Method for predicting nicotine release amount in tobacco smoke and tobacco heating device

Abstract

The invention relates to a method for predicting the nicotine release amount in tobacco smoke and a tobacco heating device.The total plant alkaloid content in tobacco and the adding proportion of glycerin are substituted into a nonlinear prediction equation established in advance, and the establishment method of the nonlinear prediction equation comprises the steps that tobacco raw materials are subjected to grading treatment to obtain tobacco leaves A of different grades; detecting the total plant alkaloid content in the tobacco leaves A of each grade; glycerin with different mass fractions is added into the tobacco leaves A of each grade, multiple tobacco leaves B are obtained, and the mass fraction H of glycerin in the tobacco leaves B is larger than or equal to 0; heating the tobacco leaf B to generate smoke, capturing and extracting nicotine components in the smoke, and determining and analyzing the nicotine components by adopting gas chromatography to obtain the nicotine release amount of the tobacco leaf B; and fitting the nonlinear prediction equation by taking the total plant alkaloid content and the addition proportion of glycerol as independent variables and the nicotine release amount as a dependent variable. According to the method, the numerical value of the nicotine release amount generated when other tobaccos are heated can be predicted.

Description

Technical Field

[0001] This application relates to the field of tobacco processing and analysis technology, and in particular to a method for predicting the amount of nicotine released in tobacco smoke and a tobacco heating device. Background Technology

[0002] In the production process of heated cigarettes, the amount of nicotine released directly affects the sensory quality of the product and the consumer experience. Traditional methods rely on a large number of repeated experiments and chromatographic analysis to determine the amount of nicotine released, which is not only time-consuming and labor-intensive, but also difficult to provide real-time and effective feedback for production process optimization and formula design.

[0003] Furthermore, nicotine release is a complex process influenced by multiple factors, such as the total alkaloid content of the tobacco raw material and the proportion of glycerin added during processing. However, current technologies have not effectively integrated these influencing factors, nor have they considered the complex relationship between these factors and nicotine release. This leads to a certain degree of blindness in formula design and process adjustment during product development, which not only increases trial-and-error costs but also severely restricts the precise control and efficient development of heated cigarette product quality. Summary of the Invention

[0004] Therefore, in order to predict the amount of nicotine released when tobacco is heated, and to reduce the reliance on repeated experiments in traditional detection methods and save manpower and resources, it is necessary to provide a method for predicting the amount of nicotine released in tobacco smoke and a tobacco heating device.

[0005] A method for predicting nicotine release from tobacco smoke involves substituting the total alkaloid content and glycerol addition ratio in tobacco into a pre-established nonlinear prediction equation to obtain a predicted value of nicotine release when the tobacco is heated. The method for establishing the nonlinear prediction equation includes the following steps:

[0006] Tobacco raw materials are graded according to national standards or tobacco industry standards to obtain different grades of tobacco leaves A, and the total alkaloid content of each grade of tobacco leaves A is tested.

[0007] Adding different mass fractions of glycerol to each grade of tobacco leaf A yields multiple tobacco leaves B, wherein the mass fraction H of glycerol in tobacco leaf B satisfies: H≥0;

[0008] The tobacco leaf B is heated to generate smoke, the nicotine component in the smoke is captured and extracted, and the nicotine component is measured and analyzed by gas chromatography to obtain the nicotine release amount of the tobacco leaf B.

[0009] Using the total alkaloid content and the proportion of glycerol added as independent variables, and the nicotine release amount as the dependent variable, a nonlinear prediction equation for the nicotine release amount in tobacco smoke is fitted. The expression of the nonlinear prediction equation is as follows:

[0010] ;

[0011] Where z(x, y) represents the predicted nicotine release from the tobacco raw material, x represents the proportion of glycerol added, y represents the total alkaloid content in tobacco leaf A, and k1~k 14 All represent the fitting parameters, and k1~k 14 All are real numbers.

[0012] In one embodiment, a pretreatment step is included before detecting the total alkaloid content in the tobacco leaf A. The pretreatment step is to place the tobacco leaf A under conditions of 20°C to 24°C and 50% to 70% relative humidity for 45 to 50 hours to equilibrate.

[0013] In one embodiment, when the tobacco raw material is graded, each grade of tobacco leaf A includes upper leaves, middle leaves and lower leaves.

[0014] In one embodiment, the method for preparing tobacco leaf B includes the following steps: drying the tobacco leaf A;

[0015] Glycerin is added to tobacco leaf A using a gradient method to obtain tobacco leaf B, wherein the gradient variation range is 1% and the mass fraction H is 0% to 15%;

[0016] The tobacco leaf B was placed under conditions of 28℃~32℃ and 30%~50% relative humidity for 65h~80h to equilibrate.

[0017] In one embodiment, the tobacco leaf B is heated to satisfy at least one of the following conditions:

[0018] The tobacco leaf B is ground.

[0019] The tobacco leaf B is heated in a mixed atmosphere of oxygen and nitrogen, wherein the flow rate of the mixed atmosphere is 0.1 L / min to 0.3 L / min;

[0020] The heating method is as follows: the tobacco leaf B is placed in the tobacco heating device, a mixed atmosphere is introduced into the tobacco heating device for 2 min to 4 min, and then the tobacco heating device is heated to 300℃ to 400℃ at a rate of 15℃ / s to 20℃ / s, and maintained for 4 min to 6 min.

[0021] In one embodiment, capturing and extracting nicotine from the flue gas includes the following steps:

[0022] The total particulate matter in the flue gas produced by the tobacco leaf B is captured using a Cambridge filter.

