Method for detecting and analyzing flavor substances of heated cigarettes

Abstract

The invention discloses a method for detecting and analyzing flavor substances of a heated cigarette. The method comprises the following steps: (1) trapping smoke generated after the heated cigarette is smoked through a Cambridge filter to obtain trapped smoke; (2) putting a Cambridge filter into the mixed solution, carrying out ultrasonic extraction, adding ultrapure water, washing for 4-8 minutes, and separating, dewatering and concentrating to obtain a particulate matter concentrated solution; (3) enabling the trapped flue gas to pass through a peristaltic pump, enabling the trapped flue gas to pass through a gas washing bottle with a mixed solution, and then concentrating a solution in the gas washing bottle to obtain a gas-phase substance concentrated solution; (4) respectively detecting the particle-phase substance concentrated solution and the gas-phase substance concentrated solution through GC / MS (Gas Chromatography / Mass Spectrometry) to determine a target flavor substance; and (5) mixing the particle-phase substance concentrated solution and the gas-phase substance concentrated solution, passing through a gas chromatograph, and carrying out quantitative detection. According to the method, quantitative analysis can be carried out on the smoke, particles captured by the smoke can be extracted to the maximum extent, the loss rate of the particles is increased, and the content of target flavor substances in the smoke is determined.

Description

Technical Field

[0001] The invention belongs to the technical field of methods for detecting aroma substances in heated cigarettes, and in particular relates to a method for detecting and analyzing aroma substances in heated cigarettes. Background Art

[0002] As the public pays more attention to health management, the development of traditional cigarettes is increasingly restricted, while new tobacco products represented by heated cigarettes and electronic cigarettes are showing a rapid growth trend, among which heated cigarettes are increasingly valued by the tobacco industry.

[0003] Compared with traditional cigarettes, a significant feature of heated cigarettes is that the generation of harmful substances is greatly reduced. However, the characteristics of heated cigarette raw materials and heating methods determine that their smoke generation and aroma substance decomposition and release mechanisms are significantly different from traditional cigarettes, which often result in insufficient aroma substances and smoke production, poor aroma quality, and other shortcomings. Flavor substances are an important part of traditional cigarettes. When traditional cigarettes are burned and smoked, most substances in tobacco are decomposed at 600C-900℃, and complex chemical reactions occur. Flavor substances can be well generated and released, but the heating temperature of heated cigarettes is 200℃-400℃, which causes most substances to be unable to be completely decomposed, and the aroma substances are greatly reduced, especially the generation and release of important aroma substances in traditional cigarette smoke are significantly reduced, which ultimately leads to the aroma substances in the smoking process being different from traditional cigarettes. The amount of aroma and smoke in the smoke decreases with the increase in the number of puffs, and it is difficult to achieve the satisfaction brought by traditional cigarettes. Therefore, a method for detecting aroma substances in heated cigarette smoke is needed to facilitate the subsequent research and development of heated cigarettes. Summary of the invention

[0004] The purpose of the present invention is to provide a method for detecting and analyzing aroma substances in heated cigarettes.

[0005] To achieve the above object, the present invention adopts the following technical solution:

[0006] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0007] (1) passing smoke from the heated cigarette through a Cambridge filter to capture the captured smoke;

[0008] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 25-40 minutes to obtain an extract, then adding ultrapure water, washing for 4-8 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution consists of dichloromethane and phenylethyl acetate solution; the volume of the dichloromethane and phenylethyl acetate solution is (30-45):1; the content of phenylethyl acetate in the phenylethyl acetate solution is 60 μg / ml;

[0009] (3) The captured flue gas is passed through a peristaltic pump at a constant speed of 20-25 ml / min through a gas washing bottle containing a mixed solution, and then the solution in the gas washing bottle is concentrated to obtain a gas phase substance concentrated solution;

[0010] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0011] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0012] Preferably, in step (1), the heated cigarette is smoked using the Canadian intensive smoking mode (HCl) standard, and an SM450 NGP linear smoking machine is used for smoking.

[0013] Preferably, the suction parameters are: suction volume 55 ml, duration 3 s, suction interval 30 s, and 12 puffs.

