capture method, that is, the air bag is directly connected to the smoking machine, the air bag is used to capture the mainstream smoke of cigarettes, and the smoke in the air bag is absorbed into the sample tube through a syringe pump, and put into a thermal desorption- The desorption detection and analysis by GC-MS has the advantage of good repeatability, but this method uses the gas phase components captured by the smoking machine in the combustion state, and is not suitable for the capture of volatile aroma substances in the heating and non-combustion state.

The other is the off-line capture method, which can be applied to the capture of volatile aroma substances in a heated non-combustion state. It uses a thermogravimetric analyzer or a pyrolysis instrument to heat up and crack the sample. After the tube is adsorbed, put it into the thermal desorption GC-MS for desorption detection and analysis. The advantage is good repeatability. However, the small sample size of this method makes the response value of the volatile substances obtained by cracking low, which makes the analysis difficult. . Moreover, this method does not pass through the Cambridge filter when capturing gas phase components, and particulate matter will be introduced, which will interfere with the analysis of volatile gas phase components, thereby affecting the analysis results.

Contents of the invention

The object of the present invention is to propose a device, detection system and method for capturing volatile aroma substances under heating of tobacco, which can capture a large amount of aroma substances in a heated non-combustion state of tobacco samples, so as to detect the trace amounts of aroma substances in the tobacco sample. ingredients.

In order to achieve the above purpose, the first aspect of the present invention provides a device for capturing volatile aroma substances under heating of tobacco, including: a pyrolysis reaction tube 12, a heating module and a gas capturing module 5, the heating module is arranged on the Around the pyrolysis reaction tube 12, it is used to heat the tobacco sample 8 placed in the pyrolysis reaction tube 12 to carry out the pyrolysis reaction. One end of the pyrolysis reaction tube 12 is fed with reaction gas, and the other end is connected with the The gas capture module 5 is connected to the gas capture module 5, and the gas capture module 5 is used to collect the volatile aroma substances after the pyrolysis reaction.

Further, it also includes a particulate matter collection module 6 arranged between the pyrolysis reaction tube 12 and the gas collection module 5 , and the particulate matter collection module 6 is provided with a Cambridge filter.

Further, it also includes a temperature control module 4 for controlling the heating module to control the reaction temperature and reaction time.

Further, a flow control module 2 is also included, which is used to control the flow rate of the reaction gas passing into the pyrolysis reaction tube 12 .

Further, the heating module includes: an infrared lamp 7, a thermocouple 9, an insulating layer 10, and an installation body 11 with a hollow portion, the installation body 11 is sleeved outside the pyrolysis reaction tube 12, and the There is an annular cavity between the inner wall of the installation body 11 and the outer wall of the pyrolysis reaction tube 12, the infrared lamp 7 is arranged in the installation body 11, and the thermocouple 9 is arranged in the pyrolysis reaction tube 12. On the outer wall of the pipe 12 , the insulation layer 10 is wrapped around the outside of the installation body 11 .

Further, a vacuum pump 13 is also included, and the vacuum pump 13 is arranged at an end of the gas capture module 5 away from the pyrolysis reaction tube 12 .

In order to achieve the above object, the second aspect of the present invention provides a detection system for volatile aroma substances under heating of tobacco, including: the trapping device described in the above embodiments, a thermal desorption instrument, a gas chromatograph and a mass spectrometer detector,

The thermal desorption instrument is used to analyze and process the volatile aroma substances;

The gas chromatograph is used for gas chromatographic separation of the volatile aroma substances after analytical treatment;

The mass spectrometer detector is used for qualitative analysis of the components of the volatile aroma substances.

Further, the gas trapping module 5 is also used for adding an internal standard substance, so as to conduct a semi-quantitative analysis on the relative content of each component in the volatile aroma substances by using the internal standard method.

In order to achieve the above purpose, the third aspect of the present invention provides a method for detecting volatile aroma substances under heating of tobacco, based on the detection system described in the above embodiments, including:

The volatile aroma substances after the pyrolysis reaction are collected by the gas capture module 5;

Using a thermal desorption instrument to analyze and process the volatile aroma substances;

Using a gas chromatograph to carry out gas chromatographic separation of the volatile aroma substances after the analytical treatment;

A mass spectrometer is used to perform qualitative analysis on the components of the volatile aroma substances.

Further, it also includes: using internal standard method to conduct semi-quantitative analysis on the relative content of each component in the volatile aroma substances.

Further, the qualitative analysis is to search the NIST library of the target peak on the full scan spectrum, and assist the retention time in qualitative analysis.

Further, the working conditions of the pyrolysis reaction tube 12 are:

The furnace temperature is 150°C-250°C; the reaction atmosphere is 0%-50%; the heating time is 5min-50min.