[0023] An internal standard solution and an alcohol solvent were added to the Cambridge filter, shaken, and allowed to stand to obtain an extract containing the nicotine component.

[0024] In one embodiment, the internal standard solution contains one or more of n-heptadecane, 1,5-butanediol, carvone, quinoline, 2-methylquinoline, and n-octadecane; the alcohol solvent contains isopropanol.

[0025] In one embodiment, the determination and analysis includes quantitative analysis of nicotine release in flue gas using an internal standard curve method.

[0026] In one embodiment, the gas chromatography in the gas chromatography method satisfies one or more of the following conditions:

[0027] The chromatographic column was an HP-INNOWAX capillary column with dimensions of 30m × 0.25mm × 0.25μm;

[0028] The carrier gas is helium, the carrier gas control mode is constant flow mode, and the carrier gas flow rate is 0.5 mL / min to 2 mL / min;

[0029] The injection volume is 1 μL to 2 μL;

[0030] The injection method is split injection, with a split ratio of (8-12):1; the injection port temperature is 200℃-300℃.

[0031] Heating program: Initial temperature is 100℃~120℃, hold for 3min~5min, increase to 200℃~250℃ at a rate of 10℃ / min~20℃ / min, hold for 2min~3min, detect temperature at 260℃~290℃, and tail purge flow rate is 20mL / min~30mL / min.

[0032] This application also provides a tobacco heating device for heating tobacco leaf B as described in any of the above embodiments, the tobacco heating device comprising:

[0033] The shell has an internal cavity;

[0034] A quartz tube is placed inside the cavity, and the inside of the quartz tube has a heating space for placing the tobacco leaf B. The quartz tube has an air inlet end and an air outlet end that are connected to the heating space.

[0035] The gas supply assembly is connected to the heating space through the gas inlet end and is used to add gas into the heating space.

[0036] A heating component is disposed within the cavity and located outside the quartz tube to heat the quartz tube and cause the tobacco leaf B to generate smoke.

[0037] A Cambridge filter, located at the outlet end, is used to capture the smoke produced by the tobacco leaf B.

[0038] Compared with existing technologies, the method for predicting nicotine release in tobacco smoke provided in this application establishes a nonlinear prediction equation for the total alkaloid content, glycerol content, and nicotine release in tobacco. This equation can directly predict the nicotine release that other tobacco products will produce when heated. This not only reduces the reliance on repeated experiments in traditional detection methods, saving manpower and resources, but also more accurately captures the complex nonlinear relationship between the total alkaloid content, glycerol content, and nicotine release, providing guidance for subsequent product development, process optimization, and quality control. Attached Figure Description

[0039] To more clearly illustrate the technical solutions in the embodiments of this application or the conventional technology, the drawings used in the description of the embodiments or the conventional technology will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0040] Figure 1 A flowchart of a method for predicting nicotine release in tobacco smoke according to an embodiment of this application;

[0041] Figure 2 This is a surface plot of the nicotine release from tobacco leaf B in Example 1;

[0042] Figure 3 This is a surface plot of the nicotine release from tobacco leaf B in Example 2;

[0043] Figure 4 This is a surface plot of the nicotine release from tobacco leaf B in Example 3;

[0044] Figure 5 This is a surface plot of the nicotine release from tobacco leaf B in Example 4;

[0045] Figure 6 This is a schematic diagram of the structure of a tobacco heating device according to an embodiment of this application.

[0046] Reference numerals: 1. Tobacco heating device; 101. Tobacco leaf B;

[0047] 10. Shell; 11. Cavity; 20. Quartz tube; 21. Heating space; 22. Air inlet; 23. Air outlet;

[0048] 30. Gas supply assembly; 31. Gas cylinder; 32. Mixed gas controller;

[0049] 40. Heating component; 41. Thermocouple; 42. Infrared filament;

[0050] 50. Cambridge filter; 60. Thermostat; 70. Quartz boat. Detailed Implementation

[0051] To facilitate understanding of this application, a more complete description will be provided below with reference to the accompanying drawings. Preferred embodiments of this application are shown in the drawings. However, this application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of this application.

[0052] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0053] In this application, "optionally," "optionally," and "optional" mean that something is optional, that is, it means that it is selected from either "with" or "without." If there are multiple "optional" entries in a technical solution, unless otherwise specified, and there are no contradictions or mutual constraints, each "optional" entry is independent.

[0054] In this application, terms such as "preferred," "better," "more suitable," and "ideal" are merely used to describe implementation methods or embodiments that achieve better results, and should be understood not to limit the scope of protection of this application.

[0055] The terms “having,” “containing,” “comprising,” and “including” as used in this application are synonyms and are inclusive or open-ended, not excluding additional, uncited members or features. Members or features include, for example, materials or components, structures, elements, instruments, etc.; non-limiting examples of members or features include actions, conditions under which actions occur, timing, states, etc.

[0056] In this application, the technical features or solutions described in open-ended language include both closed-ended technical features or solutions consisting of the listed contents and open-ended technical features or solutions that include the listed contents.

[0057] In this application, if the unit of a data range is only followed by the right endpoint, it means that the units of the left and right endpoints are the same.

[0058] In this application, where the method flow involves multiple steps, unless otherwise explicitly stated herein, there is no strict order restriction on the execution of these steps; they can be executed in any order other than those described. Moreover, any step may include multiple sub-steps or multiple stages, which are not necessarily completed at the same time, but can be executed at different times, and their execution order is not necessarily sequential, but can be performed alternately or simultaneously with other steps or parts of the sub-steps or stages of other steps.

