CN108645941A - The detection device and detection method of orange taste ingredient the amount of migration in a kind of filter stick - Google Patents

Abstract

The invention relates to a detection device and detection method for the migration of orange flavor components in a filter rod. The device includes several heating chambers. One end of the heating chamber is connected to an air inlet, and the other end is connected to an air outlet pipe. The air outlet pipe is arranged around a turntable, and the turntable includes The first air intake pipe, the first air intake pipe rotates with the turntable, one end of the first air intake pipe communicates with one of the air outlet pipes at a certain moment, the other end of the first air intake pipe communicates with one end of the second air intake pipe, the second air intake pipe is fixed, and the other One end is connected with the filter rod holder, the filter rod holder is connected with the smoke trap, and the smoke trap is connected with the smoking machine. The device of the invention avoids the background interference of complex smoke components, significantly improves the precision and accuracy of measurement results; has a simple structure, is convenient to operate, reduces the influence of complex smoke, and avoids complex sample purification and enrichment operations. The analysis method of the invention is simple, fast, accurate, high in sensitivity, low in detection limit, effective and feasible, easy to operate, accurate and sensitive, and has popularization and application value.

Description

A detection device and detection method for the migration of orange-flavored components in a filter stick

technical field

The invention relates to a detection device, in particular to a detection device for the migration of orange flavor components in a filter rod, and also to a detection method, which belongs to the technical field of physical and chemical inspection of tobacco auxiliary materials.

Background technique

The development and application of cigarette flavoring and additives is becoming one of the most critical technologies for maintaining the taste of cigarettes in the work of harm reduction and coke reduction. Filter flavoring is an important way of flavoring. Adding flavors and fragrances directly to cigarette filters has the following advantages: first, it can avoid the loss and pyrolysis of flavors during cigarette storage and smoking; second, it can avoid the loss of flavors during cigarette static burning; third, it can reduce tobacco and filter. Wait for the retention of spices to increase the transfer efficiency; 4. A variety of flavoring methods can be used.

At present, the commonly used special flavoring filter sticks include multi-component compound flavoring filter, pop-bead filter, flavoring sheet filter, flavoring thread filter, particle flavoring filter, molded paper flavoring filter, triacetin flavoring filter etc. Orange essential oil was originally used as a fungicide and sedative, and now it is widely used in food, daily chemicals, and medicine. Orange essential oil has entered the Food Flavor and Extract Manufacturers Association (FEMA) Food Flavor List. At the same time, it is also included in the food spices allowed by China's food additive use hygienic standards. At present, orange flavor is widely used in special flavoring filters such as multi-component compound flavoring filters, pop-bead filters, flavored slice filters, and granular flavoring filters.

At present, the test method for the migration of ingredients added to special flavoring filter sticks into cigarette smoke usually uses a smoking machine to suck cigarettes, and then capture the smoke components for analysis. Due to the very complex background generated when the cigarette is burned, it will seriously interfere with the determination of the migration components of the special flavoring filter rod, the determination of its components is very difficult, and the error of the analysis results is also very large. How to truly and accurately analyze and detect the safety components of special flavoring filter sticks has become the focus of tobacco analysis research.

Contents of the invention

In order to solve the problems of the technologies described above, the object of the present invention is to provide a detection device and a detection method for the migration of orange flavor components in a filter stick, and the specific scheme of the present invention is as follows:

A detection device for the migration of orange flavor components in a filter rod, comprising several heating chambers, one end of the heating chamber is connected to an air inlet, and the other end is connected to an air outlet pipe, the air outlet pipe is arranged around a turntable, and the turntable includes a first air inlet pipe, the first air inlet pipe The air pipe rotates with the turntable, one end of the first air inlet pipe communicates with one of the air outlet pipes at a certain moment, the other end of the first air inlet pipe communicates with one end of the second air inlet pipe, the second air inlet pipe is fixed, and the other end is connected with the filter rod holder , the filter rod holder is connected to the smoke trap, and the smoke trap is connected to the smoking machine.

Further, there are 10 heating chambers, each of which is equipped with a temperature regulating device, and the heating temperature range is 30-200°C.