[0014] Preferably, the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter uses 10-15ml of the mixed solution, the diameter of the Cambridge filter is 44mm; and the ultrasonic extraction time is 25min.

[0015] Preferably, in step (3), the solution in the scrubbing bottle consists of dichloromethane and phenylethyl acetate solution, and the volume ratio of dichloromethane to phenylethyl acetate solution is 30:1.

[0016] Preferably, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0017] Preferably, the chromatographic column heating condition is as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0018] Preferably, the mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250°C, transfer line temperature 290°C, full scan mode scanning, scan range 30m / z-500m / z, solvent delay 3min.

[0019] Preferably, in step (4), the target aroma substance is benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate, pyrrole ...ol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2-methylpyrazol, 2- One or more of vanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenol ketone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone, and 4-cyclopentene-1,3-dione.

[0020] Preferably, the target aroma substance standard solutions of different concentrations in the step (4) are prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions respectively, and store them in a refrigerator at 4°C.

[0021] The method of the present invention adopts an ultrasonic extraction method, which can extract the particles captured by the smoke to the greatest extent, thereby improving the loss rate of the particles; the target aroma substance is determined by detection, and then a quantitative analysis is performed through a standard product of the target aroma substance, thereby clarifying the content of the target aroma substance in the smoke, and providing a basis for the subsequent development and addition of flavors and fragrances in heated cigarettes. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The accompanying drawings described below are some embodiments of the present invention, rather than all embodiments. For those skilled in the art, other accompanying drawings can be obtained based on these accompanying drawings without creative work.

[0023] Figure 1 is the chromatogram of the target aroma standard solution;

[0024] In the figure, 1, acetoin; 2, methyl pyruvate; 3, pyridine; 4, pyrrole; 5, cyclopentanone; 6, butyl acetate / ethyl lactate; 7, dimethylpyrazine; 8, furfural; 9, isovaleric acid; 10, 4-cyclopentane-1,3-dione; 11, 2-acetylfuran; 12, 5-methylfurfural; 13, phenol; 14, 1,2-cyclohexanedione; 15, N-methyl-2-pyrrolecarboxaldehyde; 16, limonene; 17, methylcyclopentenolone; 18, benzyl alcohol; 19, acetophenone; 20, furanone; 21, tea ketone; 22, menthol; 23, benzoic acid; 24, 5-hydroxymethylfurfural; 25 , dextrorotatory carvone; 26, phenylethyl acetate; 27, indole; 28, resorcinol; 29, 4-vinylguaiacol; 30, coconut aldehyde; 31, methyl cinnamate; 32, vanillin; 33, isovanillin; 34, β-ionone; 35, nerolidol; 36, lauric acid; 37, phyton; 38, farnesol; 39, tetradecanoic acid; 40, (5E,9E)-6,10,14-dimethylpentadeca-5,9,13-trien-2-one; 41, methyl palmitate; 42, benzyl cinnamate; 43, geranylgeraniol; 44, acetylcitrate tributyl ester; 45, cinnamic cinnamate. DETAILED DESCRIPTION

[0025] In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the specific implementation methods of the present invention will be described below with reference to the accompanying drawings. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings and other implementation methods can be obtained based on these drawings without creative work. In addition, the design orientation only represents the relative position relationship between the components, not the absolute position relationship.

[0026] In the following examples, the target aroma substance standards were purchased from Shanghai MacLean Biochemical Technology Co., Ltd.; the heated cigarettes were provided by Henan China Tobacco Industrial Co., Ltd., and the internal standard was phenylethyl acetate.