[0059] In this application, the exemplary descriptions such as "in some implementations (or embodiments)" and "in one implementation (or embodiment)" may cover, but are not limited to, the following meanings: these solutions can be combined with other solutions in a suitable manner to form new technical solutions.

[0060] In this application, the terms "first aspect," "second aspect," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or quantity, nor should they be construed as implicitly indicating the importance or quantity of the indicated technical features. Moreover, "first aspect," "second aspect," etc., serve only as a non-exhaustive enumeration and should be understood not to constitute a closed limitation on quantity.

[0061] In this application, when numerical intervals (i.e., numerical ranges) are mentioned, unless otherwise specified, the distribution of selectable numerical values ​​within the numerical interval is considered continuous, and includes the two endpoints of the numerical interval (i.e., the minimum and maximum values), as well as every numerical value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that numerical interval, it includes the two endpoint integers of the numerical range, as well as every integer between the two endpoints, which is equivalent to directly listing every integer. When multiple numerical ranges are provided to describe features or characteristics, these numerical ranges can be merged. In other words, unless otherwise specified, the numerical ranges disclosed herein should be understood to include any and all subranges included therein. The "numerical value" in the numerical interval can be any quantitative value, such as a number, percentage, ratio, etc. The term "numerical interval" can be broadly included to include numerical interval types such as percentage intervals, ratio intervals, and proportion intervals.

[0062] There are no special restrictions on the source of any raw materials used in this application; they may be purchased from the market or prepared using conventional methods known to those skilled in the art.

[0063] There are no particular restrictions on the purity of any raw materials used in this application. This application preferably uses analytical grade, spectral grade, or conventional purity used in the field for detecting mainstream cigarette smoke.

[0064] Traditional methods for detecting nicotine release rely on numerous repeated experiments and multiple chromatographic analyses, which are not only time-consuming and labor-intensive, but also make it difficult to provide real-time and effective feedback for production process optimization and formulation design.

[0065] Based on this, the embodiments of this application provide at least one method for predicting the amount of nicotine released in tobacco smoke and a tobacco heating device for heating tobacco to generate smoke.

[0066] In the first aspect of this application, a method for determining the amount of nicotine released from tobacco smoke is provided. This method involves substituting the total alkaloid content and the glycerol addition ratio in tobacco into a pre-established nonlinear prediction equation to obtain a predicted value of the amount of nicotine released when tobacco is heated. (Refer to...) Figure 1 The method for establishing nonlinear prediction equations includes the following steps:

[0067] S100: Tobacco raw materials are graded according to national standards or tobacco industry standards to obtain different grades of tobacco leaves A, and the total alkaloid content in each grade of tobacco leaves A is tested.

[0068] S200: Add different mass fractions of glycerol to tobacco leaves A of each grade to obtain multiple tobacco leaves B, where the mass fraction of glycerol H in tobacco leaves B satisfies: H≥0;

[0069] S300: Heat tobacco leaf B to generate smoke, capture and extract nicotine components in the smoke, and use gas chromatography to determine and analyze the nicotine components to obtain the nicotine release amount of tobacco leaf B.

[0070] S400: Using the total alkaloid content and the proportion of added glycerol as independent variables, and nicotine release as the dependent variable, a nonlinear prediction equation for nicotine release in tobacco smoke was fitted. The expression of the nonlinear prediction equation is as follows:

[0071] ;

[0072] Where z(x, y) represents the predicted nicotine release from the tobacco raw material, x represents the proportion of glycerol added, y represents the total alkaloid content in tobacco leaf A, and k1~k 14 All represent the fitting parameters, and k1~k 14 All are real numbers.

[0073] In one embodiment, when grading the tobacco raw materials according to national standards or tobacco industry standards in step S100, national standards are preferred. For example, the tobacco raw materials are graded according to the national standard "Flue-cured Tobacco" (GB 2635-1992). Preferably, each grade of tobacco leaf A after grading includes upper leaves, middle leaves, and lower leaves; it should be explained that "upper," "middle," and "lower" here refer to the growth position of the tobacco leaves on the tobacco plant.

[0074] In one embodiment, a pretreatment step is included before detecting the total alkaloid content in tobacco leaf A. This pretreatment step involves placing tobacco leaf A at a temperature of 20°C–24°C and a relative humidity of 50%–70% for 45–50 hours to equilibrate. Non-limitingly, the temperature can be, but is not limited to, 20°C, 21°C, 22°C, 23°C, 24°C, or any value or range between two of the above; the relative humidity can be, but is not limited to, 50%, 52%, 54%, 56%, 58%, 60%, 62%, 64%, 66%, 68%, 70%, or any value or range between two of the above; and the equilibration time can be, but is not limited to, 45 hours, 46 hours, 47 hours, 48 ​​hours, 49 hours, 50 hours, or any value or range between two of the above.

[0075] It should also be noted that this application does not impose any particular restrictions on the specific method for detecting the total alkaloid content in each grade of tobacco leaf A. Any detection method known to those skilled in the art is acceptable. Those skilled in the art can select and adjust the method according to the actual measurement situation, detection requirements and detection results. This application preferably refers to the method in the national standard "Determination of Total Alkaloids in Tobacco and Tobacco Products - Continuous Flow Method" (GB / T 23356-2022) to detect the total alkaloid content in each grade of tobacco leaf A.