The detection method of the migration amount of the orange flavor component in the filter stick related to the present invention uses the detection device of claim 1 or 2 to detect, comprising the following steps:

Step (1), determine the number of suction ports

Insert a temperature measuring probe into the starting part of the far lip end of the cigarette to be tested that contains the flavoring filter, smoke on a conventional smoking machine, and measure the starting position of the flavoring filter through the temperature measuring probe when each puff is smoked the temperature of the smoke and determine the number of puffs for the whole cigarette;

Step (2), set the temperature of the required heating chamber according to the number of suction ports

Set the air temperature in several heating chambers of the detection device according to the actual smoking temperature of the cigarette, and set the number of suction ports;

Step (3), suction

Connect the smoking machine, the smoke trap and the filter rod holder in sequence, remove the filter tip of the special filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions, The air sucked comes from heating chambers with different temperatures, which are switched in turn according to the number of suction ports. The temperature of the airflow through the filter tip of each suction is consistent with the actual airflow temperature of the cigarette smoking machine; the smoke trap is used for flue gas cleaning. decapture;

Step (4), component analysis;

After trapping, ultrasonic extraction was performed using a mixed solution of ethanol and acetonitrile, followed by GC-MS analysis.

Further, the trapping method of the smoke trap is Cambridge filter trap, cold trap trap, absorption liquid trap or simulated artificial saliva trap.

Further, in step (4), the chromatographic analysis conditions are as follows:

Chromatography: The chromatographic column is a capillary column DB-5, 30 m×0.25mm×0.25μm; the carrier gas is helium; the volume flow rate is 2.0mL/min, the injection volume is 5 µL; splitless; heating program: initial temperature 400°C , kept for 5 minutes, raised to 150°C at 5°C/min, kept for 5 minutes, and finally raised to 280°C at 10°C/min, held for 1 minute.

Further, in step (4), the mass spectrometry analysis conditions are as follows:

Mass spectrometry: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600 v; electron energy: 70 eV.

Further, in step (4), ultrasonic extraction is performed using a mixed solution of 50ml ethanol and 150ml acetonitrile.

Compared with the prior art, the present invention has the following beneficial effects:

(1) The device of the present invention uses purified air flow for elution, which eliminates the background interference of complex smoke components generated during the actual cigarette burning process, and significantly improves the precision and accuracy of the measurement results.

(2) The present invention is simple in structure and easy to operate. Several heating chambers are set around the turntable, and different temperatures can be set to achieve a very good suction temperature of the human oral cavity. In the case of oral suction temperature, the influence of complex smoke is reduced.

(3) Simple headspace or solvent extraction can be used for direct analysis, which makes the determination of orange flavor components very easy, and avoids the complicated sample purification and analysis of conventional special flavored filter rod components to the smoke migration analysis. enrichment operation.

(4), the analysis method of the present invention is simple, fast, accurate, high sensitivity, low detection limit, effective and feasible, easy to operate, accurate and sensitive, and the test period is shortened by 10-15 minutes compared with the existing detection method, which has the value of popularization and application .

Description of drawings

Fig. 1 is the structural representation of detection device of the present invention;

In Figure 1: I is the turntable; II is the filter rod holder; III is the smoke trap; IV is the smoking machine; V is the air inlet;

1-the first communication port, 1'-the first heating chamber; 2-the second communication port, 2'-the second heating chamber; 3-the third communication port, 3'-the third heating chamber; 4-the fourth communication 4'-the fourth heating chamber; 5-the fifth communication port, 5'-the fifth heating chamber; 6-the sixth communication port, 6'-the sixth heating chamber; 7-the seventh communication port, 7'- Seventh heating chamber; 8-eighth communication port, 8'-eighth heating chamber; 9-ninth communication port, 9'-ninth heating chamber; 10-tenth communication port, 10'-tenth heating chamber; 11-the first air intake pipe; 12-the second air intake pipe.

Detailed ways

The present invention will be described in further detail below in conjunction with the accompanying drawings and examples, but the present invention is not limited in any way, and any changes or improvements based on the teachings of the present invention fall within the protection scope of the present invention.