[0027] Example 1

[0028] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0029] (1) The smoke from the heated cigarette was passed through a Cambridge filter to obtain captured smoke; the heated cigarette was smoked using the Canadian deep smoking mode (HCl) standard and an SM450 NGP linear smoking machine; the smoking parameters were a puff volume of 55 ml, a puff duration of 3 s, a puff interval of 30 s, and 12 puffs;

[0030] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 25 minutes to obtain an extract, then adding ultrapure water, washing for 4 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution is composed of dichloromethane and ethyl acetate solution; the volume of the dichloromethane and ethyl acetate solution is 30:1; the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter disc uses 10ml of the mixed solution, and the diameter of the Cambridge filter disc is 44mm;

[0031] (3) The captured flue gas is passed through a peristaltic pump at a constant speed of 20 ml / min through a gas washing bottle, and then the solution in the gas washing bottle is concentrated to obtain a gas phase substance concentrate; the solution in the gas washing bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume of dichloromethane and phenylethyl acetate solution is 30:1.

[0032] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0033] The target aroma substance standard solutions of different concentrations were prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions, respectively, and store them in a refrigerator at 4°C;

[0034] The target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate, pyrrole, isovanillin Aldehyde, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone, 4-cyclopentene-1,3-dione;

[0035] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0036] In the above method, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0037] The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0038] The mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scan range 30 m / z-500 m / z, solvent delay 3 min.

[0039] Example 2

[0040] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0041] (1) passing smoke from the heated cigarette through a Cambridge filter to capture the captured smoke;

[0042] The heated cigarettes were smoked using the Canadian deep smoking mode (HCl) standard using an SM450 NGP linear smoking machine; the smoking parameters were 55 ml of puff volume, 3 s of duration, 30 s of puff interval, and 12 puffs;

[0043] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 30 minutes to obtain an extract, then adding ultrapure water, washing for 8 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution is composed of dichloromethane and ethyl acetate solution; the volume of the dichloromethane and ethyl acetate solution is 45:1; the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter disc uses 15ml of the mixed solution, and the diameter of the Cambridge filter disc is 44mm;

[0044] (3) The captured flue gas is passed through a scrubbing bottle at a constant speed of 25 ml / min by a peristaltic pump, and then the solution in the scrubbing bottle is concentrated to obtain a gas phase substance concentrate; the solution in the scrubbing bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume ratio of dichloromethane to phenylethyl acetate solution is 30:1.

[0045] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0046] The target aroma substance standard solutions of different concentrations were prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions, respectively, and store them in a refrigerator at 4°C;

[0047] The target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate , pyrrole, isovanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone,

[0048] 4-Cyclopentene-1,3-dione;

[0049] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0050] In the above method, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0051] The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0052] The mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scan range 30 m / z-500 m / z, solvent delay 3 min.

[0053] Example 3

[0054] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0055] (1) The smoke from the heated cigarette was passed through a Cambridge filter to obtain captured smoke; the heated cigarette was smoked using the Canadian deep smoking mode (HCl) standard and an SM450 NGP linear smoking machine; the smoking parameters were a puff volume of 55 ml, a duration of 3 s, a puff interval of 30 s, and 12 puffs;

[0056] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 35 minutes to obtain an extract, then adding ultrapure water, washing for 5 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution is composed of dichloromethane and ethyl acetate solution; the volume of the dichloromethane and ethyl acetate solution is 35:1; the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter disc uses 12ml of the mixed solution, and the diameter of the Cambridge filter disc is 44mm;

[0057] (3) The captured flue gas is passed through a peristaltic pump at a constant speed of 22 ml / min through a gas washing bottle, and then the solution in the gas washing bottle is concentrated to obtain a gas phase substance concentrate; the solution in the gas washing bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume of dichloromethane and phenylethyl acetate solution is 30:1.

[0058] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0059] The target aroma substance standard solutions of different concentrations were prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions, respectively, and store them in a refrigerator at 4°C;

[0060] The target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate , pyrrole, isovanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone,

[0061] 4-Cyclopentene-1,3-dione;

[0062] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0063] In the above method, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0064] The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0065] The mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scan range 30 m / z-500 m / z, solvent delay 3 min.