[0076] In one embodiment, the method for preparing tobacco leaf B includes the following steps:

[0077] S210: Dry tobacco leaves A;

[0078] S220: Glycerin is added to tobacco leaf A using a gradient method to obtain tobacco leaf B, wherein the gradient variation range is 1% and the mass fraction H is 0% to 15%;

[0079] S230: Place tobacco leaves B under conditions of 28℃~32℃ and 30%~50% relative humidity for 65h~80h to equilibrate.

[0080] In step S210, the tobacco leaves of each grade A are placed in a horizontal drying oven for drying at a temperature of 130℃ to 170℃ for a time of 4 min to 10 min. Non-limitingly, the drying temperature can be, but is not limited to, 130℃, 135℃, 140℃, 145℃, 150℃, or any value or range between two of the above; the drying time can be, but is not limited to, 4 min, 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, or any value or range between two of the above. It should also be noted that the horizontal drying oven is a conventional horizontal drying oven in the art and can be commercially available.

[0081] In step S220, it should be explained that when adding glycerol to tobacco leaf A in a gradient manner for each grade of tobacco leaf A, a maximum of 16 kinds of tobacco leaf B containing different mass fractions of H can be obtained, so as to improve the accuracy of subsequent fitting of nonlinear prediction equations.

[0082] In step S230, preferably, the tobacco leaves B are placed under conditions of a temperature of 28°C to 32°C and a relative humidity of 30% to 50% for 65 to 80 hours to re-equilibrate. Non-limitingly, the temperature can be, but is not limited to, 28°C, 29°C, 30°C, 31°C, 32°C, or any two of the above values ​​or a range thereof; the relative humidity can be, but is not limited to, 30%, 35%, 40%, 45%, 50%, or any two of the above values ​​or a range thereof; and the equilibration time can be, but is not limited to, 65 hours, 66 hours, 68 hours, 70 hours, 72 hours, 74 hours, 76 hours, 78 hours, 80 hours, or any two of the above values ​​or a range thereof.

[0083] In one embodiment, the heated tobacco leaf B satisfies at least one of the following conditions:

[0084] The tobacco leaves B are ground.

[0085] Tobacco leaf B is heated in a mixed atmosphere of oxygen and nitrogen, with a flow rate of 0.1 L / min to 0.3 L / min.

[0086] The heating method is as follows: tobacco leaf B is placed in tobacco heating device 1, a mixed atmosphere is introduced into tobacco heating device 1 for 2 min to 4 min, and then the heating device is heated to 300℃ to 400℃ at a rate of 15℃ / s to 20℃ / s and maintained for 4 min to 6 min.

[0087] Schematic illustration: The conditions for heating tobacco leaf B include: heating tobacco leaf B ground into powder; the heating atmosphere is composed of 20% oxygen and 80% nitrogen; the flow rate of the mixed atmosphere is 0.2 L / min; after introducing the mixed atmosphere into the tobacco heating device 1 for 3 minutes, the heating device is heated to 350°C at a rate of 18°C / s and maintained for 5 minutes to generate smoke from tobacco leaf B. Furthermore, it should be noted that after the smoke collection is complete, under the condition of continuous introduction of the mixed atmosphere, new tobacco leaf B is used for heating only after the tobacco heating device 1 cools down to a certain temperature.

[0088] In one embodiment, capturing and extracting nicotine from flue gas includes the following steps:

[0089] S310: Uses Cambridge filters to capture total particulate matter in the flue gas produced from tobacco leaf B;

[0090] S320: Add internal standard solution and alcohol solvent to Cambridge filter, shake and let stand to obtain an extract containing nicotine.

[0091] In step S310, this application does not impose any special restrictions on the specifications of the Cambridge filter; any Cambridge filter well-known to those skilled in the art can be used. Similarly, there are no restrictions on the method for capturing tobacco leaf B using the Cambridge filter; any method well-known to those skilled in the art can be used. It should also be noted that in this embodiment, the tobacco heating device 1 of this application is used to capture tobacco leaf B 101. The tobacco heating device 1 of this application includes at least a quartz tube 20 with an internal heating space 21 for placing tobacco leaf B 101, an air supply component 30 connected to the heating space 21 through the air inlet end 22 of the quartz tube 20, and a Cambridge filter 50 disposed at the air outlet end 23 of the quartz tube 20. Since the outlet end 23, heating space 21 and inlet end 22 of the quartz tube 20 are interconnected, when the gas supply component 30 blows a mixed atmosphere into the heating space 21 inside the quartz tube 20, it can drive the smoke generated by the tobacco leaf B 101 to escape from the outlet end 23, thereby enabling the Cambridge filter 50 located at the outlet end 23 to capture the smoke generated by the tobacco leaf B 101.

[0092] In one embodiment, in step S320, the internal standard solution contains one or more of n-heptadecane, 1,5-butanediol, carvone, quinoline, 2-methylquinoline, and n-octadecane; the alcohol solvent contains isopropanol. Preferably,

[0093] An internal standard solution is obtained by dissolving the internal standard in isopropanol, with a mass concentration of 0.500 mg / mL to 4.000 mg / mL. Non-limitingly, the mass concentration of the internal standard solution can be, but is not limited to, 0.500 mg / mL, 1.000 mg / mL, 2.000 mg / mL, 3.000 mg / mL, 4.000 mg / mL, or any value or range between two of the above.

[0094] Non-limiting, in step S320, the shaking is performed on a shaker for 20 to 40 minutes at room temperature.