Further, the operating temperature condition of the thermal desorber is:

The analysis temperature of the sample tube is 150°C-250°C; the valve temperature is 150°C-250°C; the transfer line temperature is 150°C-250°C, the high temperature of the trap is 150°C-250°C, and the low temperature of the trap is -20-1°C.

Further, the working time and flow conditions of the thermal desorption instrument are: thermal desorption dry blowing time 1min, desorption time 4-16min; chromatographic column flow rate 1-3mL/min; desorption flow rate: 10-40mL/min ; Outlet shunt 40 ~ 70mL/min; inlet shunt 40 ~ 70mL/min.

Further, the working conditions of the mass spectrometer are:

The temperature of the transmission line is 280°C, the temperature of the ion source is 230°C, the tuning voltage is 370V, the solvent delay is: 0-4.8min; the detection mode is full scan mode MS-scan.

Further, the condition of gas chromatography separation is:

Use HP-5MS capillary column 60m×0.25mm×0.25um; column oven temperature rise program: keep at 50°C for 2 minutes, raise the temperature to 150°C at 1.5°C/min and hold for 0 min, then raise the temperature to 280°C at 100°C/min and hold for 1 minute ; Carrier gas: helium.

Further, the volatile aroma substances include: 2,3-pentanedione, furfural, furfuryl alcohol, 2-acetylfuran, benzaldehyde, 5-methyl-2-furfuraldehyde, 6-methyl-5-heptan En-2-one, 3-methylcyclopentane-1,2-dione, phenylacetaldehyde, 2-acetylpyrrole, phenylethyl alcohol, solanone, pyrrole, 2-methylpyrazine, methylcyclopentyl Enolone, 2-acetyl-5-methylfuran, acetophenone, 2-acetyl-5-methylfuran, acetophenone, ethylcyclopentenolone, 2-methoxy-4- Methylphenol, Geranylacetone.

Based on the above technical scheme, the volatile aroma substance trapping device under tobacco heating of the present invention can put a relatively large amount of tobacco samples in the pyrolysis reaction tube, one end of the pyrolysis reaction tube is passed into the reaction gas, and the other end is connected with the gas trapping It is connected to the set module and heated by the heating module to carry out the pyrolysis reaction, so that the gas capture module captures a large amount of aroma substances in the heating and non-combustion state of the tobacco sample, so as to detect the trace components in the aroma substances more accurately .

Description of drawings

The accompanying drawings described here are used to provide a further understanding of the present invention and constitute a part of the application. The schematic embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute improper limitations to the present invention. In the attached picture:

Fig. 1 is a structural schematic diagram of an embodiment of the volatile aroma substance trapping device under tobacco heating of the present invention;

Fig. 2 is a schematic flow chart of an embodiment of the method for detecting volatile aroma substances under heating of tobacco according to the present invention;

Fig. 3 is the TIC spectrogram of single-grade shredded tobacco A in the heating and non-combustion state;

Fig. 4 is the TIC spectrogram of single-grade shredded tobacco B in a heated non-combustion state;

Fig. 5 is the TIC spectrogram of the single-grade cut tobacco C in the heating and non-combustion state.

Explanation of reference signs

1-gas source; 2-flow control module; 3-controller; 4-temperature control module; 5-gas capture module; 6-particle capture module; 7-infrared lamp; 8-tobacco sample; 9 - thermocouple; 10 - insulation layer; 11 - installation body; 12 - pyrolysis reaction tube; 13 - vacuum pump.

Detailed ways

The present invention will be described in detail below. In the following paragraphs, different aspects of the embodiments are defined in more detail. Aspects so defined may be combined with any other aspect or aspects unless specifically stated otherwise. In particular, any feature considered to be preferred or advantageous may be combined with one or more other features which are considered to be preferred or advantageous.

In order to solve the problem of capturing the volatile aroma substances in the heating and non-combustion state of tobacco in the prior art, the sample load of the pyrolysis instrument and the thermogravimetric method is small, resulting in the low quality of the obtained volatile aroma substances, and it is impossible to detect the trace components. Problem, the present invention provides a device for trapping volatile aroma substances under tobacco heating.

As shown in Figure 1, the volatile aroma substance trapping device under tobacco heating of the present invention comprises: a pyrolysis reaction tube 12, a heating module and a gas trapping module 5, and the heating module is arranged around the pyrolysis reaction tube 12 for The tobacco sample 8 placed in the pyrolysis reaction tube 12 is heated to carry out the pyrolysis reaction. The two ends of the pyrolysis reaction tube 12 are closed with end caps, and one end is connected to the gas source 1 through a trachea to feed in the reaction gas, for example, A certain volume of nitrogen and oxygen mixed gas is used to control the reaction atmosphere, and the other end is connected to the gas capture module 5 through a gas pipe, and the gas capture module 5 is used to collect volatile aroma substances after the pyrolysis reaction. Wherein, the pyrolysis reaction tube 12 can be selected as a slender quartz glass tube, and is horizontally installed in the heating chamber, and a relatively large amount of tobacco samples 8 can be accommodated inside it, which overcomes the thermal cracking instrument and the thermogravimetric method in the prior art. Place the problem of small sample volume. The gas capture module 5 can be a gas adsorption tube equipped with tenax adsorbent, and the two ends of the adsorption tube can be sealed.

