CN110850009A - Simulation determination method for migration of cooling agent component in cigarette filter stick to cigarette smoke - Google Patents

Abstract

The invention relates to a simulation determination method for migration of cooling agent components in a cigarette filter stick to cigarette smoke, and belongs to the technical field of analytical chemistry. The method comprises the following steps: the cigarette filter stick added with the cooling agent is placed into a purging pipe, the device provided by the invention is adopted to simulate real smoking of a cigarette to purge the filter stick, the adsorption cold trap is used for trapping the components of the purged cooling agent, the content of the components of the cooling agent is measured through a gas chromatography-mass spectrometry connected with a dynamic headspace after trapping is finished, and then the mobility is calculated. The method can meet the requirement of accurately measuring the migration quantity of the cooling agent component in the cigarette filter stick to the cigarette smoke, and provides a scientific, simple and convenient new method for objectively evaluating the release and effect of the cooling agent component in the cigarette filter stick.

Description

A simulation method for measuring the migration of cooling agent components in cigarette filter rods to cigarette smoke

technical field

The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for simulating the measurement of the migration of cooling agent components in cigarette filter rods to cigarette smoke.

Background technique

Cooling agents are a class of chemicals that can have a cooling effect on the human mouth and sense of smell. For example, L-menthol, which has the advantages of fresh and cool taste, low price and easy availability, is widely used in many fields such as daily chemicals, food, tobacco, medical and health products, etc. With the increasingly strong demand for cooling flavors by consumers, scientific and technological workers have developed a variety of new cooling agents to meet the consumer needs in different fields. Cool type is more common in foreign countries, and the domestic market demand has also shown an increasing trend in recent years. At present, the common cooling agents in the tobacco industry are L-menthol, isopulegol, menthone, menthyl lactate, menthone glycerol ketal, N-ethyl-p-menthyl-3-carboxamide, 2-isopropyl Base-N,2,3-trimethylbutanamide and other ingredients are usually compounded by a variety of ingredients to meet the taste and durability of cigarettes.

At present, various cigarette manufacturers at home and abroad have developed a number of cigarette cooling agent addition technologies, such as tobacco addition, cigarette paper addition, filter addition and so on. Due to the advantages of avoiding the loss and pyrolysis during the storage and burning of cigarettes, avoiding the loss during the static burning of cigarettes, and increasing the transfer efficiency of functional components, adding a cooling agent to the filter tip is an important method for making cool-flavored cigarettes. . In order to improve the retention effect of adding cooling ingredients and highlight the personalized style of cigarette products, cigarette product developers have also developed new ways to add cooling agents such as popping beads, granules, and incense threads with the goal of expanding consumer groups. At present, new filter materials such as popping beads, granules, and incense threads have been increasingly used in more cigarette brands at home and abroad, and have shown a rapid growth trend.

At present, the methods of analyzing and detecting the components of the cooling agent added to the filter generally adopt the direct determination of the content of the added components in the filter, or use the smoking machine to capture the cigarette smoke for analysis. Direct measurement is simple, but cannot objectively reflect the release of added components into cigarette smoke during smoking. If cigarette smoke is analyzed, the sample analysis process is not complicated, and there are thousands of chemical components produced by cigarette combustion. The complex background will inevitably have a great impact on the analysis of added cooling components. Therefore, how to overcome the deficiencies of the existing technology is an urgent problem to be solved in the field of analytical chemistry technology.

SUMMARY OF THE INVENTION

The purpose of the present invention is to solve the deficiencies of the prior art, and to provide a simulation method for measuring the migration of cooling agent components in a cigarette filter rod to cigarette smoke, which can satisfy the accurate measurement of the migration amount of the cooling flavor components added in the filter rod. It provides a scientific and simple new method for the evaluation of the release amount of the cooling agent added in the filter rod.

Unless otherwise specified, the percentages used in the present invention are by weight.

The purpose of the present invention is achieved through the following technical solutions.

For achieving the above object, the technical scheme adopted in the present invention is as follows:

A simulation method for measuring the migration of cooling agent components in cigarette filter rods to cigarette smoke, using the following devices:

The device includes an airflow preheating chamber, a numerically controlled three-way valve, a purging pipe and a dynamic headspace gas chromatography-mass spectrometry instrument;

The numerical control three-way valve is set between the air preheating chamber and the purging pipe;

The air outlet of the purging pipe is connected with the dynamic headspace gas chromatography-mass spectrometry instrument;

The airflow preheating chamber is connected with the air inlet of the numerical control three-way valve;

It includes the following steps:

Step (1), air purging: put the filter rod into the purging tube, and then start the heating program of the air pre-heating chamber, so that the temperature of the purging air at each puff interval and the actual smoking air of the cigarettes circulate on the smoking machine The temperature of the filter rod is the same; after adjusting the heating program, start to switch through the three-way valve to simulate the suction of a smoking machine to purge the filter rod. When , the airflow directly enters the atmosphere; at the same time, the actual number of puffs of the cigarette is simulated;

Step (2), adsorption trap trapping, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter rod enters the trap of the dynamic headspace gas chromatography-mass spectrometry instrument for trapping. , the cooling agent components adsorbed in the desorption trap are analyzed by high temperature, and then enter the gas chromatography-mass spectrometer to be detected, and the mobility is calculated;

Described cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N,2,3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl -3-Carboxamide and Menthone Glycerol Ketal.

The numerical control three-way valve can realize automatic switching, which can simulate the standard smoking conditions of smoking machines. When the cigarette is in a static combustion state, the air flow does not pass through the filter rod and is directly discharged to the outside. Purge.

Further, preferably, the gas preheating chamber is a quartz glass tube, and infrared radiation is used to preheat the gas in the tube. This setting can realize the temperature program of the gas in the cavity, so that the temperature of the airflow passing through the filter rod is consistent with the actual purging temperature of the cigarette smoke.

Further, preferably, the purging pipe includes a pipe body and a pipe cap; the pipe body and the pipe cap are connected; two sealing rings for fixing the filter rod and only allowing the air flow to pass through the filter tip are arranged in the pipe body , and two sealing rings are respectively arranged at both ends of the filter rod. The sealing ring can realize the sealing between the filter rod and the purging pipe wall, avoid the side passage of the purging air flow, and ensure that the air flow can pass through the filter rod. By adjusting the size and position of the sealing ring up and down, it can meet the needs of all cigarette filter specifications, such as conventional cigarettes, medium cigarettes, thin cigarettes, long filter cigarettes, short filter cigarettes, etc., as shown in Figure 3.

Further, preferably, in step (1), the filter rod is purged by simulating the ISO standard suction mode, continuously purging for 2 seconds in every 1 minute, and the flow rate of the purging airflow is 17.5 mL/min; simulating Canadian deep pumping The filter rod is purged in suction mode, continuously purged for 2 seconds every 30 times, and the flow rate of the purge airflow is 22.5mL/min; purge 8-10 times.