[0095] In one embodiment, the determination and analysis includes quantitative analysis of nicotine release in tobacco smoke using an internal standard curve method. Specifically, this method establishes a standard curve by analyzing the ratio of the chromatographic peak areas of nicotine standard working solutions of different concentrations to the corresponding standard components, thereby enabling quantitative analysis of nicotine release in tobacco smoke. For example, the limit of detection for quantitative analysis of nicotine release in tobacco smoke using the internal standard curve method is 0.0096 mg / mL, and the limit of quantification is 0.032 mg / mL.

[0096] In one embodiment, the gas chromatography in the gas chromatography method satisfies one or more of the following conditions:

[0097] The chromatographic column was an HP-INNOWAX capillary column with dimensions of 30m × 0.25mm × 0.25μm;

[0098] The carrier gas is helium, the carrier gas control mode is constant flow mode, and the carrier gas flow rate is 0.5 mL / min to 2 mL / min;

[0099] The injection volume is 1 μL to 2 μL;

[0100] The injection method is split injection, with a split ratio of (8-12):1; the injection port temperature is 200℃-300℃.

[0101] Heating program: Initial temperature is 100℃~120℃, hold for 3min~5min, increase to 200℃~250℃ at a rate of 10℃ / min~20℃ / min, hold for 2min~3min, detect temperature at 260℃~290℃, and tail purge flow rate is 20mL / min~30mL / min.

[0102] Indicatively, the conditions met by gas chromatography include: constant flow carrier gas control mode, carrier gas flow rate of 1.0 mL / min, injection volume of 1 μL, split ratio of 10:1; injection port temperature of 250 °C; and temperature program: initial temperature of 100 °C, hold for 4 min, increase to 230 °C at a rate of 15 °C / min, and hold for 2.5 min.

[0103] In some embodiments, in step S400, the total alkaloid content, the glycerol addition ratio, and the detected nicotine release amount in the corresponding tobacco leaf B are correlated. A surface plot of nicotine release in tobacco raw material smoke is plotted with the glycerol addition ratio as the independent variable x, the total alkaloid content as the independent variable y, and the nicotine release amount as the dependent variable z. A nonlinear prediction equation for nicotine release in tobacco leaf smoke is then fitted. Illustratively, multiple real numbers are substituted into the nonlinear prediction equation based on the nicotine release surface plot, and the error caused by each real number between the nonlinear prediction equation and the nicotine release surface plot is compared. The real number with the smallest error is selected as the fitting parameters k1 to k2. 14 The value of ; for multiple nonlinear prediction equations obtained simultaneously, the model determination coefficient of each nonlinear prediction equation can also be obtained simultaneously, and the equation with the model determination coefficient closest to 1 is selected as the final nonlinear prediction equation. Furthermore, the "error" is preferably expressed as the sum of squared errors or root mean square error.

[0104] The method for predicting nicotine release from tobacco smoke provided above establishes a nonlinear prediction equation for the total alkaloid content, glycerol content, and nicotine release in tobacco. This equation can directly predict the nicotine release from other tobacco products when heated. This not only reduces the reliance on repeated experiments in traditional detection methods, saving manpower and resources, but also more accurately captures the complex nonlinear relationship between the total alkaloid content, glycerol content, and nicotine release, providing guidance for subsequent product development, process optimization, and quality control.

[0105] The following are some examples.

[0106] The embodiments of this application will be described in detail below with reference to examples. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of this application. For experimental methods in the following embodiments where conditions are not specified, reference should be made to the guidelines given in this application, or to experimental manuals or conventional conditions in the art, or to the conditions recommended by the manufacturer, or to experimental methods known in the art.

[0107] In the following examples, the measurement parameters of the raw material components may have slight deviations within the weighing accuracy range unless otherwise specified. Temperature and time parameters are subject to acceptable deviations due to instrument testing accuracy or operational precision.

[0108] Example 1

[0109] 1. Materials and Methods

[0110] 1.1 Materials

[0111] The tobacco raw materials come from Fujian Province in China and are supplied by Zhejiang China Tobacco Industry Co., Ltd.

[0112] 1.2 Instruments and Reagents

[0113] Instruments: Gas chromatograph (Agilent 8890A; equipped with autosampler, column oven, thermal conductivity detector (TCD), flame ionization detector (FID), Agilent ChemStation chromatography management software, Agilent Technologies, USA); Ultrasonic cleaner (SB-3200DT, Xinzhi Biotechnology Co., Ltd.); Analytical balance (CP2245, Sartorius, Germany); Horizontal drying oven (Model 101-0AB, Hebei Feisifu Instrument Co., Ltd.); Full-temperature shaking incubator (HZQ-F160, Taicang Experimental Equipment Factory); Ultrapure water generator (ELGA / MILLTI-Q, Millipore, USA); Grinder (XL-20B, Guangzhou Xulang Machinery Equipment Co., Ltd.).

[0114] Reagents: Nicotine standard (98.2%, Beijing Beifang Weiye Metrology Technology Research Institute), isopropanol, chloroform (chromatographic grade, Dicoma Technology Co., Ltd.), nicotine, glycerol, n-heptadecane, 1,4-butanediol (98%, Bailingwei Technology Co., Ltd.)

[0115] 1.3 Preparation of Standard Solutions

[0116] Internal standard solution: Accurately weigh 0.25 g of n-heptadecane and 2.0 g of 1,5-butanediol, dissolve them in isopropanol and dilute to a volumetric flask of 500 mL to obtain the internal standard solution, wherein the concentration of n-heptadecane is 0.500 mg / mL and the concentration of 1,5-butanediol is 4.000 mg / mL.