Example 1

The detection device of this embodiment includes a first heating chamber 1', a second heating chamber 2', a third heating chamber 3', a fourth heating chamber 4', a fifth heating chamber 5', a sixth heating chamber 6', The seventh heating chamber 7', the eighth heating chamber 8', the ninth heating chamber 9', and the tenth heating chamber 10', one end of each heating chamber is connected to the air inlet, and the other end is connected to the air outlet pipe, and the air outlet pipe surrounds the turntable 1 Set to form the first communication port 1, the second communication port 2, the third communication port 3, the fourth communication port 4, the fifth communication port 5, the sixth communication port 6, the seventh communication port 7, The eighth communication port 8, the ninth communication port 9, the tenth communication port 10, the first air intake pipe 11 is included on the turntable 1, and the first air intake pipe 11 rotates with the turntable 1, and one end of the first air intake pipe 11 connects with it at a certain moment. One communication port communicates, the other end of the first air inlet pipe 11 communicates with one end of the second air inlet pipe 12, the second air inlet pipe 12 is fixed, the other end of the second air inlet pipe 12 is connected with the filter rod holder II, and the filter rod holder II Connect the smoke trap III, the smoke trap III is connected to the smoking machine IV, an air intake pipe can be arranged at one end of the air inlet, and one end of the air intake pipe is connected with the air inlet V.

The heating chamber is equipped with a temperature regulating device, and the heating temperature range is 30-200°C. There is an electronic heating component on the heating chamber, which can quickly heat the air in the chamber to the specified temperature and control the temperature precisely.

The turntable and the smoking machine are connected with the control system, and the control system controls the automatic rotation and switching of the turntable, and is consistent with the cigarette smoking process of the smoking machine, that is, when the first puff is taken, the first communication port communicates with the first intake pipe 11; When the second port is used, switch to the second communication port so that the second communication port communicates with the first air intake pipe 11; When switching, the outside air will not directly enter the first air intake pipe, and the air in the entire suction process comes from each heating chamber, which highly simulates human smoking.

The filter rod holder is a filter tip holder with adjustable circumference, and its circumference can be adjusted to meet all the circumference specifications of commercially available cigarettes. The smoke trap is a Cambridge filter. The gas paths between all components are metal or glass heat-insulated pipelines.

The detection method of the migration amount of the orange flavor component in the filter stick of the present embodiment uses the above-mentioned detection device to carry out as follows:

Insert a temperature-measuring probe at the far lip end of the cigarette with a flavored composite filter of A brand, and insert a temperature-measuring probe into it, smoke it on an ordinary smoking machine, and use the temperature-measuring probe to measure the amount of time passed during each puff. The temperature of the smoke at the beginning of the incense filter, and determine the number of puffs in the whole cigarette.

According to the measured suction temperature and the number of suction ports, set the air temperature in the heating chamber required in the detection device, among which, heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃), heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃) , Heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

Remove the filter tip of the brand A flavored composite filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions (ISO smoking mode), and when you take the first puff, The hot air in the first heating chamber passes through the filter stick; then it is switched by the turntable, when the second port is sucked, the hot air in the second heating chamber passes through the filter rod, and so on, the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and elutes the components of the flavoring compound filter.

The simulated flue gas is eluted and collected by Cambridge filter. The captured Cambridge filter was subjected to ultrasonic extraction with a mixed solution of 50ml ethanol and 150ml acetonitrile, followed by GC-MS analysis under the following conditions:

Chromatographic conditions: chromatographic column is capillary column DB-5 (30 m×0.25mm×0.25μm); carrier gas is helium; volume flow rate is 2.0mL/min, injection volume is 5µL; splitless; heating program: initial temperature 400 ℃, keep for 5min, raise the temperature to 150℃ at 5℃/min, keep for 5min, finally raise the temperature to 280℃ at 10℃/min, keep for 1min;

Mass spectrometry conditions: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600 v; electron energy: 70ev. The analysis results of orange flavor components are shown in Table 1.

Example 2

The detection method of the migration amount of orange flavor components in the filter stick of the present embodiment uses the detection device of embodiment 1 to carry out as follows:

Insert a temperature-measuring probe at the beginning of the fragrance-thread-containing filter cigarette of brand B, smoke it on an ordinary smoking machine, and use the temperature-measuring probe to measure the temperature of the smoke passing through the fragrance thread during each puff. And determine the puff number of the whole cigarette.

According to the measured suction temperature and the number of suction ports, set the air temperature in the heating chamber required in the detection device, among which, heating chamber 1' (first port 35.4°C), heating chamber 2' (second port 36.5°C) ℃), heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃) , Heating chamber 7' (7th port 47.1 ℃). Set the number of suction ports to 7 in total.