That is to simulate the ISO standard smoking mode to purge the filter rod and simulate the 2s smoking time of cigarettes. Enter the purging pipe to purge and elute the explosive beads in the filter rod. The purging time is 2s; after that, simulate the time of 58s of cigarette static combustion. The air inlet enters the air inlet, and then enters the atmosphere from the other air outlet, without passing through the filter rod.

Purge 8-10 times, that is, simulate 8-10 suctions.

Further, it is preferred that, in step (2), the adsorption material of the trap is polybutadiene-coated silica gel particles, which have large adsorption capacity for cooling agent components, good stability at high temperature, adsorption and desorption Reversible and can be reused many times. The trap temperature is -10°C, the high temperature analytical desorption temperature is 180-240°C, the desorption time is 2-5min, the transfer line temperature is 220-260°C, and the valve box temperature is 220-260°C.

Further, preferably, the preparation method of polybutadiene-coated silica gel particles is as follows:

Add polybutadiene, sensitizer and toluene into the beaker, and after mixing, add silica gel particles modified with triethoxyvinylsilane, ultrasonically vibrate the reaction, after the reaction is completed, the toluene is evaporated by rotary evaporation, and then added to the container. Argon gas is introduced into the container with the product, and after being sealed, radiation crosslinking is carried out, then washed with benzene and acetone in turn, and dried to obtain the final product;

The mass ratio of polybutadiene, sensitizer, and triethoxyvinylsilane-modified silica gel particles is 12~15:1.0~1.5:120~150;

The ratio of the mass of polybutadiene to the volume of toluene is 12 to 15 g: 0.8 to 1.2 L.

Further, it is preferred that the particle size of the silica gel particles is 100-150 mesh; the drying temperature is 200°C, and the time is 6h; the ultrasonic oscillation time is 35-45min; the quality of the benzene and acetone used for washing are both triethoxy The mass of the silica gel particles modified by vinyl silane is 2~3 times; the sensitizer is ethylene glycol bismethacrylate or diethylene glycol bismethacrylate.

Further, preferably, in step (2), the gas chromatography conditions are as follows: the chromatographic column is an HP-Innowax elastic quartz capillary column with a specification of 30 m × 0.25 mm × 0.25 μm ; the inlet temperature is 250 ° C; the split ratio is 20 : 1; the initial oven temperature was held at 50 °C for 1 min, then increased to 100 °C at 10 °C/min, then increased to 210 °C at 5 °C/min, and then increased to 240 °C at 30 °C/min, held for 5 min; carrier gas For helium, constant flow 1.0mL/min.

Further, preferably, in step (2), the mass spectrometry conditions are as follows: the temperature of the auxiliary interface is 220 °C; the ionization mode is electron bombardment source, the ionization energy is 70 eV, the temperature of the ion source is 230 °C, the temperature of the quadrupole is 150 °C, and the solvent delay time 4.0 min, using selected ion monitoring mode.

Further, preferably, in step (2), the method for calculating the mobility is: the amount of the simulated actual suction cooling agent component measured by gas chromatography-mass spectrometer is divided by the total amount of the cooling agent component, The mobility was obtained; mobility=(peak area simulating actual suction measurement results/peak area of total amount)×100%.

When simulating the actual suction of the amount of cooling agent components, every time a filter rod is purged, a new filter rod is replaced and purged again, and a total of not less than 5 filter rods are used;

The method for detecting the total amount of the cooling agent components is as follows: use the same device, replace a new filter rod, use 180-240 ℃ gas to continuously purge the filter rod for 8-15 minutes, and replace the new filter rod after purging Continue purging, and purge no less than 5 filter rods in total (the number of filter rods purging is the same as the number of purging components when simulating the actual suction of cooling agent components), and measure the total amount of cooling agent components . The total measurement conditions of trapping, desorption, GC, and MS are exactly the same as the measurement conditions for simulating the actual suction of the cooling agent components.

This is because the cooling agent components only migrate in a small amount. In order to reach the quantitative limit of the instrument, at least 5 filter rods should be purged accumulatively.

When the heating program is set in the present invention, for cigarettes of different specifications, the smoking machine is actually smoked first, and the actual temperature of the smoke passing through the filter rod is measured by a thermocouple, and then the setting is made according to the measurement result.

The principle of the ion selection parameter of the present invention: in the mass spectrometry ion fragments of each solvent residue, ions with higher specificity and response are selected as quantitative ions; other 1-2 fragment ions are selected as auxiliary qualitative ions. The ion selection parameters are shown in Table 1. Typical chromatogram 4.

Table 1. Quantitative and qualitative selected ions of cooling agent components

Further, preferably, in order to achieve quantitative analysis of cooling agent components, 7 kinds of cooling agent reference substances are used in the present invention to prepare a mixture of six concentration levels of 250, 100, 50, 25, 10 and 1.0 mg/mL. Standard working solution preparation solution, inject 1.0 µL under the preferred chromatographic conditions to prepare the working curve, and the cooling agent components entering the chromatographic system are 250, 100, 50, 25, 10 and 1.0 µg respectively. Taking the response value (chromatographic peak) of the quantitative ion of the cooling agent as the Y value of the ordinate, and the concentration of the cooling agent as the X value of the abscissa, the working curve is shown in Table 2. According to the comparison of the chromatographic peak signal of the sample to be tested and the working curve, the quantitative analysis of the components of the migratory cooling agent can be realized.

Table 2. Working curves of seven cooling agents

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

(1), the inventive method comprehensively considers the transfer of the cooling agent component compounds in the cigarette filter rod to the cigarette smoke, overcomes the traditional filter rod cooling agent composition detection method, mainly measures the total content in the filter rod , without considering their migration into cigarette smoke. The method of the invention can accurately measure the migration rate of the cooling components added in the cigarette filter rod to the cigarette smoke, so as to determine the release amount and release rule of the added cooling components. The measurement results of the method can effectively guide different types of The addition amount and proportion of cooling flavor in cigarette filter rods, and can objectively evaluate the actual effect of cooling flavor cigarette filter rods.

(2) The present invention adopts the device with simple structure and easy operation. Compared with the direct analysis of cigarette smoke, the interference caused by the complex background generated by cigarette combustion on the determination of cooling agent components can be deducted; the entire analysis process is online operation, which avoids errors caused by multiple sample transfers in other methods. The component determination results are more accurate and reliable; and compared with other simulated migration devices, the device simulation of the present invention is closer to the actual situation of cigarette smoking, and the obtained results are more objective and reliable.