[0066] Example 4

[0067] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0068] (1) The smoke from the heated cigarette was passed through a Cambridge filter to obtain captured smoke; the heated cigarette was smoked using the Canadian deep smoking mode (HCl) standard and an SM450 NGP linear smoking machine; the smoking parameters were a puff volume of 55 ml, a duration of 3 s, a puff interval of 30 s, and 12 puffs;

[0069] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 40 minutes to obtain an extract, then adding ultrapure water, washing for 6 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution is composed of dichloromethane and ethyl acetate solution; the volume of the dichloromethane and ethyl acetate solution is 40:1; the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter disc uses 11ml of the mixed solution, and the diameter of the Cambridge filter disc is 44mm;

[0070] (3) The captured flue gas is passed through a gas washing bottle at a constant speed of 21 ml / min by a peristaltic pump, and then the solution in the gas washing bottle is concentrated to obtain a gas phase substance concentrate; the solution in the gas washing bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume ratio of dichloromethane to phenylethyl acetate solution is 30:1.

[0071] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0072] The target aroma substance standard solutions of different concentrations were prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions, respectively, and store them in a refrigerator at 4°C;

[0073] The target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate , pyrrole, isovanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone,

[0074] 4-Cyclopentene-1,3-dione;

[0075] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0076] In the above method, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0077] The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0078] The mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scan range 30 m / z-500 m / z, solvent delay 3 min.

[0079] Example 5

[0080] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0081] (1) passing smoke from the heated cigarette through a Cambridge filter to capture the captured smoke;

[0082] The heated cigarettes were smoked using the Canadian deep smoking mode (HCl) standard using an SM450 NGP linear smoking machine; the smoking parameters were 55 ml of puff volume, 3 s of duration, 30 s of puff interval, and 12 puffs;

[0083] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 28 minutes to obtain an extract, then adding ultrapure water, washing for 7 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution is composed of dichloromethane and ethyl acetate solution; the volume of the dichloromethane and ethyl acetate solution is 33:1; the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter disc uses 13ml of the mixed solution, and the diameter of the Cambridge filter disc is 44mm;

[0084] (3) The captured flue gas is passed through a scrubber bottle at a constant speed of 23 ml / min through a peristaltic pump, and then the solution in the scrubber bottle is concentrated to obtain a gas phase substance concentrate; the solution in the scrubber bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume ratio of dichloromethane to phenylethyl acetate solution is 30:1.

[0085] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0086] The target aroma substance standard solutions of different concentrations were prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions, respectively, and store them in a refrigerator at 4°C;

[0087] The target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate , pyrrole, isovanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone,

[0088] 4-Cyclopentene-1,3-dione;

[0089] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0090] In the above method, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0091] The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0092] The mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scan range 30 m / z-500 m / z, solvent delay 3 min.

[0093] Example 6

[0094] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0095] (1) passing smoke from the heated cigarette through a Cambridge filter to capture the captured smoke;

[0096] The heated cigarettes were smoked using the Canadian deep smoking mode (HCl) standard using an SM450 NGP linear smoking machine; the smoking parameters were 55 ml of puff volume, 3 s of duration, 30 s of puff interval, and 12 puffs;

[0097] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 32 minutes to obtain an extract, then adding ultrapure water, washing for 4 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution is composed of dichloromethane and ethyl acetate solution; the volume of the dichloromethane and ethyl acetate solution is 38:1; the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter disc uses 14ml of the mixed solution, and the diameter of the Cambridge filter disc is 44mm;

[0098] (3) The captured flue gas is passed through a gas washing bottle at a constant speed of 24 ml / min by a peristaltic pump, and then the solution in the gas washing bottle is concentrated to obtain a gas phase substance concentrate; the solution in the gas washing bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume ratio of dichloromethane to phenylethyl acetate solution is 30:1.

[0099] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0100] The target aroma substance standard solutions of different concentrations were prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions, respectively, and store them in a refrigerator at 4°C;

[0101] The target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate , pyrrole, isovanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone,

[0102] 4-Cyclopentene-1,3-dione;

[0103] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0104] In the above method, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0105] The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0106] The mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scan range 30 m / z-500 m / z, solvent delay 3 min.