[0117] Nicotine standard working solution: Weigh 0.02 g of nicotine standard, dissolve it in internal standard solution and dilute to volume in a 10 mL volumetric flask to obtain nicotine standard stock solution, and store at 0–4 °C. Then, gradually transfer the nicotine standard stock solution into multiple 10 mL volumetric flasks, dilute to volume with internal standard solution, and dilute stepwise to obtain nicotine standard working solutions of different concentration gradients.

[0118] 1.4 Constructing the internal standard curve

[0119] 1.4.1 Take an appropriate amount of nicotine standard working solution and filter it through a 0.45 μm filter membrane for gas chromatography analysis.

[0120] 1.4.2 The gas chromatography analysis conditions are as follows:

[0121] The chromatographic column was an HP-INNOWAX capillary column (30m × 0.25mm × 0.25μm) (Agilent Technologies, USA); the temperature program was as follows: initial temperature 100℃, hold for 4 min, increase to 230℃ at a rate of 15℃ / min, hold for 2.5 min; the injection port temperature was 250℃; the carrier gas was helium, flow rate 1.0 mL / min, constant flow mode; the air flow rate was 250 mL / min; the hydrogen flow rate was 60 mL / min; the injection volume was 1 μL; the injection method was split injection, split ratio 10:1; the FID detector temperature was 275℃; the detection temperature was 280℃, and the tail purge flow rate was 25 mL / min.

[0122] 1.5 Experimental Methods and Conditions

[0123] 1.5.1 Sample Grading

[0124] The raw tobacco leaves from Fujian Province were graded according to the national standard "Flue-cured Tobacco" (GB 2635-1992) to obtain different grades of tobacco leaves A. In this embodiment, the different grades of tobacco leaves A are upper orange-yellow grade 2, middle orange-yellow grade 3, and lower orange-yellow grade 2.

[0125] 1.5.2 Detect the total alkaloid content in tobacco leaves of each grade A.

[0126] After equilibration at 22℃ and 60% relative humidity for 48 hours, the total alkaloid content of each grade of tobacco leaf A was determined using the method in the national standard "Determination of Total Alkaloids in Tobacco and Tobacco Products - Continuous Flow Method" (GB / T 23356-2022).

[0127] 1.5.3 Preparation of Tobacco Leaf B

[0128] 1.5.3.1 Place the tobacco leaves of each grade A into a horizontal drying oven for drying at a temperature of 150℃ for 5 minutes.

[0129] 1.5.3.2: Glycerin of different mass fractions was added to each grade of tobacco leaf A using a gradient method to obtain tobacco leaf B. The gradient range was 1%, and the mass fraction H ranged from 0% to 15%. This means that each grade of tobacco leaf A yielded 16 tobacco leaves B. The leaves were then equilibrated for 72 hours in a temperature and humidity environment of 30℃ and 40% relative humidity.

[0130] 1.5.3.3: Place tobacco leaf B under conditions of 30℃ and 40% relative humidity for 72 hours to equilibrate.

[0131] 1.5.4: Heating tobacco leaf B to generate smoke, capturing and extracting nicotine components from the smoke, and using gas chromatography to determine and analyze the nicotine components to obtain the nicotine release amount of tobacco leaf B.

[0132] 1.5.4.1: Conditions for heating tobacco leaves B to produce smoke

[0133] The tobacco leaf B is ground and sieved through a 40-mesh sieve to form powdered tobacco leaf B. 0.4g of powdered tobacco leaf B is placed on a quartz boat 70 and then placed in the heating space 21 inside the quartz tube 20 of the tobacco heating device 1.

[0134] When heating powdered tobacco leaf B, the mixed atmosphere consists of 20% oxygen and 80% nitrogen at a flow rate of 0.2 L / min. After introducing the mixed atmosphere into the tobacco heating device 1 for 3 minutes, the heating device is heated to 350°C at a rate of 18°C / s and maintained for 5 minutes to generate smoke from tobacco leaf B. After the smoke from one tobacco leaf B is collected, the mixed atmosphere is continuously introduced until the tobacco heating device 1 cools down to a certain temperature before replacing it with a new tobacco leaf B for heating.

[0135] 1.5.4.2 Capture of total particulate matter in flue gas

[0136] The tobacco heating device 1 of this application is used to capture tobacco leaves B. The tobacco heating device 1 of this application includes at least a quartz tube 20 with a heating space 21 for placing tobacco leaves B, an air supply component 30 connected to the heating space 21 through the air inlet 22 of the quartz tube 20, and a Cambridge filter 50 located at the air outlet 23 of the quartz tube 20. Since the air outlet 23, the heating space 21, and the air inlet 22 of the quartz tube 20 are interconnected, when the air supply component 30 blows a mixed atmosphere into the heating space 21 inside the quartz tube 20, it can drive the smoke generated by tobacco leaves B to escape from the air outlet 23, thereby enabling the Cambridge filter 50 located at the air outlet 23 to capture the smoke generated by tobacco leaves B. It should be noted that in 1.5.4.1, after stopping the heating of the quartz tube 20, the Cambridge filter 50 should be removed after the tobacco heating device 1 drops to a certain temperature while the mixed atmosphere is continuously introduced. In other words, the Cambridge filter 50 can be removed before replacing the new tobacco leaf B.

[0137] 1.5.4.3 Sample Preparation for Nicotine Analysis in Flue Gas

[0138] Cambridge Filter 50, which captures total particulate matter from tobacco leaves of all grades B, was transferred to 50 mL Erlenmeyer flasks. 20 mL of internal standard solution was added, and the mixture was shaken on a shaker at room temperature for 30 min, allowed to stand for 5 min, and then filtered through a 0.45 μm organic filter membrane into a chromatographic bottle to obtain an extract containing nicotine. The extract was then further analyzed by gas chromatography.