(3), in the present invention, a precision purging tube is adopted, and the purging tube is a ferrule type structure with a sealing ring, and the sealing ring can realize the sealing between the filter rod and the purging tube wall, so as to avoid the side of the purging airflow passing through (Ensure that the airflow can pass through the filter rod). Through the adjustment of the size and position of the sealing ring (upper and lower), it can meet the testing requirements of all specifications of cigarette filter rods (conventional cigarettes, medium cigarettes, thin cigarettes, long filter cigarettes, short filter cigarettes, etc.).

(4) In the present invention, polybutadiene-coated silica gel is also used for the first time as the adsorption material of the trap. The material has large adsorption capacity, good stability at high temperature, good reversibility of adsorption and desorption of cooling agent component compounds, and high adsorption and analytical completeness of the components to be tested, which can significantly improve the accuracy and precision of analysis results.

Description of drawings

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

Figure 2 is an exploded view of the purge pipe;

Among them, 1. Airflow preheating chamber; 2. Numerical control three-way valve; 3. Purge pipe; 3-1, pipe body; 3-2, pipe body; 3-3, sealing ring; 4, dynamic headspace gas chromatography Mass spectrometry instrument; 5, filter rod; 5-1, upper filter rod core; 5-2, lower filter rod core; 5-3, tipping paper; 6, explosive beads;

Fig. 3 is the schematic diagram of installing different types of cigarette filter rods in the purging pipe; wherein, a is a filter rod of a conventional cigarette, b is a filter rod of a thin cigarette, and c is a filter rod of a short filter cigarette;

Fig. 4 is the detection chromatogram of 7 kinds of cooling agent standards;

Wherein, 1 is menthone, 2 is isopulegol, 3 is L-menthol, 4 is 2-isopropyl-N,2,3-trimethylbutanamide (WS-23), and 5 is menthyl lactate ester, 6 is N-ethyl-p-menthyl-3-carboxamide (WS-3), 7 is menthone glycerol ketal.

Detailed ways

The present invention will be further described in detail below in conjunction with the embodiments.

Those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. If no specific technology or condition is indicated in the examples, the technology or condition described in the literature in the field or the product specification is used. If the materials or equipment used are not marked with the manufacturer, they are all conventional products that can be obtained through purchase.

The triethoxyvinylsilane-modified silica gel particles used in the present invention are purchased from Nanjing Nengde New Material Technology Co., Ltd., and are spherical silica gel, 100-150 mesh.

Example 1

A simulation method for measuring the migration of cooling agent components in a cigarette filter rod to cigarette-smoke, using the following devices:

As shown in Figures 1 to 3, the device comprises an airflow preheating chamber 1, a numerically controlled three-way valve 2, a purge pipe 3 and a dynamic headspace gas chromatography-mass spectrometry instrument 4;

The numerical control three-way valve 2 is arranged between the airflow preheating chamber 1 and the purging pipe 3;

The air outlet of the purging pipe 3 is connected with the dynamic headspace gas chromatography-mass spectrometry instrument 4;

The airflow preheating chamber 1 is connected to the air inlet of the numerically controlled three-way valve 2 .

It includes the following steps:

Step (1), air purging: put the filter rod into the purging tube, and then start the heating program of the air pre-heating chamber, so that the temperature of the purging air at each puff interval and the actual smoking air of the cigarettes circulate on the smoking machine The temperature of the filter rod is the same; after adjusting the heating program, start to switch through the three-way valve to simulate the suction of a smoking machine to purge the filter rod. When , the airflow directly enters the atmosphere; at the same time, the actual number of puffs of the cigarette is simulated;

Step (2), adsorption trap trapping, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter rod enters the trap of the dynamic headspace gas chromatography-mass spectrometry instrument for trapping. , the cooling agent components adsorbed in the desorption trap are analyzed by high temperature, and then enter the gas chromatography-mass spectrometer to be detected, and the mobility is calculated;

Described cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N,2,3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl -3-Carboxamide and Menthone Glycerol Ketal.

In step (1), the filter rod was purged by simulating the ISO standard suction mode, continuously purging for 2 seconds every 1 minute, the flow rate of the purging gas flow was 17.5 mL/min, and the purging was performed 8 times.

In step (2), the adsorption material of the trap is polybutadiene-coated silica gel particles, the temperature of the trap is -10°C, the high-temperature desorption temperature is 200°C, the desorption time is 3min, and the temperature of the transmission line is 220°C. Valve box temperature 220 ℃.

In step (2), the gas chromatography conditions are as follows: the chromatographic column is an HP-Innowax elastic quartz capillary column with a specification of 30 m×0.25 mm×0.25 μm ; the inlet temperature is 250° C.; the split ratio is 20:1; The temperature was kept at 50°C for 1 min, then increased to 100°C at 10°C/min, then increased to 210°C at 5°C/min, then increased to 240°C at 30°C/min, and held for 5min; the carrier gas was helium, constant flow 1.0mL/min.

In step (2), the mass spectrometry conditions are as follows: the auxiliary interface temperature is 220 °C; the ionization mode is electron bombardment source, the ionization energy is 70 eV, the ion source temperature is 230 °C, the quadrupole temperature is 150 °C, the solvent delay time is 4.0 min, and the selected ion is used. monitoring mode.

In step (2), in step (2), the method for calculating the mobility is as follows: the amount of the simulated actual suction cooling agent component measured by gas chromatography-mass spectrometry is divided by the total amount of the cooling agent component, get the mobility;

When simulating the measurement of the actual suction of the cooling agent components, every time a filter rod is purged, a new filter rod is replaced, and purging again, a total of 5 filter rods are used;

The method for detecting the total amount of the cooling agent components is as follows: use the same device, replace a new filter rod, use 200 ℃ gas to continuously purge the filter rod for 10 minutes, and then replace the new filter rod to continue purging after purging. Purge 5 filter rods to determine the total amount of cooling agent components.

The test cigarette filter rods were conventional cigarettes (cooling agent was added with triacetin during the filter rod forming process), and the size was 30 mm.

The determination results showed that three cooling components, isopulegol, L-menthol and WS-23, were detected in the filter rod, and the total contents were 34.2, 221.8 and 155.2 μg/piece, respectively, which migrated to cigarette smoke and simulated the release. The amount of cigarette smoke was 5.47, 29.1 and 18.4 μg/stick, respectively, and the simulated measurement results of the mobility from the filter rod to cigarette smoke were 16.0%, 13.1% and 11.9%, respectively.

Example 2

A simulation method for measuring the migration of cooling agent components in cigarette filter rods to cigarette smoke, using the following devices:

As shown in Figures 1 to 3, the device comprises an airflow preheating chamber 1, a numerically controlled three-way valve 2, a purge pipe 3 and a dynamic headspace gas chromatography-mass spectrometry instrument 4;

The numerical control three-way valve 2 is arranged between the airflow preheating chamber 1 and the purging pipe 3;

The air outlet of the purging pipe 3 is connected with the dynamic headspace gas chromatography-mass spectrometry instrument 4;

The airflow preheating chamber 1 is connected to the air inlet of the numerically controlled three-way valve 2 .

