Preparation method and application of a post-nasal smoke adsorption material

Abstract

The application provides a preparation method of a post-nasal smoke adsorbing material, which comprises the following steps: taking 1,3,5-triformylbenzene, 1,4-diaminobenzene and ethylenediamine, adding them into dimethyl sulfoxide, and stirring them uniformly; slowly adding an aqueous acetic acid solution, stirring and reacting for 2 hours under the protection of nitrogen at 50 DEG C, adding 1-10 mg of graphene oxide, stirring uniformly, and obtaining a reaction solution; adding the reaction solution into a Pyrex tube, freezing and degassing the reaction solution for three times through a liquid nitrogen bath, sealing the Pyrex tube, and reacting for 48 hours at 150 DEG C; after the reaction is completed, centrifugal filtration is performed to take out the precipitate, the precipitate is washed with chloroform and ethanol for three times, the obtained powder is vacuum dried at 100 DEG C for 12 hours, and the adsorbing material powder is obtained. The post-nasal smoke adsorbing material obtained by the application can better adsorb post-nasal smoke, and especially has a good adsorbing effect on components with low polarity in the smoke.

Description

Technical Field

[0001] The present invention relates to the field of adsorption material preparation, and in particular to a preparation method and application of a postnasal smoke adsorption material. Background Art

[0002] Aroma is one of the most important sensory qualities of food and determines consumer acceptance. Aroma perception is the sum of the chemical stimulation, physiological reaction, and psychological effect of aroma compounds on humans, and is the result of the interaction between humans and food. Aroma perception includes two independent pathways: the anterior nasal cavity and the posterior nasal cavity. The anterior nasal cavity pathway refers to the perception of aroma in the environment through the nostrils, providing early warning signals of the external environment and information on the edibility of food. The posterior nasal cavity pathway emphasizes the perception of food aroma during the chewing process (oral processing), providing information on food acceptance and sensory enjoyment, and also reflects human behavioral characteristics.

[0003] For cigarettes, anterior nasal aroma primarily consists of the olfactory aroma and sidestream aroma of the cigarette. Retronasal aroma, the aroma perceived through the posterior nasal cavity during smoking, is the primary influence on the aroma and taste of cigarettes. Therefore, retronasal smoke testing can accurately reflect the aroma and taste of cigarettes. Currently, cigarette smoke analysis primarily relies on the standard smoking machine-Cambridge filter capture method, which exhibits significant differences in exposure patterns compared to actual exposures. Currently, no suitable adsorption capture and analysis method for retronasal smoke has been developed.

[0004] In order to solve the above problems, the present invention is proposed. Summary of the Invention

[0005] The purpose of the present invention is achieved through the following technical solutions.

[0006] A first aspect of the present invention provides a method for preparing a postnasal smoke adsorbent material, comprising the following steps:

[0007] Step (1): Take 1,3,5-trimethylbenzene, 1,4-diaminobenzene and ethylenediamine, add them into dimethyl sulfoxide, and stir evenly;

[0008] Step (2): slowly add acetic acid aqueous solution, under nitrogen protection, at 50° C., stir and react for 2 h, add 1-10 mg of graphene oxide, stir evenly to obtain a reaction solution;

[0009] Step (3): The reaction solution of step (2) was added to a Pyrex tube, frozen and degassed three times in a liquid nitrogen bath, and the Pyrex tube was sealed and reacted at 150°C for 48 hours. After the reaction was completed, the precipitate was removed by centrifugation and washed three times with chloroform and ethanol. The obtained powder was vacuum dried at 100°C for 12 hours to obtain adsorption material powder.

[0010] Preferably, in step (1), the molar ratio of 1,3,5-trimethylbenzene, 1,4-diaminobenzene and ethylenediamine is 1:(1.25-1.45):(0.05-0.25).

[0011] Preferably, the volume of dimethyl sulfoxide in step (1) is 100-200 ml.

[0012] Preferably, the concentration of the acetic acid aqueous solution in step (2) is 1-3 mol / L;

[0013] The second aspect of the present invention provides an application of an adsorption material prepared by the preparation method described in the first aspect for postnasal smoke analysis and detection.

[0014] Preferably, the obtained adsorption material powder is added to the purge and capture tube of a portable postnasal smoke capture device to a height of 1-5 cm for postnasal smoke adsorption. After the adsorption is completed, it is taken out and directly subjected to purge and capture-GCMS analysis at 100-300°C, or analyzed and detected after elution with ether or n-hexane.

[0015] Preferably, the portable postnasal smoke capture device comprises the following components:

[0016] Nasal mask (1), drying tube (2), trap (3), buffer bottle (4), pump (5);

[0017] The trap (3) comprises: a condenser (31), a purge trap (32), a connecting pipe III (34), a fixed rubber plug I (37) and a fixed rubber plug II (38).

[0018] Preferably, the nasal mask (1) and the drying tube (2) are connected via a connecting tube I (11).

[0019] Preferably, the drying tube (2) has an inner diameter of 0.3 cm to 2 cm and a height of 3 cm to 6 cm.

[0020] Preferably, a drying tube additive (21) is added into the drying tube (2), and the height of the drying tube additive (21) added into the drying tube (2) is 2 cm to 5 cm.

[0021] Preferably, a drying tube partition (22) is provided at the bottom of the drying tube (2), and the drying tube partition (22) is a sand core partition with a thickness of 2 mm and a micropore diameter of 80-120 microns.

[0022] Preferably, the drying tube (2) and the trap (3) are connected via a connecting tube II (23).

[0023] Preferably, the condenser (31) can be a reflux condenser or a straight condenser with a length of 15 cm to 30 cm and an inner diameter greater than 0.5 cm.

[0024] Preferably, the purge collection tube (32) is filled with 1-5 cm of adsorption material.