The volatile aroma substance trapping device under tobacco heating according to the embodiment of the present invention is suitable for trapping volatile aroma substances in the non-combustion state of tobacco heating, and the pyrolysis reaction tube is used as the tobacco pyrolysis reactor, which can accommodate a relatively large amount of tobacco For the sample, one end of the pyrolysis reaction tube is fed with the reaction gas, and the other end is connected to the gas capture module, and is heated by the heating module to carry out the pyrolysis reaction, so that the gas capture module captures relatively A large amount of aroma substances, in order to more accurately detect the trace components in the aroma substances.

In an improved embodiment of the present invention, the trapping device also includes a particulate matter trapping module 6 arranged between the pyrolysis reaction tube 12 and the gas trapping module 5, and the particulate matter trapping module 6 is provided with a Cambridge The filter can filter out the particulate matter produced by the pyrolysis reaction of the tobacco sample 8, and try to avoid the interference of the particulate matter on the analysis of the volatile gas phase components.

In order to be able to flexibly control the pyrolysis temperature of the tobacco sample 8 in the pyrolysis reaction tube 12, the trapping device of the present invention also includes a temperature control module 4, which is used to control the heating module to control the reaction temperature and reaction time, so that the tobacco sample 8 is kept at The pyrolysis reaction occurs under suitable temperature regulation. In the actual operation process, the tobacco sample 8 can be first loaded into the decomposition reaction tube 12, and then when the reaction gas is introduced, the temperature control module 4 controls the heating module to heat rapidly and maintain a certain reaction time, so as to Tobacco sample 8 was fully subjected to pyrolysis reaction.

The progress of the pyrolysis reaction will not only be affected by the temperature parameter, but also be affected by the velocity of the reaction gas. For this reason, the trapping device of the present invention also includes a flow control module 2 , which is arranged in the gas pipe communicating with one end of the pyrolysis reaction tube 12 and used to control the flow rate of the reaction gas passing into the pyrolysis reaction tube 12 . For example: the flow control module 2 can choose components such as high-precision mass flow meters.

For each of the above-mentioned embodiments, a specific implementation form of the heating module 4 is given here. Specifically, the heating module 4 includes: an infrared lamp 7, a thermocouple 9, an insulating layer 10, and a mounting body 11 having a hollow portion. There is an annular cavity between the outer walls of the pyrolysis reaction tube 12, and the two ends of the mounting body 11 are closed by end caps. The annular cavity in the installation body 11 forms a heating cavity, and the heating cavity is a slender cavity, which can wrap the outer circumference of the pyrolysis reaction tube 12 on most of the length of the pyrolysis reaction tube 12, so as to put it into a larger At 8 o'clock, the tobacco samples with a large number of samples undergo rapid pyrolysis reaction, so as to capture a large amount of volatile aroma substances in a short period of time.

Wherein, the infrared lamp tube 7 is arranged in the mounting body 11. Preferably, the infrared lamp tube 7 is in a slender shape, and is arranged along the circumferential direction of the mounting body 11 in a manner parallel to its axis. Of course, a circular or spiral shape can also be selected. Infrared lamps. In addition, the thermocouple 9 is arranged on the outer wall of the pyrolysis reaction tube 12 , preferably at the bottom of the pyrolysis reaction tube 12 , and can quickly heat the tobacco sample 8 when the pyrolysis reaction tube 12 is placed horizontally. Furthermore, the heat insulation layer 10 is wrapped outside the installation body 11 , and during the heating process, the heat insulation layer 10 can prevent the heat from dissipating to the outside as much as possible, so as to achieve rapid temperature rise.

In another embodiment of the present invention, the trapping device also includes a vacuum pump 13, and the vacuum pump 13 is arranged at one end of the gas trapping module 5 away from the pyrolysis reaction tube 12, so that the volatile aroma substances can be adsorbed on as much as possible in a thermal desorption tube. Further, in order to be able to control the suction speed of the vacuum pump 13, a pump with an adjustable flow rate can be selected, or a flow control module 2, such as a high-precision mass flow meter, etc., can also be arranged between the gas capture module 5 and the vacuum pump 13 element.

In the embodiment given above, between the gas source 1 and one end of the pyrolysis reaction tube 12, between the other end of the pyrolysis reaction tube 12 and the particulate matter collection module 6, between the particle phase matter collection module 6 and the gas The trapping modules 5 and between the gas trapping modules 5 and the vacuum pump 13 are all connected by air pipes, such as PVC pipes, and it is also necessary to ensure the tightness of the connections between each section of air pipes and corresponding components.