The airflow preheating chamber 1 is a quartz glass tube, and infrared radiation is used to preheat the gas in the tube.

The purging pipe 3 includes a pipe body 3-1 and a pipe cap 3-2; the pipe body 3-1 and the pipe cap 3-2 are connected; Two sealing rings 3-3 that allow the airflow to pass through the filter tip, the two sealing rings 3-3 are respectively arranged at both ends of the filter rod 5;

It includes the following steps:

Step (1), air purging: put the filter rod into the purging tube, and then start the heating program of the air pre-heating chamber, so that the temperature of the purging air at each puff interval and the actual smoking air of the cigarettes circulate on the smoking machine The temperature of the filter rod is the same; after adjusting the heating program, start to switch through the three-way valve to simulate the suction of a smoking machine to purge the filter rod. When , the airflow directly enters the atmosphere; at the same time, the actual number of puffs of the cigarette is simulated;

Step (2), adsorption trap trapping, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter rod enters the trap of the dynamic headspace gas chromatography-mass spectrometry instrument for trapping. , the cooling agent components adsorbed in the desorption trap are analyzed by high temperature, and then enter the gas chromatography-mass spectrometer to be detected, and the mobility is calculated;

Described cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N,2,3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl -3-Carboxamide and Menthone Glycerol Ketal.

In step (1), the filter rod was purged by simulating the ISO standard suction mode, continuously purging for 2 seconds every 1 minute, and the flow rate of the purge air flow was 17.5 mL/min; purging was performed 8 times.

In step (2), the adsorption material of the trap is polybutadiene-coated silica gel particles, the temperature of the trap is -10°C, the high-temperature desorption temperature is 240°C, the desorption time is 5min, and the transmission line temperature is 260°C. The valve box temperature is 260°C.

In step (2), the gas chromatography conditions are as follows: the chromatographic column is an HP-Innowax elastic quartz capillary column with a specification of 30 m×0.25 mm×0.25 μm ; the inlet temperature is 250° C.; the split ratio is 20:1; The temperature was kept at 50°C for 1 min, then increased to 100°C at 10°C/min, then increased to 210°C at 5°C/min, then increased to 240°C at 30°C/min, and held for 5min; the carrier gas was helium, constant flow 1.0mL/min.

In step (2), the mass spectrometry conditions are as follows: the auxiliary interface temperature is 220 °C; the ionization mode is electron bombardment source, the ionization energy is 70 eV, the ion source temperature is 230 °C, the quadrupole temperature is 150 °C, the solvent delay time is 4.0 min, and the selected ion is used. monitoring mode.

In step (2), in step (2), the method for calculating the mobility is as follows: the amount of the simulated actual suction cooling agent component measured by gas chromatography-mass spectrometry is divided by the total amount of the cooling agent component, get the mobility;

When simulating the measurement of the actual suction of the cooling agent components, every time a filter rod is purged, a new filter rod is replaced, and purging again, a total of 6 filter rods are used;

The method for detecting the total amount of the cooling agent components is as follows: using the same device, replacing a new filter rod, using 180 ° C gas to continuously purge the filter rod for 15 minutes, and then replacing the new filter rod to continue purging after purging. A total of 6 filter rods were purged to determine the total amount of cooling agent components.

The test cigarette filter rods were conventional cigarette gel flavor-carrying filter rods with a size of 30 mm.

The measurement results showed that: Menthone, isopulegol, L-menthol and menthyl lactate were detected in the filter rod, and the total contents were 55.6, 112.8, 187.4, and 76.3 µg/piece, respectively. The simulated release amounts of cigarette smoke migration were 9.62, 17.8, 23.9 and 6.92 μg/cigarette, respectively, and the simulated measurement results of the migration rate from filter rod to cigarette smoke were 17.3%, 15.8%, 12.8% and 9.1%, respectively.

Example 3

A simulation method for measuring the migration of cooling agent components in a cigarette filter rod to cigarette smoke, characterized in that the following device is used:

As shown in Figures 1 to 3, the device comprises an airflow preheating chamber 1, a numerically controlled three-way valve 2, a purge pipe 3 and a dynamic headspace gas chromatography-mass spectrometry instrument 4;

The numerical control three-way valve 2 is arranged between the airflow preheating chamber 1 and the purging pipe 3;

The air outlet of the purging pipe 3 is connected with the dynamic headspace gas chromatography-mass spectrometry instrument 4;

The airflow preheating chamber 1 is connected to the air inlet of the numerically controlled three-way valve 2 .

The airflow preheating chamber 1 is a quartz glass tube, and infrared radiation is used to preheat the gas in the tube.

The purging pipe 3 includes a pipe body 3-1 and a pipe cap 3-2; the pipe body 3-1 and the pipe cap 3-2 are connected; Two sealing rings 3-3 that allow the airflow to pass through the filter tip, the two sealing rings 3-3 are respectively arranged at both ends of the filter rod 5;

It includes the following steps:

Step (1), air purging: put the filter rod into the purging tube, and then start the heating program of the air pre-heating chamber, so that the temperature of the purging air at each puff interval and the actual smoking air of the cigarettes circulate on the smoking machine The temperature of the filter rod is the same; after adjusting the heating program, start to switch through the three-way valve to simulate the suction of a smoking machine to purge the filter rod. At the same time, the actual number of puffs of cigarettes is simulated;

Step (2), adsorption trap trapping, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter rod enters the trap of the dynamic headspace gas chromatography-mass spectrometry instrument for trapping. , the cooling agent components adsorbed in the desorption trap are analyzed by high temperature, and then enter the gas chromatography-mass spectrometer to be detected, and the mobility is calculated;

Described cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N,2,3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl -3-Carboxamide and Menthone Glycerol Ketal.

In step (1), the filter rod was purged by simulating the ISO standard suction mode, continuously purging for 2 seconds every 1 minute, and the flow rate of the purge air flow was 17.5 mL/min; purging was performed 9 times.

In step (2), the adsorption material of the trap is polybutadiene-coated silica gel particles, the temperature of the trap is -10°C, the high-temperature desorption temperature is 180°C, the desorption time is 2min, and the transmission line temperature is 240°C. The valve box temperature is 250°C.

In step (2), the gas chromatography conditions are as follows: the chromatographic column is an HP-Innowax elastic quartz capillary column with a specification of 30 m×0.25 mm×0.25 μm ; the inlet temperature is 250° C.; the split ratio is 20:1; The temperature was kept at 50°C for 1 min, then increased to 100°C at 10°C/min, then increased to 210°C at 5°C/min, then increased to 240°C at 30°C/min, and held for 5min; the carrier gas was helium, constant flow 1.0mL/min.