[0139] The gas chromatography analysis conditions 1.5.4.4 are the same as those in 1.4.2, so they will not be repeated here.

[0140] 1.6 Fitting the nonlinear prediction equation

[0141] Using the proportion of glycerol added as the independent variable x, the total alkaloid content as the independent variable y, and the nicotine release as the dependent variable z, a surface plot of nicotine release from tobacco smoke from the Fujian production area was drawn, as follows: Figure 2 As shown, the expression for the fitted nonlinear prediction equation is as follows:

[0142] .

[0143] Where z(x,y) represents the predicted value of nicotine release from the tobacco raw material, x represents the proportion of glycerol added, and y represents the total alkaloid content in the tobacco leaf A.

[0144] 1.7 Results Evaluation

[0145] The coefficient of determination of the above nonlinear prediction equation is 0.999907, which is relatively accurate. Therefore, this nonlinear prediction equation can be used as a relatively ideal prediction equation.

[0146] Example 2

[0147] The difference between Example 2 and Example 1 lies in the source of the tobacco raw materials. In Example 2, the tobacco raw materials came from Guizhou Province in China and were provided by Zhejiang China Tobacco Industry Co., Ltd. All other conditions were exactly the same and will not be repeated here. The surface diagram of tobacco release in the smoke of tobacco leaf B obtained in this example is shown below. Figure 3 As shown, the blue dots represent the measured values ​​of nicotine release detected in step 300. The expression of the nonlinear prediction equation obtained from this is as follows:

[0148] .

[0149] The coefficient of determination of the above nonlinear prediction equation is 0.999556, which is relatively accurate. Therefore, this nonlinear prediction equation can be used as a relatively ideal prediction equation.

[0150] Example 3

[0151] The difference between Example 2 and Example 1 is that the source of the tobacco raw materials is different; the tobacco raw materials in Example 3 come from Sichuan Province, China. All other conditions are exactly the same and will not be repeated here. The surface diagram of tobacco release in the smoke of tobacco leaf B obtained in this example is shown below. Figure 4As shown, the blue dots represent the measured values ​​of nicotine release detected in step 300. The expression of the nonlinear prediction equation obtained from this is as follows:

[0152] .

[0153] The coefficient of determination of the above nonlinear prediction equation is 0.999973, which is relatively accurate. Therefore, this nonlinear prediction equation can be used as a relatively ideal prediction equation.

[0154] Example 4

[0155] The difference between Example 2 and Example 1 is that the source of the tobacco raw materials is different; the tobacco raw materials in Example 4 come from Yunnan Province in China. All other conditions are exactly the same and will not be repeated here. The surface diagram of tobacco release in the smoke of tobacco leaf B obtained in this example is shown below. Figure 5 As shown, the blue dots represent the measured values ​​of nicotine release detected in step 300. The expression of the nonlinear prediction equation obtained from this is as follows:

[0156] .

[0157] The coefficient of determination of the above nonlinear prediction equation is 0.999808, which is relatively accurate. Therefore, this nonlinear prediction equation can be used as a relatively ideal prediction equation.

[0158] In a second aspect of this application, a tobacco heating device 1 is provided for heating the aforementioned tobacco leaf B 101, see reference. Figure 6 The tobacco heating device 1 includes a housing 10, a quartz tube 20, a gas supply assembly 30, a heating assembly 40, and a Cambridge filter 50. The housing 10 has an internal cavity 11; the quartz tube 20 is placed within the cavity 11, and the quartz tube 20 has a heating space 21 for placing tobacco leaves B101. The quartz tube 20 also has an inlet end 22 and an outlet end 23 connected to the heating space 21; the gas supply assembly 30 is connected to the heating space 21 through the inlet end 22 and is used to add gas into the heating space 21; the heating assembly 40 is located within the cavity 11 and outside the quartz tube 20 to heat the quartz tube 20, thereby generating smoke from the tobacco leaves B101; the Cambridge filter 50 is located at the outlet end 23 of the quartz tube 20 and is used to capture the smoke generated by the tobacco leaves B101. The tobacco heating device 1 in this embodiment can simulate real cigarette heating conditions, ensuring that experimental data highly matches actual applications.

[0159] In one embodiment, the gas supply assembly 30 includes a gas cylinder 31 and a gas mixing controller 32. There are two gas cylinders 31, which are used to store oxygen and nitrogen respectively. The gas mixing controller 32 is connected to the two gas cylinders 31 and the gas inlet 22 of the quartz tube 20 respectively, so as to input oxygen and nitrogen into the heating space 21 inside the quartz tube 20 according to a set mixing ratio.

[0160] In one embodiment, the heating assembly 40 includes a thermocouple 41 and an infrared filament 42, both used to heat the quartz tube 20 to generate smoke from the tobacco leaves B 101 within the heating space 21. Schematic, the thermocouple 41 is located outside the quartz tube 20 to transfer heat generated by the thermocouple 41 to the quartz tube 20; the infrared filament 42 is located on the side wall of the cavity 11 of the housing 10 to transfer heat generated by the infrared filament 42 to the quartz tube 20. The tobacco heating device 1 also includes a temperature controller 60, located outside the housing 10 and communicatively connected to the heating assembly 40, to control the temperature of the heating assembly 40, thereby controlling the tobacco leaves B 101101 within the heating space 21.