Remove the filter tip of brand B flavored line filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber; then switch through the turntable, when the second port is sucked, the hot air in the second heating chamber is drawn through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the fragrance line components.

The simulated flue gas is eluted and collected by Cambridge filter. The captured Cambridge filter was subjected to ultrasonic extraction with a mixed solution of 50ml ethanol and 150ml acetonitrile, followed by GC-MS analysis under the following conditions:

Chromatography: The chromatographic column is a capillary column DB-5 (30 m×0.25mm×0.25μm); the carrier gas is helium; the volume flow rate is 2.0mL/min, the injection volume is 5 µL; splitless; heating program: initial temperature 400 ℃, keep for 5min, raise the temperature to 150℃ at 5℃/min, keep for 5min, finally raise the temperature to 280℃ at 10℃/min, and keep for 1min.

Mass spectrometry: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600 v; electron energy: 70 eV. The rest are the same as in Example 1, and the analysis results of the orange flavor components are shown in Table 1.

Example 3

The detection method of the migration amount of orange flavor components in the filter stick of the present embodiment uses the detection device of embodiment 1 to carry out as follows:

Insert a temperature-measuring probe into the initial part of the cigarette with the preformed paper and flavored filter of brand C, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the temperature that passes through the initial part of the preformed paper during each puff. The temperature of the smoke, and determine the number of puffs in the whole cigarette.

According to the measured suction temperature and the number of suction ports, set the air temperature in the heating chamber required in the detection device, among which, heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃ ), heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), Heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

Remove the filter tip of the brand C shaped paper flavored filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber is sucked; then it is switched through the turntable. When the second port is sucked, the hot air in the second heating chamber is drawn through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the components of the flavored molding paper are eluted.

The simulated flue gas is eluted and collected by Cambridge filter. The captured Cambridge filter was subjected to ultrasonic extraction with a mixed solution of 50ml of ethanol and 150ml of acetonitrile, followed by GC-MS analysis under the following conditions:

Chromatography: The chromatographic column is a capillary column DB-5 (30 m×0.25mm×0.25μm); the carrier gas is helium; the volume flow rate is 2.0mL/min, the injection volume is 5 µL; splitless; heating program: initial temperature 400 ℃, keep for 5min, raise the temperature to 150℃ at 5℃/min, keep for 5min, finally raise the temperature to 280℃ at 10℃/min, and keep for 1min.

Mass spectrometry: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600 v; electron energy: 70 eV. The rest are the same as in Example 1, and the analysis results of the orange flavor components are shown in Table 1.

Example 4

The detection method of the migration amount of orange flavor components in the filter stick of the present embodiment uses the detection device of embodiment 1 to carry out as follows:

Insert a temperature-measuring probe into the starting part of the particulate material-containing filter cigarette of D brand, smoke on an ordinary smoking machine, and measure the temperature of the smoke passing through the starting part of the particulate material through the temperature-measuring probe when each puff is drawn. , and determine the puff number of the whole cigarette.

According to the measured suction temperature and the number of suction ports, set the air temperature in the heating chamber required in the detection device, among which, heating chamber 1' (first port 35.4 °C), heating chamber 2' (second port 36.5 °C ), heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), Heating chamber 7' (7th port 47.1°C). Set the number of suction ports to 7 in total.

Remove the filter tip of brand D filter cigarette containing particulate material from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber; then switch through the turntable, when the second port is sucked, the hot air in the second heating chamber is drawn through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the particulate material components are eluted.

The simulated flue gas is eluted and collected by Cambridge filter. The captured Cambridge filter was subjected to ultrasonic extraction with a mixed solution of 50ml ethanol and 150ml acetonitrile, followed by GC-MS analysis under the following conditions:

Chromatography: The chromatographic column is a capillary column DB-5 (30 m×0.25mm×0.25μm); the carrier gas is helium; the volume flow rate is 2.0mL/min, the injection volume is 5 µL; splitless; heating program: initial temperature 400 ℃, keep for 5min, raise the temperature to 150℃ at 5℃/min, keep for 5min, finally raise the temperature to 280℃ at 10℃/min, and keep for 1min.

Mass spectrometry: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600 v; electron energy: 70 eV. The rest are the same as in Example 1, and the analysis results of the orange flavor components are shown in Table 1.