In step (2), the mass spectrometry conditions are as follows: the auxiliary interface temperature is 220 °C; the ionization mode is electron bombardment source, the ionization energy is 70 eV, the ion source temperature is 230 °C, the quadrupole temperature is 150 °C, the solvent delay time is 4.0 min, and the selected ion is used. monitoring mode.

In step (2), in step (2), the method for calculating the mobility is as follows: the amount of the simulated actual suction cooling agent component measured by gas chromatography-mass spectrometry is divided by the total amount of the cooling agent component, get the mobility;

When simulating the measurement of the actual suction of the cooling agent components, every time a filter rod is purged, a new filter rod is replaced, and purging again, a total of 5 filter rods are used;

The method for detecting the total amount of the cooling agent components is as follows: use the same device, replace a new filter rod, use 240 ℃ gas to continuously purge the filter rod for 8 minutes, and then replace the new filter rod to continue purging after purging. Purge 5 filter rods to determine the total amount of cooling agent components.

The test cigarette filter rod is a conventional cigarette bead filter rod with a size of 25 mm. Remove the filter rod from the cigarette and pinch the bursting beads, and put them into the purge tube.

The determination results showed that: Menthone, isopulegol, L-menthol and WS-23 were detected in the samples, and the total contents were 118.2, 122.6, 202.7, and 63.4 µg/piece, respectively. The simulated release amounts of gas migration were 16.78, 15.22, 22.35 and 6.27 μg/stick, respectively, and the simulated measurement results of the migration rate from filter rod to cigarette smoke were 14.2%, 12.4%, 11.0% and 9.9%, respectively.

Example 4

A simulation method for measuring the migration of cooling agent components in cigarette filter rods to cigarette smoke, using the following devices:

As shown in Figures 1 to 3, the device comprises an airflow preheating chamber 1, a numerically controlled three-way valve 2, a purge pipe 3 and a dynamic headspace gas chromatography-mass spectrometry instrument 4;

The numerical control three-way valve 2 is arranged between the airflow preheating chamber 1 and the purging pipe 3;

The air outlet of the purging pipe 3 is connected with the dynamic headspace gas chromatography-mass spectrometry instrument 4;

The airflow preheating chamber 1 is connected to the air inlet of the numerically controlled three-way valve 2 .

The airflow preheating chamber 1 is a quartz glass tube, and infrared radiation is used to preheat the gas in the tube.

The purging pipe 3 includes a pipe body 3-1 and a pipe cap 3-2; the pipe body 3-1 and the pipe cap 3-2 are connected; Two sealing rings 3-3 that allow the airflow to pass through the filter tip, the two sealing rings 3-3 are respectively arranged at both ends of the filter rod 5;

It includes the following steps:

Step (1), air purging: put the filter rod into the purging tube, and then start the heating program of the air pre-heating chamber, so that the temperature of the purging air at each puff interval and the actual smoking air of the cigarettes circulate on the smoking machine The temperature of the filter rod is the same; after adjusting the heating program, start to switch through the three-way valve to simulate the suction of a smoking machine to purge the filter rod. At the same time, the actual number of puffs of cigarettes is simulated;

Step (2), adsorption trap trapping, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter rod enters the trap of the dynamic headspace gas chromatography-mass spectrometry instrument for trapping. , the cooling agent components adsorbed in the desorption trap are analyzed by high temperature, and then enter the gas chromatography-mass spectrometer to be detected, and the mobility is calculated;

Described cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N,2,3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl -3-Carboxamide and Menthone Glycerol Ketal.

In step (1), the filter rod was purged by simulating the ISO standard suction mode, continuously purging for 2 seconds every 1 minute, the flow rate of the purge air flow was 17.5 mL/min, and purging was performed 9 times.

In step (2), the adsorption material of the trap is polybutadiene-coated silica gel particles, the temperature of the trap is -10°C, the high-temperature desorption temperature is 200°C, the desorption time is 3min, and the transmission line temperature is 240°C. Valve box temperature 240 ℃.

The preparation method of polybutadiene-coated silica gel particles is as follows: add polybutadiene, sensitizer and toluene in a beaker, after mixing, add silica gel particles modified with triethoxyvinylsilane, and ultrasonically vibrate Reaction, after the reaction is finished, the toluene is evaporated by rotary evaporation, then argon is introduced into the container containing the product, and radiation crosslinking is carried out after sealing, followed by washing with benzene and acetone, and drying to obtain the final product;

The mass ratio of polybutadiene, sensitizer, and triethoxyvinylsilane-modified silica gel particles is 12:1.0:120;

The ratio of the mass of polybutadiene to the volume of toluene was 12 g:0.8 L.

The particle size of the silica gel particles is 100~150 mesh; the ultrasonic oscillation time is 35min; the mass of benzene and acetone used for washing are 2 times the mass of the silica gel particles modified by triethoxyvinylsilane; the sensitizer is dimethyl methacrylate Ethylene glycol acrylate.

In step (2), the gas chromatography conditions are as follows: the chromatographic column is an HP-Innowax elastic quartz capillary column with a specification of 30 m×0.25 mm×0.25 μm ; the inlet temperature is 250° C.; the split ratio is 20:1; The temperature was kept at 50°C for 1 min, then increased to 100°C at 10°C/min, then increased to 210°C at 5°C/min, then increased to 240°C at 30°C/min, and held for 5min; the carrier gas was helium, constant flow 1.0mL/min.

In step (2), the mass spectrometry conditions are as follows: the auxiliary interface temperature is 220 °C; the ionization mode is electron bombardment source, the ionization energy is 70 eV, the ion source temperature is 230 °C, the quadrupole temperature is 150 °C, the solvent delay time is 4.0 min, and the selected ion is used. monitoring mode.

In step (2), in step (2), the method for calculating the mobility is as follows: the amount of the simulated actual suction cooling agent component measured by gas chromatography-mass spectrometry is divided by the total amount of the cooling agent component, get the mobility;

When simulating the measurement of the actual suction of the cooling agent components, every time a filter rod is purged, a new filter rod is replaced, and purging again, a total of 5 filter rods are used;

The method for detecting the total amount of the cooling agent components is as follows: use the same device, replace a new filter rod, use 200 ℃ gas to continuously purge the filter rod for 5 minutes, and then replace the new filter rod to continue purging after purging. Purge 5 filter rods to determine the total amount of cooling agent components.

The test cigarette filter rod is a regular cigarette with a 30 mm incense stick.

The determination results showed that four cooling components, L-menthol, menthyl lactate, WS-3 and menthone glycerol ketal were detected in the samples, and the total contents were 194.6, 208.7 , 155.2 and 88.4 µg/piece, respectively. The simulated release amounts of cigarette smoke migration were 21.62, 18.92, 15.37 and 7.24 μg/cigarette, respectively, and the simulated measurement results of the migration rate from the filter rod to cigarette smoke were 11.1%, 9.1%, 9.9% and 8.2%, respectively.

