A modified natural plant aerosol generating substrate containing an atomising agent

Abstract

The application discloses a modified natural plant aerosol generating substrate containing atomizing agent, which is used for an electric heating smoking set and comprises a quantified cell wall breaking treated natural plant raw material and an exogenous atomizing agent loaded in the natural plant raw material. The application realizes the modification of the tobacco raw material in a quantified and controllable manner by studying the cell wall breaking mechanism of the natural plant raw material and exploring the quantified cell wall breaking treatment method, breaks the cell wall of the tobacco raw material, forms an aerosol carrier, and atomizing agent absorbed in the aerosol carrier can reduce the contact with moisture in the air, thereby reducing the apparent hygroscopicity. In addition, by studying the influence of different atomizing agent components on the loading rate and the influence of the atomizing agent loading amount and the whole tobacco strand rate on the processability, an atomizing agent ratio which can be efficiently produced by using traditional processes and equipment is found, the product quality is improved, and the equipment reconstruction or modification cost is reduced.

Description

Technical Field

[0001] This invention relates to the field of novel tobacco technology, and in particular to a modified natural plant aerosol generating matrix containing an atomizing agent. Background Technology

[0002] In recent years, with the increasingly stringent tobacco control situation and consumers' growing awareness of health, new tobacco products have become increasingly popular. Heated cigarettes and other aerosol-generating products have achieved a good smoking experience after rapid development and optimization in recent years. However, due to the special heating method of heated cigarettes, existing traditional cigarette tobacco cannot be used as the filler material. Therefore, reconstituted tobacco leaves, i.e., tobacco sheets, are mostly used as filler materials. These sheets are mainly composed of tobacco dust, tobacco fragments, tobacco stems, or low-grade tobacco leaves with adhesives and other additives. They are mainly prepared by three methods: papermaking, slurry processing, and rolling. This differs significantly from traditional tobacco and requires the construction of new production lines. There have also been attempts to use traditional cigarette tobacco in heated cigarettes. To release sufficient aroma substances under heating conditions, traditional tobacco needs to undergo high-loss permeability treatments such as steam explosion and freeze-drying. However, direct high-loss permeability treatment severely reduces the processability of the tobacco, resulting in a low yield of whole tobacco leaves. Furthermore, it presents difficulties in rolling and splicing the tobacco leaves on the production line. In addition, there are reports of attempts to use biological enzymes to promote tobacco fermentation, but these only focus on the conversion of aroma substances in tobacco and fail to quantitatively break down the cell walls and quantitatively and fully absorb exogenous atomizing agents. The atomizing agents are still exposed outside the cell walls, affecting processability, and the moisture absorption problem cannot be solved. Summary of the Invention

[0003] To address the shortcomings of existing technologies and practical needs, this invention provides a modified natural plant aerosol generation matrix containing an atomizing agent. The purpose of this invention is to improve the actual absorption rate of exogenous atomizing agents by heated tobacco cells, thereby further improving processability while meeting the requirement of high aerosol loading.

[0004] To achieve this objective, the present invention adopts the following technical solution:

[0005] In a first aspect, the present invention provides a modified natural plant aerosol generating matrix containing an atomizing agent, the aerosol generating matrix being used in an electric heating smoker, comprising: natural plant raw materials subjected to quantified cell wall disruption treatment and an exogenous atomizing agent loaded within the natural plant raw materials;

[0006] The exogenous atomizing agent accounts for M% of the natural plant raw material. The exogenous atomizing agent includes glycerol and propylene glycol. The weight percentage of glycerol in the exogenous atomizing agent is m3, and the weight percentage of propylene glycol in the exogenous atomizing agent is m2, satisfying the following:

[0007]

[0008] Among them, L 30 The maximum glycerol loading of the natural plant material is L. 20 L3 is the maximum propylene glycol loading of the natural plant material, L2 is the maximum propylene glycol loading of the natural plant material after quantified cell wall disruption treatment, and C is the filament ratio of the modified natural plant aerosol generation matrix.

[0009] Furthermore, the natural plant aerosol generating matrix exhibits a first thermal weight loss temperature range [T] under thermal weight loss testing. 1L , T 1H The first thermal weight loss temperature range includes [180℃, 190℃], [190℃, 198℃], [198℃, 210℃], [210℃, 225℃] or [225℃, 250℃].