Moreover, in order to control the flow control module 2 and the temperature control module 4, a controller can also be provided. Considering the convenience of operation, the controller can have a man-machine interface, such as a computer, to easily input the components of the heating module. Parameters such as heating temperature, heating time, composition ratio of reaction gas, and feeding speed of reaction gas can be set before capturing volatile aroma substances.

The usage method and working principle of the trapping device of the present invention will be described below with reference to the embodiment shown in FIG. 1 . Weigh 0.05g-0.5g of shredded tobacco sample into the pyrolysis reaction tube 12 at the position directly above the thermocouple 9, input various parameters in the computer according to requirements, and then pass a certain proportion of The reaction gas is heated to a preset temperature and kept for a certain reaction time. The particle phase capture module 6 with a Cambridge filter is used to filter the gas generated by the reaction, and then the gas phase components are captured by the thermal desorption sample tube. At the same time, the vacuum pump 13 sucks the gas in the device, so that the volatile aroma substances can be completely adsorbed in the thermal desorption sample tube, and the thermal desorption sample tube can be sealed after receiving the gas phase components for subsequent detection ingredients used.

Secondly, the present invention also provides a detection system for volatile aroma substances under heating of tobacco. Attached instrument, used for analysis and treatment of volatile aroma substances; gas chromatograph, used for gas chromatography separation of volatile aroma substances after analysis and treatment; mass spectrometer detector, used for qualitative analysis of the components of volatile aroma substances .

The detection system of this embodiment uses a gas chromatographic separation device and a mass spectrometer to perform qualitative detection of volatile aroma substances at the same time, and can more accurately determine the types of components contained therein.

In a more preferred embodiment, the detection system can also be used for semi-quantitative analysis of the relative content of each component in the volatile aroma substances. Specifically, an internal standard substance can be added to the thermal desorption sample tube, and the internal standard semi-quantitative analysis.

It can be seen that the volatile aroma substance detection system under tobacco heating of the present invention has the functions of pyrolysis reaction, thermal desorption, gas chromatography/mass spectrometry for qualitative detection and internal standard method for semi-quantitative detection of tobacco samples , the specific operation method and experimental conditions will be described in detail in the following detection method. This kind of detection system has the advantages of simple operation, accuracy, quickness and good selectivity, and has strong practical value.

Next, after the volatile aroma substances in the tobacco sample 8 are captured, each component therein can be detected. To this end, the present invention also provides a method for detecting volatile aroma substances under tobacco heating. In one embodiment, as shown in Figure 2, the method includes the following steps:

Step 101, collect the volatile aroma substances after the pyrolysis reaction through the gas collection module 5 . This step can be realized by the trapping devices of the foregoing embodiments of the present invention, and a larger amount of volatile aroma substances can be obtained by placing more tobacco samples 8, so as to provide a basis for subsequent more accurate analysis. The trapping method The difference will directly affect the sensitivity and repeatability of the test results.

Step 102, using a thermal desorption instrument to analyze and process the volatile aroma substances, and step 102 is performed after step 101. Using thermal desorption instrument to pre-treat volatile aroma substances, the method is simple and fast, which can avoid the loss of components caused by complex pre-treatment as far as possible, and also greatly reduce the pollution of the entire gas flow system.

Step 103, using a gas chromatograph to perform gas chromatographic separation on the analyzed gas. Gas chromatographic separation is a physical separation method that uses the small difference in the distribution coefficient (solubility) of each component of the measured substance between different two phases. When the two phases move relative to each other, these substances are repeatedly distributed between the two phases. , so that only a small difference in properties produces a great effect, and the different components are separated.

Step 104, using a mass spectrometer to perform qualitative analysis on the components of the volatile aroma substances. Step 104 can be performed after step 103. Mass spectrometry uses high-speed electrons to impact gaseous molecules or atoms, accelerates the ionized positive ions into a mass spectrometer detector, and then collects and records them in the order of mass-to-charge ratio (m/z) to obtain a mass spectrum. A mass spectrum is the mass spectrum of charged particles. Using a mass spectrometer for detection can avoid misjudgment caused by possible false positives in complex system compounds.

Specifically, the qualitative analysis in step 102 and step 103 is to search the NIST library of the target peak on the full scan spectrum, and assist the retention time in qualitative analysis. The full scan spectrum is determined by a mass spectrometer detector; qualitative results can be obtained by searching the NIST library of the target peak on the full scan spectrum; when searching by qualitative software, it is based on the characteristic ion of the chromatographic peak at a certain retention time. The search of the qualitative results of the NIST library, so it is necessary to assist the retention time for qualitative. The accuracy of qualitative methods is generally measured by the degree of matching, the higher the degree of matching, the better the accuracy.