Example 5

A simulation method for measuring the migration of cooling agent components in a cigarette filter rod to cigarette smoke, characterized in that the following device is used:

As shown in Figures 1 to 3, the device comprises an airflow preheating chamber 1, a numerically controlled three-way valve 2, a purge pipe 3 and a dynamic headspace gas chromatography-mass spectrometry instrument 4;

The numerical control three-way valve 2 is arranged between the airflow preheating chamber 1 and the purging pipe 3;

The air outlet of the purging pipe 3 is connected with the dynamic headspace gas chromatography-mass spectrometry instrument 4;

The airflow preheating chamber 1 is connected to the air inlet of the numerically controlled three-way valve 2 .

The airflow preheating chamber 1 is a quartz glass tube, and infrared radiation is used to preheat the gas in the tube.

The purging pipe 3 includes a pipe body 3-1 and a pipe cap 3-2; the pipe body 3-1 and the pipe cap 3-2 are connected; The two sealing rings 3-3 that allow the airflow to pass through the filter tip are respectively arranged at both ends of the filter rod 5;

It includes the following steps:

Step (1), air purging: put the filter rod into the purging tube, and then start the heating program of the air pre-heating chamber, so that the temperature of the purging air at each puff interval and the actual smoking air of the cigarettes circulate on the smoking machine The temperature of the filter rod is the same; after adjusting the heating program, start to switch through the three-way valve to simulate the suction of a smoking machine to purge the filter rod. When , the airflow directly enters the atmosphere; at the same time, the actual number of puffs of the cigarette is simulated;

Step (2), adsorption trap trapping, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter rod enters the trap of the dynamic headspace gas chromatography-mass spectrometry instrument for trapping. , the cooling agent components adsorbed in the desorption trap are analyzed by high temperature, and then enter the gas chromatography-mass spectrometer to be detected, and the mobility is calculated;

Described cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N,2,3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl -3-Carboxamide and Menthone Glycerol Ketal.

In step (1), the filter rod was purged in a simulated Canadian deep suction mode, continuously purged for 2 seconds every 30, and the flow rate of the purge air flow was 22.5 mL/min; 9 ports were purged.

In step (2), the adsorption material of the trap is polybutadiene-coated silica gel particles, the temperature of the trap is -10°C, the high-temperature desorption temperature is 190°C, the desorption time is 3.2min, and the transmission line temperature is 250°C , the valve box temperature 250 ℃.

The preparation method of polybutadiene-coated silica gel particles is as follows: add polybutadiene, sensitizer and toluene in a beaker, after mixing, add silica gel particles modified with triethoxyvinylsilane, and ultrasonically vibrate Reaction, after the reaction is finished, the toluene is evaporated by rotary evaporation, then argon is introduced into the container containing the product, and radiation crosslinking is carried out after sealing, followed by washing with benzene and acetone, and drying to obtain the final product;

The mass ratio of polybutadiene, sensitizer, and triethoxyvinylsilane-modified silica gel particles is 15:1.5:150;

The ratio of the mass of polybutadiene to the volume of toluene was 15 g: 1.2 L.

The particle size of the silica gel particles is 100~150 mesh; the drying temperature is 200°C, and the time is 6h; the ultrasonic oscillation time is 45min; the quality of the benzene and acetone used for washing are both triethoxyvinylsilane-modified silica gel The particle mass is 3 times; the sensitizer is ethylene glycol bismethacrylate.

In step (2), the gas chromatography conditions are as follows: the chromatographic column is an HP-Innowax elastic quartz capillary column with a specification of 30 m×0.25 mm×0.25 μm ; the inlet temperature is 250° C.; the split ratio is 20:1; The temperature was kept at 50°C for 1 min, then increased to 100°C at 10°C/min, then increased to 210°C at 5°C/min, then increased to 240°C at 30°C/min, and held for 5min; the carrier gas was helium, constant flow 1.0mL/min.

In step (2), the mass spectrometry conditions are as follows: the auxiliary interface temperature is 220 °C; the ionization mode is electron bombardment source, the ionization energy is 70 eV, the ion source temperature is 230 °C, the quadrupole temperature is 150 °C, the solvent delay time is 4.0 min, and the selected ion is used. monitoring mode.

In step (2), in step (2), the method for calculating the mobility is as follows: the amount of the simulated actual suction cooling agent component measured by gas chromatography-mass spectrometry is divided by the total amount of the cooling agent component, get the mobility;

When simulating the measurement of the actual suction of the cooling agent components, every time a filter rod is purged, a new filter rod is replaced, and purging again, a total of 5 filter rods are used;

The method for detecting the total amount of the cooling agent components is as follows: use the same device, replace a new filter rod, use 180° C. gas to continuously purge the filter rod for 10 min, and then replace the new filter rod to continue purging after purging. A total of 5 filter rods were purged to determine the total amount of cooling agent components.

The test cigarette filter rod is a fine cigarette bead filter rod with a size of 35 mm. Remove the filter rod from the cigarette and pinch the bursting beads, and put them into the purge tube.

The determination results showed that: Menthone, isopulegol and L-menthol were detected in the samples, and the total contents were 208.4, 155.7 and 122.6 μg/piece, respectively, and the simulated releases to cigarette smoke were 28.32, 18.67 and 15.79 µg/stick, and the simulated results of the migration rate from filter rod to cigarette smoke were 13.6%, 12.0% and 12.9%, respectively.

Example 6

A simulation method for measuring the migration of cooling agent components in a cigarette filter rod to cigarette smoke, characterized in that the following device is used:

As shown in Figures 1 to 3, the device comprises an airflow preheating chamber 1, a numerically controlled three-way valve 2, a purge pipe 3 and a dynamic headspace gas chromatography-mass spectrometry instrument 4;

The numerical control three-way valve 2 is arranged between the airflow preheating chamber 1 and the purging pipe 3;

The air outlet of the purging pipe 3 is connected with the dynamic headspace gas chromatography-mass spectrometry instrument 4;

The airflow preheating chamber 1 is connected to the air inlet of the numerically controlled three-way valve 2 .

The airflow preheating chamber 1 is a quartz glass tube, and infrared radiation is used to preheat the gas in the tube.