[0010] Furthermore, the first thermal weight loss temperature range includes the maximum weight loss rate peak, and the temperature T1 corresponding to the maximum weight loss rate peak is in the range of [180℃, 190℃], [190℃, 198℃], [198℃, 210℃], [210℃, 225℃] or [225℃, 250℃].

[0011] Furthermore, the DTG value corresponding to the maximum weightlessness rate peak is V1, which satisfies: V1 ≤ -0.30 s -1 V1≤-0.35 s -1 V1≤-0.40 s -1 V1≤-0.45 s -1 Or V1 ≤ -0.48 s -1 .

[0012] Furthermore, the T 1L The corresponding DTG value is V 1L The T 1H The corresponding DTG value is V 1H Satisfying: V 1L = V 1H =90% × V1, and T 1L - T 1H ≤50℃, T 1L - T 1H ≤40℃, T 1L - T 1H ≤35℃, T 1L - T 1H ≤30℃, T 1L -T1H ≤27.5℃, T 1L - T 1H ≤25℃ or T 1L - T 1H ≤22.5℃.

[0013] Furthermore, the natural plant aerosol generation matrix satisfies the following:

[0014] .

[0015] Furthermore, the filament content C of the modified natural plant aerosol matrix is ​​above 60%, above 65%, above 68%, above 70%, above 72%, above 75%, above 78%, or above 80%.

[0016] Furthermore, the proportion M of the exogenous atomizing agent in the natural plant raw material is 7.5%-10.0%, 10.0-12.5%, 12.5-15.0%, 15.0-17.5%, 17.5-20.0%, 20.0-22.5%, 25.0-27.5%, or 27.5-30.0%.

[0017] Furthermore, the relationship between m2 and m3 satisfies: 6:4≤m3:m2≤4:6 or 4:6≤m3:m2≤2:8.

[0018] Furthermore, the relationship between m2 and m3 satisfies: m3 + m2 = 100%.

[0019] Furthermore, the quantitative cell wall breaking treatment includes 1 to 5 enzymatic cell wall breaking steps, each of which includes: step (1): uniformly spraying the active cell wall breaking enzyme solution onto the natural plant material; step (2): sealing the sprayed natural plant material and carrying out the enzymatic cell wall breaking reaction under constant temperature and humidity conditions.

[0020] Furthermore, in step (1), the weight ratio of the active cell wall breaking enzyme to the natural plant raw material is 0.5-1.0%, 1.0-1.5%, 1.5-2.0%, 2.0-2.5%, or 2.5-3.0%.

[0021] Furthermore, in step (1), the active cell wall-breaking enzyme includes any one or a combination of at least two of pectinase, hemicellulase, cellulase and amylase.

[0022] Furthermore, in step (2), the conditions for the enzymatic hydrolysis and cell wall breaking reaction are: temperature 25-30℃, 30-35℃, 35-40℃, 40-45℃, 45-50℃, 50-55℃ or 55-60℃, relative humidity 15-20%, 20-25%, 25-30%, 30-35%, 35-40%, 40-45%, 45-50%, 50-55%, 55-60%, 60-65%, 65-70%, 70-75% or 75-80%; and the time for a single enzymatic hydrolysis and cell wall breaking reaction is 0.5-1.0 h, 1.0-2.0 h, 2.0-4.0 h, 4.0 h-6.0 h, 6.0-8.0 h, 8.0-12.0 h or 12.0-24.0 h.

[0023] Furthermore, the active enzyme composition solution comprises the active enzyme and the exogenous atomizing agent.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] (1) This invention discovers that by using active enzymes to perform low-damage permeable treatment on tobacco leaves, it is possible to quantitatively and controllably modify tobacco raw materials, break down their cell walls, and form an aerosol carrier. The aerosol absorbed in the carrier can reduce contact with moisture in the air and reduce apparent hygroscopicity. Moreover, while maintaining processability (especially high whole tobacco yield and low aerosol extraction rate), it can absorb more aerosol and release more aroma substances during heating, allowing tobacco to be processed directly on traditional cigarette production lines. In addition, the inventors have also discovered that by keeping the actual aerosol loading rate below the whole tobacco yield, the actual aerosol extraction rate can be reduced, thereby maintaining better processability. By selecting a specific degradation enzyme composition, the enzymatic degradation reaction can be achieved in the storage environment of existing leaf storage cabinets without the need to add a special high-temperature reaction device, which greatly reduces the cost of rebuilding or modifying the production line. Since it is not necessary to use solvent soaking, microwave heating, or other processes, the loss of aroma substances is avoided, and the natural aroma of tobacco can be fully volatilized. Attached Figure Description

[0026] The above description of the present invention and the following detailed embodiments will be better understood when read in conjunction with the accompanying drawings. It should be noted that the drawings are merely examples of the claimed technical solutions.