[0161] In one embodiment, the tobacco heating device 1 further includes a quartz boat 70 disposed in the heating space 21 for placing tobacco leaf B 101 so as to facilitate the removal of tobacco leaf B 101.

[0162] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0163] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the scope of protection of this application. Therefore, the scope of patent protection for this application should be determined by the appended claims, and the specification and drawings can be used to interpret the content of the claims.

Claims

1. A method for predicting nicotine release from tobacco smoke, characterized in that, By substituting the total alkaloid content and glycerol addition ratio in the tobacco into a pre-established nonlinear prediction equation, the predicted amount of nicotine released when the tobacco is heated can be obtained. The method for establishing the nonlinear prediction equation includes the following steps: Tobacco raw materials are graded according to national standards or tobacco industry standards to obtain different grades of tobacco leaves A, and the total alkaloid content of each grade of tobacco leaves A is tested. Adding different mass fractions of glycerol to each grade of tobacco leaf A yields multiple tobacco leaves B, wherein the mass fraction H of glycerol in tobacco leaf B satisfies: H≥0; The tobacco leaf B is heated to generate smoke, the nicotine component in the smoke is captured and extracted, and the nicotine component is measured and analyzed by gas chromatography to obtain the nicotine release amount of the tobacco leaf B. Using the total alkaloid content and the proportion of glycerol added as independent variables, and the nicotine release amount as the dependent variable, a nonlinear prediction equation for the nicotine release amount in tobacco smoke is fitted. The expression of the nonlinear prediction equation is as follows: ； Where z(x, y) represents the predicted nicotine release from the tobacco raw material, x represents the proportion of glycerol added, y represents the total alkaloid content in tobacco leaf A, and k1~k 14 All represent the fitting parameters, and k1~k 14 All are real numbers.

2. The prediction method according to claim 1, characterized in that, Before detecting the total alkaloid content in the tobacco leaf A, a pretreatment step is included, which involves placing the tobacco leaf A under conditions of 20℃~24℃ and 50%~70% relative humidity for 45h~50h to achieve equilibration.

3. The prediction method according to claim 1, characterized in that, When grading the tobacco raw materials, each grade of tobacco leaf A includes upper leaves, middle leaves and lower leaves.

4. The prediction method according to claim 1, characterized in that, The preparation method of the tobacco leaf B includes the following steps: drying the tobacco leaf A; Glycerin is added to tobacco leaf A using a gradient method to obtain tobacco leaf B, wherein the gradient variation range is 1% and the mass fraction H is 0% to 15%; The tobacco leaf B was placed under conditions of 28℃~32℃ and 30%~50% relative humidity for 65h~80h to equilibrate.

5. The prediction method according to claim 1, characterized in that, Heating the tobacco leaf B satisfies at least one of the following conditions: The tobacco leaf B is ground. The tobacco leaf B is heated in a mixed atmosphere of oxygen and nitrogen, wherein the flow rate of the mixed atmosphere is 0.1 L / min to 0.3 L / min; The heating method is as follows: the tobacco leaf B is placed in the tobacco heating device, a mixed atmosphere is introduced into the tobacco heating device for 2 min to 4 min, and then the tobacco heating device is heated to 300℃ to 400℃ at a rate of 15℃ / s to 20℃ / s, and maintained for 4 min to 6 min.

6. The prediction method according to claim 5, characterized in that, The process of capturing and extracting nicotine from the flue gas includes the following steps: The total particulate matter in the flue gas produced by the tobacco leaf B is captured using a Cambridge filter. An internal standard solution and an alcohol solvent were added to the Cambridge filter, shaken, and allowed to stand to obtain an extract containing the nicotine component.

7. The prediction method according to claim 6, characterized in that, The internal standard solution contains one or more of the following: n-heptadecane, 1,5-butanediol, carvone, quinoline, 2-methylquinoline, and n-octadecane; the alcohol solvent includes isopropanol.

8. The prediction method according to claim 1, characterized in that, The determination and analysis included quantitative analysis of nicotine release in flue gas using the internal standard curve method.

9. The prediction method according to claim 8, characterized in that, The gas chromatography method described herein satisfies one or more of the following conditions: The chromatographic column was an HP-INNOWAX capillary column with dimensions of 30m × 0.25mm × 0.25μm; The carrier gas is helium, the carrier gas control mode is constant flow mode, and the carrier gas flow rate is 0.5 mL / min to 2 mL / min; The injection volume is 1 μL to 2 μL; The injection method is split injection, with a split ratio of (8-12):1; the injection port temperature is 200℃-300℃. Heating program: Initial temperature is 100℃~120℃, hold for 3min~5min, increase to 200℃~250℃ at a rate of 10℃ / min~20℃ / min, hold for 2min~3min, detect temperature at 260℃~290℃, and tail purge flow rate is 20mL / min~30mL / min.

10. A tobacco heating device, characterized in that, The tobacco heating device, used for heating tobacco leaf B as described in any one of claims 1 to 9, comprises: The shell (10) has an internal cavity (11). A quartz tube (20) is placed inside the cavity (11), and the quartz tube (20) has a heating space (21) for placing the tobacco leaf B (101). The quartz tube (20) has an air inlet (22) and an air outlet (23) connected to the heating space (21). The gas supply assembly (30) is connected to the heating space (21) through the gas inlet (22) and is used to add gas into the heating space (21); A heating assembly (40) is disposed in the cavity (11) and located outside the quartz tube (20) to heat the quartz tube (20) so that the tobacco leaf B (101) produces smoke; A Cambridge filter (50) is located at the outlet (23) for capturing the smoke generated by the tobacco leaf B (101).

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