The purging pipe 3 includes a pipe body 3-1 and a pipe cap 3-2; the pipe body 3-1 and the pipe cap 3-2 are connected; The two sealing rings 3-3 that allow the airflow to pass through the filter tip are respectively arranged at both ends of the filter rod 5;

It includes the following steps:

Step (1), air purging: put the filter rod into the purging tube, and then start the heating program of the air pre-heating chamber, so that the temperature of the purging air at each puff interval and the actual smoking air of the cigarettes circulate on the smoking machine The temperature of the filter rod is the same; after adjusting the heating program, start to switch through the three-way valve to simulate the suction of a smoking machine to purge the filter rod. When , the airflow directly enters the atmosphere; at the same time, the actual number of puffs of the cigarette is simulated;

Step (2), adsorption trap trapping, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter rod enters the trap of the dynamic headspace gas chromatography-mass spectrometry instrument for trapping. , the cooling agent components adsorbed in the desorption trap are analyzed by high temperature, and then enter the gas chromatography-mass spectrometer to be detected, and the mobility is calculated;

Described cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N,2,3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl -3-Carboxamide and Menthone Glycerol Ketal.

In step (1), the filter rod was purged in a simulated Canadian deep suction mode, continuously purged for 2 seconds every 30 days, and the flow rate of the purge airflow was 22.5 mL/min; purging was performed 9 times.

In step (2), the adsorption material of the trap is polybutadiene-coated silica gel particles, the temperature of the trap is -10°C, the high-temperature desorption temperature is 200°C, the desorption time is 2.8min, and the transmission line temperature is 230°C , the valve box temperature 230 ℃.

Add polybutadiene, sensitizer and toluene into the beaker, and after mixing, add silica gel particles modified with triethoxyvinylsilane, ultrasonically vibrate the reaction, after the reaction is completed, the toluene is evaporated by rotary evaporation, and then added to the container. Argon gas is introduced into the container with the product, and after being sealed, radiation crosslinking is carried out, then washed with benzene and acetone in turn, and dried to obtain the final product;

The preparation method of polybutadiene-coated silica gel particles is as follows: add polybutadiene, sensitizer and toluene in a beaker, after mixing, add silica gel particles modified with triethoxyvinylsilane, and ultrasonically vibrate Reaction, after the reaction is finished, the toluene is evaporated by rotary evaporation, then argon is introduced into the container containing the product, and radiation crosslinking is carried out after sealing, followed by washing with benzene and acetone, and drying to obtain the final product;

The mass ratio of polybutadiene, sensitizer, and triethoxyvinylsilane-modified silica gel particles is 13:1.2:145;

The ratio of the mass of polybutadiene to the volume of toluene was 13 g:1 L.

The particle size of the silica gel particles is 100-150 mesh; the drying temperature is 200°C, and the time is 6h; the ultrasonic oscillation time is 40min; the mass of benzene and acetone used for washing are respectively triethoxyvinylsilane-modified silica gel The mass of particles is 2.3 and 2.7 times; the sensitizer is triethylene glycol bismethacrylate;

In step (2), the gas chromatography conditions are as follows: the chromatographic column is an HP-Innowax elastic quartz capillary column with a specification of 30 m×0.25 mm×0.25 μm ; the inlet temperature is 250° C.; the split ratio is 20:1; The temperature was kept at 50°C for 1 min, then increased to 100°C at 10°C/min, then increased to 210°C at 5°C/min, then increased to 240°C at 30°C/min, and held for 5min; the carrier gas was helium, constant flow 1.0mL/min.

In step (2), the mass spectrometry conditions are as follows: the auxiliary interface temperature is 220 °C; the ionization mode is electron bombardment source, the ionization energy is 70 eV, the ion source temperature is 230 °C, the quadrupole temperature is 150 °C, the solvent delay time is 4.0 min, and the selected ion is used. monitoring mode.

In step (2), in step (2), the method for calculating the mobility is as follows: the amount of the simulated actual suction cooling agent component measured by gas chromatography-mass spectrometry is divided by the total amount of the cooling agent component, get the mobility;

When simulating the measurement of the actual suction of the cooling agent components, every time a filter rod is purged, a new filter rod is replaced, and purging again, a total of 5 filter rods are used;

The method for detecting the total amount of the cooling agent components is as follows: use the same device, replace a new filter rod, use 185 ℃ gas to continuously purge the filter rod for 10 minutes, and then replace the new filter rod to continue purging after purging. Purge 5 filter rods to determine the total amount of cooling agent components.

The test cigarette filter rod is a medium cigarette bead filter rod with a size of 25 mm. Remove the filter rod from the cigarette and pinch the bursting beads, and put them into the purge tube.

The determination results showed that: Menthone, isopulegol and L-menthol were detected in the samples, and the total contents were 188.4, 257.8 and 208.9 μg/piece, respectively, and the simulated releases to cigarette smoke were 26.77, 33.20, and 25.18 μg/stick, and the simulated measurement results of the mobility from filter rod to cigarette smoke were 14.2%, 12.9% and 12.1%, respectively.

In addition, in order to accurately measure the total amount of cooling agent components in the filter rod, filter rods with artificially added 7 kinds of cooling agent components are prepared in the present invention, and the addition amount of the 7 kinds of components in each cigarette filter rod is 100 μg respectively. . After the filter rod was put into the purge tube, 180°C was used for continuous purging for 10 min, so that the cooling agent components in the filter rod could be completely blown out. The method of Example 3 was used to measure the total amount of cooling agent components. table 3. As can be seen from the results in Table 3, the recovery rates of the determination results of the seven cooling agents are all greater than 87.2%, indicating that the recovery rate of the total amount determination results of this method is high, and the results are reliable. At the same time, artificially prepared filter rods containing these 7 kinds of cooling agents were used to simulate real smoking and purging of cigarettes.

table 3

From the results in Table 3, it can be seen that the seven cooling agents did migrate, and the mobility was between 7.62% and 15.6%; and the mobility was directly related to the boiling point of the compound. The higher the boiling point, the lower the mobility. , indicating that adding menthone, isopulegol, L-menthol and other low-boiling components to the filter rod is beneficial to the release to the smoke.

Five parallel determinations of the migration amount were carried out on the same filter rod, and the relative standard deviation (RSD) was between 3.6 and 4.3%, indicating that the method has good reproducibility and can satisfy the accurate determination of the migration amount of the filter rod added with cooling agent. requirements. Because the migratory cooling agent components in the cigarette filter rods are likely to enter the human mouth and be felt by the smoker's taste, the method of the present invention can accurately measure the migration rate of the cooling flavor components added in the cigarette filter rods to the cigarette smoke. , so as to determine the release amount and release rule of the added cooling flavor components. The determination results of this method can effectively guide the addition amount and addition ratio of cooling flavor in different types of cigarette filter rods, and can effectively control the cooling flavor of cigarette filter rods. Make an objective evaluation of the actual effect.

The foregoing has shown and described the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above-mentioned embodiments. The above-mentioned embodiments and descriptions only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Various changes and modifications fall within the scope of the claimed invention. The claimed scope of the present invention is defined by the appended claims and their equivalents.