The detection method of the embodiment of the present invention uses thermal desorption- gas chromatography/mass spectrometry (ATD-GC/MS) to analyze the components in the volatile aroma substances. The method is simple, accurate, fast and has good selectivity. , has high practical value, provides a research platform for the formation mechanism of main smoke components in the process of tobacco pyrolysis, and has practical guiding significance for the development of new tobacco products. Among them, good selectivity is an index related to accuracy, which means that the target peak and impurity peak appearing in the same retention time can be qualitatively and distinguished by mass spectrometry software, and the target peak can be better selected and judged.

Moreover, it can avoid misjudgment caused by possible false positives of complex system compounds as much as possible, so that the qualitative detection of each component in the volatile aroma substances has a higher accuracy.

After qualitatively analyzing the specific components of the volatile aroma substances in the previous embodiment, in order to carry out semi-quantitative analysis on the content of each specific component, in another embodiment of the present invention, the detection method can further include the following: step:

Step 105, using the internal standard method to conduct semi-quantitative analysis on the relative content of each component in the volatile aroma substances. The specific process is as follows: Since the two ends of the thermal desorption sample tube are sealed with a cap with a sealing ring inside, it is necessary to take out the cap first, add an internal standard into it, and then put the cap on to seal after adding. Preferably, phenylethyl acetate is selected as the internal standard, and its concentration is known. Assuming that the mass spectrometer has the same response value to the target compound and the internal standard at the same concentration, according to the following formula, the internal standard and the target The corresponding value to calculate the concentration of the target substance:

Wherein, the A _{target substance} and the A _{internal standard substance} are respectively the peak areas of the internal standard substance and the target substance in the chromatogram;

C _{target substance} and C _{internal standard substance} are the concentration values of internal standard substance and target substance respectively.

The relative content of each aroma component can be calculated by using the internal standard method for detection, which is simple and quick, and can also reduce the impact of chromatographic condition changes on the quantitative results, so as to improve the accuracy and precision of the detection method of the present invention; The effect of changing conditions on quantitative results to further improve accuracy and precision.

During the process of capturing and detecting volatile aroma substances, it is necessary to set the working conditions of the pyrolysis reaction tube 12, thermal desorption instrument, gas chromatographic separation and mass spectrometer detector. The range of conditions that can be selected for each component will be given below according to the experimental results, and the preferred values will be given.

In a specific embodiment, in the method of the present invention, the reactor conditions of the pyrolysis reaction tube 12 are: furnace temperature 150°C to 250°C (for example, 150°C, 180°C or 210°C); the reaction atmosphere is 0 %-50% (eg 0%, 5% or 50%); the heating time is 5min-50min (eg 5min, 10min, or 15min).

In a specific embodiment, in the method of the present invention, the working temperature conditions of the thermal desorber are: sample tube analysis temperature 150°C-250°C (for example 150°C, 180°C or 210°C); valve temperature 150°C ℃～250℃ (such as 150℃, 180℃ or 200℃); transfer line temperature 150℃～250℃ (such as 150℃, 180℃ or 210℃), trap high temperature 150℃～250℃ (such as 150℃, 180℃ °C or 210 °C), trap low temperature -20 ~ 1 °C (eg -10 °C, 0 °C or -20 °C).

In a specific embodiment, in the method of the present invention, the working time and flow conditions of the thermal desorption instrument are: thermal desorption dry blowing time 1min, desorption time 4～16min (such as 4min, 8min or 12min) ;Column flow rate: 1～3mL/min (for example, 21mL/min); desorption flow rate: 10～40mL/min (for example, 20mL/min); outlet split flow: 40～70mL/min (for example, 45mL/min); inlet split flow: 40～ 70mL/min (eg 45mL/min).

In a specific embodiment, in the method of the present invention, the gas chromatographic separation conditions are: adopt HP-5MS capillary column (60m × 0.25mm × 0.25um); Raise the temperature at 1.5°C/min to 150°C and keep it for 0min, then raise the temperature at 100°C/min to 280°C and keep it for 1min; Mass spectrometry detection.

In a specific embodiment, in the method of the present invention, the working conditions of the mass spectrometer detector are: transmission line temperature 280°C, ion source temperature 230°C, tuning voltage 370V, solvent delay: 0-4.8min; detection mode It is full scan mode (MS-scan).

In a specific embodiment, in the method of the present invention, the measured components of the method are the volatile aroma substances of tobacco in a heated non-combustion state, including 2,3-pentanedione, furfural, furfuryl alcohol, 2 -Acetylfuran, benzaldehyde, 5-methyl-2-furfuraldehyde, 6-methyl-5-hepten-2-one, 3-methylcyclopentane-1,2-dione, phenylacetaldehyde , 2-acetylpyrrole, phenethyl alcohol, solanone, pyrrole, 2-methylpyrazine, methylcyclopentenolone, 2-acetyl-5-methylfuran, acetophenone, 2-acetyl- 5-methylfuran, acetophenone, ethyl cyclopentenolone, 2-methoxy-4-methylphenol, geranyl acetone and other characteristic aroma components of tobacco.