Example 5

The detection method of the migration amount of orange flavor components in the filter stick of the present embodiment uses the detection device of embodiment 1 to carry out as follows:

Insert a temperature-measuring probe into the beginning of the filter on a cigarette with an E-brand triacetin flavored filter, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the beginning of each puff through the filter The temperature of the smoke, and determine the number of puffs of the whole cigarette.

According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the detection device, temperature heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃), Heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

Remove the filter tip of the brand E triacetin flavored filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions, and when taking the first puff, pass the filter rod The hot air in the first heating chamber is sucked; then it is switched through the turntable, and when the second port is sucked, the hot air in the second heating chamber is drawn through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the flavored triacetin component.

The simulated flue gas is collected by Cambridge filter for flue gas elution. The captured Cambridge filter was subjected to ultrasonic extraction with a mixed solution of 50ml ethanol and 150ml acetonitrile, followed by GC-MS analysis under the following conditions:

Chromatography: The chromatographic column is a capillary column DB-5 (30 m×0.25mm×0.25μm); the carrier gas is helium; the volume flow rate is 2.0mL/min, the injection volume is 5 µL; splitless; heating program: initial temperature 400 ℃, keep for 5min, raise the temperature to 150℃ at 5℃/min, keep for 5min, finally raise the temperature to 280℃ at 10℃/min, and keep for 1min.

Mass spectrometry: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600 v; electron energy: 70 eV. The rest are the same as in Example 1, and the analysis results of the orange flavor components are shown in Table 1.

Example 6

The detection method of the migration amount of orange flavor components in the filter stick of the present embodiment uses the detection device of embodiment 1 to carry out as follows:

Insert a temperature-measuring probe into the part of the F-brand puffed-pear cigarette where the puffed-puff is installed, smoke it on an ordinary smoking machine, use the temperature-measured probe to measure the temperature of the smoke passing through the puff-puff part during each puff, and determine the temperature of the whole cigarette number of suction ports.

According to the measured suction temperature and the number of suction ports, set the air temperature in the heating chamber required in the detection device, among which, heating chamber 1' (first port 35.4 °C), heating chamber 2' (second port 36.5 °C ), heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), Heating chamber 7' (7th port 47.1°C). Set the number of suction ports to 7 in total.

Remove the filter tip of brand F explosive bead cigarette from the cigarette, install it on the filter rod holder, pinch the explosive bead, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber is sucked; then it is switched through the turntable. When the second port is sucked, the hot air in the second heating chamber is drawn through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the added ingredients in the popping beads.

Simulated artificial saliva was used to elution and trap simulated smoke. Using 50ml ethanol and 150ml acetonitrile mixed solution for ultrasonic extraction, followed by GC-MS analysis, the analysis conditions are as follows:

Chromatography: The chromatographic column is a capillary column DB-5 (30 m×0.25mm×0.25μm); the carrier gas is helium; the volume flow rate is 2.0mL/min, the injection volume is 5 µL; splitless; heating program: initial temperature 400 ℃, keep for 5min, raise the temperature to 150℃ at 5℃/min, keep for 5min, finally raise the temperature to 280℃ at 10℃/min, and keep for 1min.

Mass spectrometry: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600v; electron energy: 70ev. The analysis results of orange flavor components are shown in Table 1.

Example 7

The detection method of the migration amount of orange flavor components in the filter stick of the present embodiment uses the detection device of embodiment 1 to carry out as follows:

Insert a temperature-measuring probe at the beginning of the cigarette with the flavor-filter on G brand cigarettes containing the flavor-filter filter, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the temperature of the smoke passing through the flavor-piece during each puff, and determine The number of puffs in a whole cigarette.

According to the measured suction temperature and the number of suction ports, set the air temperature in the heating chamber required in the detection device, among which, heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃ ), heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), Heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

Remove the filter tip of the brand G cigarette containing flavor filter tip from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions. The hot air in the first heating chamber; then switch through the turntable, when the second port is sucked, the hot air in the second heating chamber is drawn through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when smoking a cigarette, and elutes the ingredients of the flavor sheet.

The simulated flue gas is eluted and trapped by cold trap trapping. Using 50ml ethanol and 150ml acetonitrile mixed solution for ultrasonic extraction, followed by GC-MS analysis, the analysis conditions are as follows:

Chromatography: The chromatographic column is a capillary column DB-5 (30 m×0.25mm×0.25μm); the carrier gas is helium; the volume flow rate is 2.0mL/min, the injection volume is 5 µL; splitless; heating program: initial temperature 400 ℃, keep for 5min, raise the temperature to 150℃ at 5℃/min, keep for 5min, finally raise the temperature to 280℃ at 10℃/min, and keep for 1min.