Claims (10)

1. A simulation determination method for migration of cooling agent components in a cigarette filter stick to cigarette smoke is characterized by comprising the following steps:

the device comprises an airflow preheating cavity, a numerical control three-way valve, a purging pipe and a dynamic headspace gas chromatography-mass spectrometry instrument;

the numerical control three-way valve is arranged between the airflow preheating cavity and the purging pipe;

the gas outlet of the purging pipe is connected with a dynamic headspace gas chromatography-mass spectrometry instrument;

the airflow preheating cavity is connected with an air inlet of the numerical control three-way valve;

the method comprises the following steps:

step (1), purging with gas flow: putting the filter stick into a purging pipe, starting a heating program of the airflow preheating cavity to heat, and enabling the temperature of the purging airflow at each opening to be consistent with the temperature of the filter stick which is actually sucked and circulated by the cigarette on the smoking machine; after the temperature rise program is adjusted, switching is carried out through a three-way valve, the smoking machine is simulated to suck and blow the filter rods, air flow enters a blowing pipe to pass through the filter rods during simulated sucking, and the air flow directly enters the atmosphere during simulated static combustion; meanwhile, the actual number of suction openings of the cigarette is simulated;

step (2), trapping by an adsorption trap, thermal desorption sample injection and gas chromatography-mass spectrometry analysis: the gas passing through the filter stick enters a trap of a dynamic headspace gas chromatography-mass spectrometry instrument for trapping, after trapping is finished, the cooling agent components adsorbed in the trap are desorbed through high-temperature analysis, then the gas enters the gas chromatography-mass spectrometry instrument for detection, and the mobility is calculated;

the cooling agent comprises menthone, isopulegol, L-menthol, 2-isopropyl-N, 2, 3-trimethylbutanamide, menthyl lactate, N-ethyl-p-menthyl-3-carboxamide and menthone glycerol ketal.

2. The method for simulated measurement of the migration of cooling agent components in a cigarette filter stick to cigarette smoke according to claim 1, wherein the airflow preheating chamber is a quartz glass tube, and infrared radiation is used for preheating gas in the tube.

3. The method for the simulated determination of the migration of cooling agent components in a cigarette filter stick to cigarette smoke according to claim 1, wherein the purging tube comprises a tube body and a tube cap; the pipe body is connected with the pipe cap; two sealing rings which are used for fixing the filter stick and only allow airflow to pass through from the filter tip are arranged in the tube body, and the two sealing rings are respectively arranged at two ends of the filter stick.

4. The method for simulated determination of migration of cooling agent components in a cigarette filter stick to cigarette smoke according to claim 1, wherein in step (1), the filter stick is purged by simulating an ISO standard suction mode, purging is continued for 2 seconds every 1 minute, and the flow rate of purge gas flow is 17.5 mL/min; the Canadian deep suction mode is simulated to purge the filter stick, the purging lasts for 2 seconds every 30 minutes, and the flow rate of the purging airflow is 22.5 mL/min; purging for 8-10 times.

5. The method for simulated measurement of the migration of cooling agent components in the cigarette filter stick to the cigarette smoke according to claim 1, wherein in the step (2), the adsorption material of the trap is polybutadiene coated silica gel particles, the temperature of the trap is-10 ℃, the high-temperature desorption temperature is 180 ℃ minus 240 ℃, the desorption time is 2-5min, the transmission line temperature is 220 ℃ minus 260 ℃, and the valve box temperature is 220 ℃ minus 260 ℃.

6. The method for simulated measurement of migration of cooling agent components in the cigarette filter stick to cigarette smoke according to claim 5, wherein the preparation method of the polybutadiene coated silica gel particles is as follows:

adding polybutadiene, a sensitizer and toluene into a beaker, uniformly mixing, adding silica gel particles modified by triethoxyvinylsilane, carrying out ultrasonic oscillation reaction, carrying out rotary evaporation to remove toluene after the reaction is finished, introducing argon into a container filled with a product, carrying out radiation crosslinking after sealing, washing with benzene and acetone in sequence, and drying to obtain the modified silica gel particles;

the mass ratio of polybutadiene to the sensitizer to the triethoxy vinyl silane modified silica gel particles is 12-15: 1.0-1.5: 120 to 150 parts;

the mass ratio of polybutadiene to the volume of toluene is 12-15 g: 0.8-1.2L.

7. The simulated measurement method for migration of cooling agent components in the cigarette filter stick to cigarette smoke according to claim 6, wherein the particle size of silica gel particles is 100-150 meshes; the drying temperature is 200 ℃, and the drying time is 6 h; the ultrasonic oscillation time is 35-45 min; the mass of benzene and acetone used for washing is 2-3 times that of the triethoxyvinylsilane modified silica gel particles; the sensitizer is ethylene glycol dimethacrylate or triethylene glycol dimethacrylate.

8. The method for simulated measurement of the migration of cooling agent components in a cigarette filter stick to cigarette smoke according to claim 1, wherein in the step (2), the gas chromatography conditions are as follows: the chromatographic column is HP-Innowax elastic quartz capillary column with specification of 30 m × 0.25mm × 0.25μm; the temperature of a sample inlet is 250 ℃; the split ratio is 20: 1; keeping the initial temperature of the column box at 50 ℃ for 1 min, then increasing the temperature to 100 ℃ at 10 ℃/min, then increasing the temperature to 210 ℃ at 5 ℃/min, then increasing the temperature to 240 ℃ at 30 ℃/min, and keeping the temperature for 5 min; the carrier gas was helium with a constant flow of 1.0 mL/min.

9. The method for simulated determination of migration of cooling agent components in a cigarette filter stick to cigarette smoke according to claim 1, wherein in step (2), mass spectrometry conditions are as follows: the temperature of the auxiliary interface is 220 ℃; the ionization mode is an electron bombardment source, the ionization energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, the solvent delay time is 4.0 min, and a selective ion monitoring mode is adopted.

10. The method for simulated measurement of the migration of cooling agent components in a cigarette filter stick to cigarette smoke according to claim 1, wherein in the step (2), the method for calculating the migration rate comprises the following steps: the amount of the simulated actual sucked cooling agent component measured by a gas chromatography-mass spectrometer is divided by the total amount of the cooling agent component to obtain the mobility;

when the measurement of the components of the actually sucked cooling agent is simulated, each filter stick is replaced by a new filter stick after being blown, the filter sticks are blown again, and not less than 5 filter sticks are used in total;

the method for detecting the total amount of the cooling agent components comprises the following steps: and (3) replacing a new filter stick by adopting the same device, continuously purging the filter stick for 8-15 min by using 180-plus-240 ℃ gas, continuously purging by replacing the new filter stick again after purging is finished, purging not less than 5 filter sticks totally, and measuring the total amount of the components of the cooling agent.

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