[0107] Example 7

[0108] A method for detecting and analyzing aroma substances in heated cigarettes, comprising the following steps:

[0109] (1) passing smoke from the heated cigarette through a Cambridge filter to capture the captured smoke;

[0110] The heated cigarettes were smoked using the Canadian deep smoking mode (HCl) standard using an SM450 NGP linear smoking machine; the smoking parameters were 55 ml of puff volume, 3 s of duration, 30 s of puff interval, and 12 puffs;

[0111] (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 37 minutes to obtain an extract, then adding ultrapure water, washing for 6 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution is composed of dichloromethane and ethyl acetate solution; the volume of the dichloromethane and ethyl acetate solution is 42:1; the parameters of the ultrasonic extraction are: ultrasonic power of 500w, ultrasonic frequency of 40KHz; each Cambridge filter disc uses 15ml of the mixed solution, and the diameter of the Cambridge filter disc is 44mm;

[0112] (3) The captured flue gas is passed through a peristaltic pump at a constant speed of 22 ml / min through a gas washing bottle, and then the solution in the gas washing bottle is concentrated to obtain a gas phase substance concentrate; the solution in the gas washing bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume ratio of dichloromethane to phenylethyl acetate solution is 30:1.

[0113] (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured;

[0114] The target aroma substance standard solutions of different concentrations were prepared by the following method: weigh the target aroma substance standard, use dichloromethane as solvent, prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml, 100.8945μg / ml mixed standard solutions, respectively, and store them in a refrigerator at 4°C;

[0115] The target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, methyl pyruvate , pyrrole, isovanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone,

[0116] 4-Cyclopentene-1,3-dione;

[0117] (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

[0118] In the above method, the chromatographic conditions are: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; carrier gas is nitrogen, flow rate 1mL / min; injection is at a split ratio of 5:1, and the injection volume is 1μL.

[0119] The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

[0120] The mass spectrometry conditions are: electron impact ionization (EI) mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scan range 30 m / z-500 m / z, solvent delay 3 min.

[0121] In the above embodiment, Figure 1 The chromatogram of the target aroma substance is shown. After the detection data of the target aroma substance standard solution with different concentrations are processed, the standard curve equation and R square are obtained, as shown in Table 1. Table 1 shows the standard curve equation and R square of the target aroma substance.

[0122]

[0123]

[0124]

[0125] According to the content of Table 1, R square is close to 1, indicating that the calculation using the equation in the table is accurate. In the standard curve equation, X represents the ratio of the concentration of the target aroma substance to the concentration of the internal standard, and Y represents the ratio of the peak area of ​​the target substance in the sample to the peak area of ​​the internal standard.

[0126] According to the peak area of ​​the target aroma substance obtained in the example, combined with the standard curve equation, those skilled in the art can calculate the concentration of the target aroma substance and achieve quantitative analysis.

Claims

1. A method for detecting and analyzing aroma substances in heated cigarettes, characterized in that: The following steps are involved: (1) passing smoke from the heated cigarette through a Cambridge filter to capture the captured smoke; (2) placing a Cambridge filter disc into the mixed solution, ultrasonically extracting for 25-40 minutes to obtain an extract, then adding ultrapure water, washing for 4-8 minutes, separating, removing water, and concentrating to obtain a particulate matter concentrate; the mixed solution consists of dichloromethane and phenylethyl acetate solution; the volume of the dichloromethane and phenylethyl acetate solution is (30-45):1; the content of phenylethyl acetate in the phenylethyl acetate solution is 60 μg / ml; (3) The captured flue gas is passed through a peristaltic pump at a constant speed of 20-25 ml / min through a gas washing bottle containing a mixed solution, and then the solution in the gas washing bottle is concentrated to obtain a gas phase substance concentrated solution; (4) The concentrated liquid of the particulate matter and the concentrated liquid of the gaseous matter are respectively tested by GC / MS to determine the target aroma substance; after the standard solutions of the target aroma substance with different concentrations are passed through the gas chromatograph, a standard curve of the target aroma substance is configured; (5) After the particulate matter concentrate and the gaseous matter concentrate are mixed, they are passed through a gas chromatograph and compared with a standard curve of the target aroma substance for quantitative detection.