Mass spectrometry: ion source: EI; gas interface temperature: 280°C; transfer line temperature: 280°C; ion source temperature: 230°C; electron multiplier voltage: 1600 v; electron energy: 70 eV. The analysis results of orange flavor components are shown in Table 1.

Table 1 Analysis results of orange flavor components

It can be seen from Table 1 that the sample detection in the above examples is not affected by complex smoke, and can truly reflect the components of the orange-flavored components in the filter.

It can be seen that using the detection device and method of this embodiment can accurately analyze the migration amount of orange-flavored components in the special flavored filter, which improves the analysis sensitivity of the sample and shortens the detection cycle.

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of the present invention. within the scope of protection.

Claims (7)

1. the detection device of orange taste ingredient the amount of migration in a kind of filter stick, it is characterised in that：Including several heating chambers, heating chamber one end Air inlet is connected, the other end connects escape pipe, and escape pipe is arranged around turntable, includes the first air inlet pipe, the first air inlet on turntable Pipe is rotated with turntable, and first air inlet pipe one end is at a time connected to one of escape pipe, the first air inlet pipe other end with Second air inlet pipe one end is connected to, and the second air inlet pipe is fixed, and the other end is connect with filter stick clamper, and filter stick clamper connection flue gas is caught Storage, Fume collector connect smoking machine.

2. detection device according to claim 1, it is characterised in that：Heating chamber is 10, and temperature is equipped in heating chamber Regulating device, heating temperature range are 30-200 DEG C.

3. the detection method of orange taste ingredient the amount of migration in a kind of filter stick, it is characterised in that：It is filled using the detection of claims 1 or 22 It sets and is detected, include the following steps：

Step（1）, puff number determine

It is inserted into thermoprobe at the remote lip end charging starting position containing Flavoring filter of cigarette to be measured, is taken out on conventional smoking machine It inhales, originates the temperature of position flue gas when measuring every mouthful of suction by thermoprobe by Flavoring filter, and determine whole branch cigarette Puff number；

Step（2）, according to puff number set needed for heating chamber temperature

The air themperature in several heating chambers of detection device is set by the practical suction temperatures of cigarette, and sets puff number；

Step（3）, suction

Smoking machine, Fume collector and filter stick clamper are sequentially connected, the filter tip of extraordinary filter tip cigarette is taken from cigarette Under, it is installed on filter stick clamper, starts smoking machine and aspirated by standard conditions, heating of the air from different temperatures of suction Chamber switches successively according to puff number, and every mouthful of gas flow temperature for being aspirated through filter tip is and when the practical suction of cigarette smoking machine Gas flow temperature it is consistent；Flue gas elution trapping is carried out using Fume collector；

Step（4）, constituent analysis；

After trapping, ultrasonic extraction is carried out using ethyl alcohol and acetonitrile mixed solution, carries out GC-MS analyses later.

4. detection method according to claim 3, it is characterised in that：The Trapping ways of Fume collector are caught for cambridge filter Collection, cold trap trapping, absorbing liquid trapping or simulation artificial saliva trapping.

5. detection method according to claim 3, it is characterised in that：Step（4）In, chromatographiccondition is as follows：

Chromatography：Chromatographic column is capillary column DB-5,30 m × 0.25mm × 0.25 μm；Carrier gas is helium；Volume flow is 2.0mL/min, 5 μ L of sample size；It does not shunt；Temperature program：400 DEG C of initial temperature is kept 5min, is warming up to 5 DEG C/min 150 DEG C, 5min is kept, is finally warming up to 280 DEG C with 10 DEG C/min, keeps 1min.

6. detection method according to claim 3, it is characterised in that：Step（4）In, mass spectral analysis condition is as follows：

Mass spectrum：Ion source：EI；Makings interface temperature：280℃；Transmission line temperature is 280 DEG C；Ion source temperature：230℃；Electronics Multiplier voltage：1600 v；Electron energy：70 ev.

7. detection method according to claim 3, it is characterised in that：Step（4）In, using 50ml ethyl alcohol and 150ml second Nitrile mixed solution carries out ultrasonic extraction.