The solution of the present invention will be described in detail below in conjunction with the examples, but those skilled in the art will understand that the following examples are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Those who do not indicate the specific conditions in the examples are carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used were not indicated by the manufacturer, and they were all commercially available conventional products.

In the following three examples, the shredded tobacco, heating temperature, holding time, pyrolysis reaction temperature and air flow rate are all different, which only illustrate that different grades of shredded tobacco can detect the gaseous phase components in the flue gas under different test conditions. It is the scope of patent protection of the present application. These conditional parameters have nothing to do with tobacco grades, different grades of tobacco and conditional parameters can be interleaved. Moreover, the detection result can be expressed by TIC spectrum (total ion current diagram), which can be obtained by the following method: the components flowing out through chromatographic separation continuously enter the mass spectrometer, and the mass spectrometer scans continuously for data collection, and a piece of information is obtained by each scan. Mass spectrum, add up all ion intensities in a mass spectrum to get a total ion current intensity. Among them, the peak area of the TIC spectrum can be used for quantification, and the peak apex search can be used for qualitative; peaks generated at multiple time points represent different compounds.

Example 1:

The detection method of the present invention is used to perform qualitative and quantitative analysis and detection on the single-grade shredded tobacco A sample.

1. Sample pretreatment: Weigh 0.1g single-grade cut tobacco sample, place it in a heating device, and quickly raise the temperature to 180°C while passing air at a flow rate of 1.5L/min, keep it for 10min, and desorb the sample with heat Receive the gas phase components in the tube, add 2 μL of phenylethyl acetate internal standard solution with a concentration of 0.1226 mg/mL, seal it, and place it in a thermal desorption instrument for sample injection;

2. The conditions of the tobacco pyrolysis reactor are: furnace temperature 180°C, reaction gas 50% air, flow rate 1.5L/min; heating time 10min.

3. The conditions of the thermal desorption instrument are: sample tube analysis temperature 210°C; valve temperature 200°C; transfer line temperature 220°C, trap high temperature 220°C, trap low temperature -10°C; dry blowing time 1min, desorption time 15min ; Chromatographic column flow 1mL/min; desorption flow: 20mL/min; outlet split 49mL/min; inlet split 50mL/min.

4. After thermal desorption and sample injection, enter the gas chromatography for separation. The chromatographic separation conditions are: use HP-5MS capillary column (60m×0.25mm×0.25um); ℃/min to 150 ℃ for 0 min, then 100 ℃/min to 280 ℃ for 1 min; carrier gas: helium (purity 99.999%);

5. The diverted gas enters the mass spectrometry detection after being separated by gas chromatography. The mass spectrometry detection conditions are: transfer line temperature 280°C, ion source temperature 230°C, tuning voltage 370V, solvent delay: 0-4.8min; scanning mass range: 35 ~455, the detection mode is full scan mode (MS-scan).

6. Qualify the full scan spectrum.

The analysis and determination of the volatile aroma substances of the single-grade shredded tobacco A under the heating and non-combustion state, the qualitative and semi-quantitative results are shown in Table 1, and the TIC spectrum is shown in Figure 3.

Table 1 Qualitative and quantitative results of volatile aroma substances in single-grade shredded tobacco A under heating and non-combustion state

It can be seen from Table 1 above that 2,3-pentanedione, furfural, furfuryl alcohol, 2-acetylfuran, benzaldehyde, 5-methyl-2-furfuraldehyde, 6-methyl-5-hepten-2-one, 3-methylcyclopentane-1,2-dione, phenylacetaldehyde, 2-acetylpyrrole, phenylethyl alcohol, solanone and other tobacco characteristic aroma components, Its content is 0.08-41.07ppm; in addition, acetic acid, acrylic acid, pyridine, succinic dialdehyde and other irritating or unpleasant odors were detected, and the content was all in the range of 0.15-11.6ppm.

Example 2:

The detection method of the present invention is used to perform qualitative and quantitative analysis and detection on the single-grade shredded tobacco B sample.

1. Sample pretreatment: Weigh 0.1g single-grade cut tobacco sample, place it in a heating device, and quickly raise the temperature to 200°C while passing air at a flow rate of 1.5L/min, keep it for 5min, and desorb the sample with heat The tube receives the gas phase components, adds 2 μL of phenylethyl acetate internal standard solution with a concentration of 0.1226 mg/mL, seals it, and places it in a thermal desorber for sample injection.