2. A method for detecting and analyzing aroma substances in heated cigarettes according to claim 1, characterized in that: In the step (1), the heated cigarette is smoked using the Canadian deep smoking mode standard and an SM450NGP linear smoking machine is used for smoking.

3. A method for detecting and analyzing aroma substances in heated cigarettes according to claim 1 or 2, characterized in that: The puffing parameters are: puffing volume 55 ml, duration 3 s, puffing interval 30 s, and 12 puffs.

4. The method for detecting and analyzing aroma substances in heated cigarettes according to claim 1, characterized in that: In step (2), the parameters of the ultrasonic extraction are: ultrasonic power is 500w, ultrasonic frequency is 40KHz; each Cambridge filter uses 10-15ml of the mixed solution, the diameter of the Cambridge filter is 44mm; and the ultrasonic extraction time is 25min.

5. The method for detecting and analyzing aroma substances in heated cigarettes according to claim 1, characterized in that: In step (3), the solution in the washing bottle is composed of dichloromethane and phenylethyl acetate solution, and the volume ratio of dichloromethane to phenylethyl acetate solution is 30:

1.

6. The method for detecting and analyzing aroma substances in heated cigarettes according to claim 1, characterized in that: The chromatographic conditions are as follows: HP-5 chromatographic column; injection port temperature 250°C; FID detector temperature 250°C; nitrogen carrier gas, flow rate 1 mL / min; injection at a split ratio of 5:1, injection volume 1 μL.

7. A method for detecting and analyzing aroma substances in heated cigarettes according to claim 6, characterized in that: The chromatographic column heating conditions are as follows: hold at 45°C for 10 min, then heat to 54°C at a rate of 2°C / min and hold for 3 min, then heat to 114°C at a rate of 3°C / min and hold for 3 min, then heat to 128°C at a rate of 2°C / min and hold for 2 min, then heat to 130°C at a rate of 2°C / min and hold for 3 min, then heat to 250°C at a rate of 10°C / min and hold for 5 min, then heat to 270°C at 20°C / min and hold for 10 min.

8. The method for detecting and analyzing aroma substances in heated cigarettes according to claim 1, characterized in that: The mass spectrometry conditions are: electron impact ionization mode, ionization voltage 70 eV, ion source temperature 250° C., transfer line temperature 290° C., full scan mode scanning, scanning range 30 m / z-500 m / z, solvent delay 3 min.

9. The method for detecting and analyzing aroma substances in heated cigarettes according to claim 1, characterized in that: In step (4), the target aroma substances are benzyl alcohol, acetophenone, furfural, cyclopentanone, pyridine, isovaleric acid, 2-methylpyrazine, farnesol, phenylethyl acetate, 4-vinylguaiacol, tea ketone, coconut aldehyde, limonene, lauric acid, nerolidol, N-methyl-2-pyrrolecarboxaldehyde, methylcyclopentenolone, cinnamic acid cinnamate benzoic acid, benzyl cinnamate, vanillin, geranylgeraniol, DL-menthol, methyl palmitate, acetone Methyl cinnamate, pyrrole, isovanillin, furanone, methyl cinnamate, 2-acetylfuran, phenol, acetoin, 5E,9E-6,10,14-trimethylpentadeca-5,9,13-triene-2-one, 5-methylfurfural, phyton, resorcinol, acetyl tributyl citrate, ethyl cyclopentenolone, 1,2-cyclohexanedione, 5-hydroxymethylfurfural, butyl acetate, ethyl lactate, dextrorotatory carvone, indole, β-ionone, One or more of 4-cyclopentene-1,3-dione.

10. The method for detecting and analyzing aroma substances in heated cigarettes according to claim 1, characterized in that: In step (4), standard solutions of target aroma substances with different concentrations are prepared by the following method: Weigh the target aroma substance standards and use dichloromethane as solvent to prepare 1.2612μg / ml, 2.5224μg / ml, 5.0447μg / ml, 10.0895μg / ml, 16.1687μg / ml, 30.2684μg / ml, 50.4473μg / ml and 100.8945μg / ml mixed standard solutions respectively and store them in a 4°C refrigerator.

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