[0025] Preferably, the buffer bottle (4) has two openings, one opening is sealedly connected to the connecting pipe III (34) through a sealing plug (42), and the other opening is connected to the pump through a connecting pipe IV (41).

[0026] Preferably, the pump (5) can generate a negative pressure of 500-10 kPa at the nasal mask (1) after being connected and turned on.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] 1. The present invention prepares an adsorption material for postnasal smoke for the first time and applies it to the analysis and detection of postnasal smoke.

[0029] 2. The postnasal smoke adsorption material obtained by the present invention can effectively adsorb postnasal smoke, especially has a good adsorption effect on low-polarity components in the smoke. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 Schematic diagram of the synthesis of Example 1;

[0031] Figure 2 It is a portable post-nasal smoke capture device;

[0032] (1) Nose mask; (11) Connecting tube I; (2) Drying tube; (21) Drying tube additive; (22) Drying tube partition; (23) Connecting tube II; (31) Condenser tube; (32) Purge and collection tube; (34) Connecting tube III; (37) Fixed rubber plug I; (38) Fixed rubber plug II; (42) Sealing plug; (4) Buffer bottle; (41) Connecting tube IV; (5) Pump connection. DETAILED DESCRIPTION

[0033] The present invention is described below with reference to specific examples, but the embodiments of the present invention are not limited thereto. Experimental methods where specific conditions are not specified in the examples are generally based on conventional conditions and those described in the manual, or according to the conditions recommended by the manufacturer. The general equipment, materials, and reagents used are all commercially available unless otherwise specified.

[0034] Example 1

[0035] 2mmol of 1,3,5-trimethylbenzene, 2.7mmol of 1,4-diaminobenzene and 0.3mmol of ethylenediamine were added to dimethyl sulfoxide and stirred evenly. Then 60ml of 3mol / L acetic acid aqueous solution was slowly added. Under nitrogen protection, the reaction was stirred at 50°C for 2h. Then 6mg of graphene oxide was added and stirred evenly. The reaction solution was then added to a Pyrex tube, frozen and degassed three times in a liquid nitrogen bath. After the Pyrex tube was sealed, the reaction was carried out at 150°C for 48h. After the reaction was completed, the precipitate was removed by centrifugation and washed three times with chloroform and ethanol. The obtained powder was vacuum dried at 100°C for 12h to obtain the desired adsorption material powder. The synthesis schematic is shown as follows: Figure 1 shown.

[0036] Surface data of the samples were measured using a physical adsorption instrument using nitrogen adsorption at 77 K. The specific surface area was calculated using the BET model, and the pore size distribution was obtained using the BJH model. The data are shown in Table 1. As can be seen from the table, the adsorbent material of the present invention has a large specific surface area and nanometer-scale pore diameters, demonstrating excellent adsorption performance.

[0037] Table 1 BET specific surface area and pore size data of adsorption materials

[0038]

[0039] The resulting adsorbent material powder is added to a portable post-nasal smoke capture device such as Figure 2 In the purge collection tube (32) shown, a height of 3 cm was added to conduct the post-nasal smoke adsorption experiment.

[0040] Brand A cigarettes were selected as test cigarettes. After lighting the cigarettes, the tester took a puff and quickly covered their nose with a retronasal capture device. After the retronasal smoke was completely exhaled, they took a second puff, and this cycle repeated. Seven puffs were taken evenly from each cigarette, and groups of four were puffed. After adsorption was complete, the samples were removed, eluted with n-hexane (containing an internal standard), and analyzed by GC-MS. The results are shown in Table 2.

[0041] Comparative Example 1

[0042] Silica gel with a particle size of 40-75 μm was selected to replace the adsorption material in Example 1, and other conditions remained unchanged. The results of GC-MS analysis are shown in Table 2.

[0043] Table 2 GC-MS data of different adsorption materials

[0044]

[0045]

[0046] As shown in Table 2, the adsorption material used in the example detected 29 postnasal smoke components with a total detection concentration of 183.48 mg / stick. The corresponding silica gel adsorption material used in the control example detected 17 postnasal smoke components with a total detection concentration of 47.43 mg / stick. The adsorption capacity and adsorption strength were significantly weaker than those of the adsorption material of the present invention, further confirming the superiority of the method of the present invention.

Claims

1. A method for preparing a postnasal smoke adsorbent material, characterized in that: It includes the following steps: Step (1): Take 1,3,5-trimethylbenzene, 1,4-diaminobenzene and ethylenediamine, add them into dimethyl sulfoxide, and stir evenly; Step (2): slowly add acetic acid aqueous solution, under nitrogen protection, at 50°C, stir and react for 2 hours, add 1-10 mg of graphene oxide, stir evenly, and obtain a reaction solution; Step (3): The reaction solution of step (2) was added to a Pyrex tube, frozen and degassed three times in a liquid nitrogen bath, the Pyrex tube was sealed, and the reaction was carried out at 150°C for 48 hours. After the reaction was completed, the precipitate was removed by centrifugal filtration, washed three times with chloroform and ethanol, and the obtained powder was vacuum dried at 100°C for 12 hours to obtain an adsorption material powder; Wherein, the molar ratio of 1,3,5-trimethylbenzene, 1,4-diaminobenzene and ethylenediamine in step (1) is 1:(1.25~1.45):(0.05~0.25).

2. The preparation method according to claim 1, characterized in that The volume of dimethyl sulfoxide in step (1) is 100-200 ml.

3. The preparation method according to claim 1, characterized in that The concentration of the acetic acid aqueous solution in step (2) is 1-3 mol / L.

4. Use of the adsorbent material prepared by the preparation method of the postnasal smoke adsorbent material according to claim 1 for postnasal smoke analysis and detection.

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