2. The conditions of the tobacco pyrolysis reactor are as follows: the furnace temperature is 200° C., the reaction gas is 50% air, the flow rate is 1.2 L/min; the heating time is 5 minutes.

3. After thermal desorption sample injection, conduct thermal desorption-GC analysis, the results are shown in Figure 2:

The analysis and determination of the volatile aroma substances of the single-grade shredded tobacco B under the heating and non-combustion state, the qualitative and quantitative results are shown in Table 2, and the TIC spectrum is shown in Figure 4.

Table 2 Qualitative and quantitative results of volatile aroma substances in single-grade shredded tobacco B under heating and non-combustion state

It can be seen from Table 2 above that 2,3-pentanedione, pyrrole, 2-methylpyrazine, furfural, furfuryl alcohol, methylcyclopentenolone, 2- Acetylfuran, benzaldehyde, 5-methyl-2-furylcarbaldehyde, 2-acetyl-5-methylfuran, phenylacetaldehyde, acetophenone and other characteristic aroma components of tobacco, the content of which is 0.08-75.04ppm; In addition, irritating or unpleasant odors such as acetic acid, acrylic acid, pyridine, and succinic dialdehyde were detected, and the contents were all in the range of 0.36-2.31 ppm.

Example 3:

The detection method of the present invention is used to perform qualitative and quantitative analysis and detection on the finished shredded tobacco C sample.

1. Sample pretreatment: Weigh 0.05g of finished cut tobacco sample, place it in a heating device, and quickly raise the temperature to 250°C while passing air at a flow rate of 1.5L/min, keep it for 20min, and desorb the sample tube with thermal desorption. Receive the gas phase components, add 2 μL of phenylethyl acetate internal standard solution with a concentration of 0.1226 mg/mL, seal it, and place it in a thermal desorber for sample injection.

2. The conditions of the tobacco pyrolysis reactor are: the furnace temperature is 250°C, the reaction gas is 50% air, the flow rate is 1.0L/min; the heating time is 20min.

3. After thermal desorption sample injection, perform thermal desorption-GC analysis. The volatile aroma substances of the finished tobacco cut C were analyzed and measured under the heating and non-combustion state. The qualitative and quantitative results are shown in Table 3, and the TIC spectrum is shown in Figure 5.

Table 3 Qualitative and quantitative results of volatile aroma substances in finished cut tobacco C under heating and non-combustion state

It can be seen from the above table 3 that 2,3-pentanedione, pyrrole, furfural, furfuryl alcohol, benzaldehyde, 5-methyl-2-furfuraldehyde, and methylcyclopentadione were detected under the heating and non-combustion state of single-grade shredded tobacco C. Enolone, 2-acetyl-5-methylfuran, phenylacetaldehyde, acetophenone, phenylethyl alcohol, ethylcyclopentenolone, 2-methoxy-4-methylphenol, solanone, fragrance Leafy acetone and other characteristic aroma components of tobacco, the content is 0.21-30.78ppm; in addition, acetic acid, pyridine, 2-picoline, phenol and other irritating or unpleasant odors are detected, the content is 0.12-10.89 in the ppm range.

The device, detection system and method for capturing volatile aroma substances under heating of tobacco provided by the present invention have been described in detail above. It should be understood that the present invention is not limited to the form disclosed herein, should not be regarded as excluding other embodiments, but can be used in various other combinations, modifications and environments, and can be used within the scope of the inventive concept described herein, through the above-mentioned Modified by teaching or skill or knowledge in a related field. However, modifications and changes made by those skilled in the art do not depart from the spirit and scope of the present invention, and all are within the protection scope of the present invention.

Claims (15)

1. A device for trapping volatile aroma substances under tobacco heating, characterized in that it comprises: a pyrolysis reaction tube (12), a heating module, a gas trapping module (5) and a vacuum pump (13), and the heating module is set Around the pyrolysis reaction tube (12), it is used to heat the tobacco sample (8) placed in the pyrolysis reaction tube (12) to perform pyrolysis reaction, and the pyrolysis reaction tube (12) One end of one end is passed into the reaction gas, and the other end is connected with the gas capture module (5), the gas capture module (5) is used to collect the volatile aroma substances after the pyrolysis reaction, and the vacuum pump (13) is set At the end of the gas capture module (5) away from the pyrolysis reaction tube (12); The device for capturing volatile aroma substances under heating of tobacco also includes a particulate phase capture module (6) arranged between the pyrolysis reaction tube (12) and the gas capture module (5), the particulate phase A Cambridge filter disc is arranged in the object trapping module (6). 2 . The device for trapping volatile aroma substances under heating of tobacco according to claim 1 , further comprising a temperature control module ( 4 ) for controlling the heating module to control the reaction temperature and reaction time. 3 . 3. The device for trapping volatile aroma substances under heating of tobacco according to claim 1, further comprising a flow control module (2) for controlling the reaction gas passing into the pyrolysis reaction tube (12) flow rate. 4. The device for trapping volatile aroma substances under heating of tobacco according to claim 1, characterized in that, the heating module comprises: an infrared lamp (7), a thermocouple (9), an insulating layer (10) and a The mounting body (11) of the hollow part, the mounting body (11) is sleeved outside the pyrolysis reaction tube (12), and the inner wall of the mounting body (11) is in contact with the pyrolysis reaction tube (12) There is an annular cavity between the outer walls of ), the infrared lamp (7) is arranged in the installation body (11), and the thermocouple (9) is arranged on the outer wall of the pyrolysis reaction tube (12) , the thermal insulation layer (10) is wrapped outside the installation body (11). 5. A detection system for volatile aroma substances under heating of tobacco, characterized in that it comprises: the trapping device described in any one of claims 1 to 4, a thermal desorption instrument, a gas chromatograph and a mass spectrometry detector, The thermal desorption instrument is used to analyze and process the volatile aroma substances; The gas chromatograph is used for gas chromatographic separation of the volatile aroma substances after analytical treatment; The mass spectrometer detector is used for qualitative analysis of the components of the volatile aroma substances. 6. The system for detecting volatile aroma substances under heating of tobacco according to claim 5, characterized in that, the gas capture module (5) is also used to add internal standard substances, so as to use internal standard method to measure the volatile aroma substances. The relative content of each component in the aroma substances was analyzed semi-quantitatively. 7. A method for detecting volatile aroma substances under heating of tobacco, characterized in that, based on the detection system according to claim 5 or 6, comprising: collecting the volatile aroma substances after the pyrolysis reaction through the gas trapping module (5); Using a thermal desorption instrument to analyze and process the volatile aroma substances; Using a gas chromatograph to carry out gas chromatographic separation of the volatile aroma substances after the analytical treatment; A mass spectrometer is used to perform qualitative analysis on the components of the volatile aroma substances. 8 . The method for detecting volatile aroma substances under heating of tobacco according to claim 7 , further comprising: semi-quantitatively analyzing the relative content of each component in the volatile aroma substances by using an internal standard method. 9. The method for detecting volatile aroma substances under heating of tobacco according to claim 7, wherein the qualitative analysis is to search the NIST library of the target peak on the full scan spectrum, and assist the retention time for qualitative analysis. 10. The method for detecting volatile aroma substances under heating of tobacco according to claim 7, characterized in that, the working conditions of the pyrolysis reaction tube (12) are: The furnace temperature is 150°C-250°C; the reaction atmosphere is 0%-50%; the heating time is 5min-50min. 11. The method for detecting volatile aroma substances under heating of tobacco according to claim 7, wherein the working temperature condition of the thermal desorption instrument is: The analysis temperature of the sample tube is 150°C-250°C; the valve temperature is 150°C-250°C; the transfer line temperature is 150°C-250°C, the high temperature of the trap is 150°C-250°C, and the low temperature of the trap is -20-1°C. 12. The method for detecting volatile aroma substances under heating of tobacco according to claim 7, characterized in that, the working time and flow conditions of the thermal desorption instrument are: thermal desorption dry blowing time 1min, desorption time 4～ 16min; chromatographic column flow rate: 1-3mL/min; desorption flow rate: 10-40mL/min; outlet split flow: 40-70mL/min; inlet split flow: 40-70mL/min. 13. The method for detecting volatile aroma substances under heating of tobacco according to claim 7, wherein the working conditions of the mass spectrometer are: The transfer line temperature is 280°C, the ion source temperature is 230°C, the tuning voltage is 370V, the solvent delay is: 0-4.8min; the detection mode is full-scan mode (MS-scan). 14. The method for detecting volatile aroma substances under heating of tobacco according to claim 7, characterized in that the conditions for gas chromatographic separation are: HP-5MS capillary column is used; column oven temperature rise program: keep at 50°C for 2 minutes, raise the temperature at 1.5°C/min to 150°C and hold for 0 min, then raise the temperature at 100°C/min to 280°C and hold for 1 minute; carrier gas: helium. 15. The method for detecting volatile aroma substances under heating tobacco according to claim 7, wherein the volatile aroma substances include: 2,3-pentanedione, furfural, furfuryl alcohol, 2-acetylfuran, Benzaldehyde, 5-methyl-2-furfuraldehyde, 6-methyl-5-hepten-2-one, 3-methylcyclopentane-1,2-dione, phenylacetaldehyde, 2-acetyl Pyrrole, phenylethyl alcohol, solanone, pyrrole, 2-methylpyrazine, methylcyclopentenolone, 2-acetyl-5-methylfuran, 2-acetyl-5-methylfuran, acetophenone , Ethyl cyclopentenolone, 2-methoxy-4-methylphenol, geranyl acetone.