[0027] Figure 1 This is a morphological image of tobacco leaf cells treated with pectinase under a transmission electron microscope.

[0028] Figure 2 This is a morphological image of tobacco leaf cells treated with hemicellulase under a transmission electron microscope.

[0029] Figure 3This is a morphological image of tobacco leaf cells treated with hemicellulase under a transmission electron microscope.

[0030] Figure 4 The graph shows the cell wall rupture rate after treatment with different concentrations of pectinase.

[0031] Figure 5A This is a graph showing the TG curves of tobacco leaves treated with different concentrations of pectinase.

[0032] Figure 5B These are DSC curves of tobacco leaves treated with different concentrations of pectinase.

[0033] Figure 6A These are TG curves of tobacco leaves treated with different enzyme combinations.

[0034] Figure 6B These are DSC curves of tobacco leaves treated with different enzyme combinations;

[0035] Figure 7A These are the TG curves for different aerosol generation matrices;

[0036] Figure 7B These are DSC curves for different aerosol generation matrices;

[0037] Figure 8A These are TG curves after adding different amounts of atomizing agent;

[0038] Figure 8B These are DSC curves after adding different amounts of atomizing agent;

[0039] Figure 9 This is a schematic diagram of the maximum atomizing agent load testing device of the present invention, wherein the reference numerals are explained as follows: 1-tobacco shreds, 2-extrusion container, 3-force application probe;

[0040] Figure 10 This is a schematic diagram of the main equipment deployment of the production line of the present invention. Detailed Implementation

[0041] To further illustrate the technical means and effects of this invention, the following description, in conjunction with embodiments and accompanying drawings, provides a further explanation of the invention. It is understood that the specific embodiments described herein are merely illustrative of the invention and not intended to limit it.

[0042] The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used herein, are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not limited to those elements and may also include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.

[0043] "Optional" or "any one" means that the matter or event described thereafter may or may not occur, and the description includes both the possibility that the event will occur and the possibility that the event will not occur.

[0044] The indefinite articles “a” and “an” preceding an element or component of this invention do not impose any limitation on the quantity (i.e., number of occurrences) of the element or component. Therefore, “an” or “a” should be interpreted as including one or at least one, and the singular form of an element or component also includes the plural form, unless the quantity clearly refers only to the singular form.

[0045] The terms "one embodiment," "some embodiments," "exemplary," "specific example," or "some examples," etc., used in this invention refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the invention. In this document, the illustrative expressions of the above terms are not necessarily directed at the same embodiment or example.

[0046] I. Raw Materials

[0047] Unless otherwise specified below, the tobacco used is 2021 Henan Sanmenxia Mianchi C3F Qinyan 96 flue-cured tobacco.

[0048] The patent holder also used the following flue-cured tobacco leaves for experiments: Chenzhou Guiyang B2F, C2F, X2F; Yongzhou Lanshan B3F, C2F, X2F; Sanmenxia Mianchi B2F, C3F, X3F; Guizhou Zunyi B2F, C2F, X2F; Bijie Dafang B3F, C3F, X2F; Guizhou Bijie B2F, C2F, X3F; Yunnan Yuxi B3F, C3F, X2F; Yunnan Kunming B2F, C3F, X2F; Yunnan Dali B2F, C3F, X2F, including tobacco seed varieties such as Honghua Dajinyuan, Cuibi No. 1, and Qinyan 96. In addition, the patent holder also used burley tobacco, aromatic tobacco, cigar tobacco, sun-cured tobacco, and cloves for experiments. Unless otherwise specified below, this patent also applies to the above-mentioned raw materials.

[0049] II. Enzyme Preparations

[0050] 1. Pectinase: Activity 60000 U / g, purchased from Beijing Xiasheng Biotechnology Development Co., Ltd., the main components are protopectinase, polygalacturonase, pectin lyase and pectin esterase.

[0051] 2. Hemicellulase: Activity 50000 U / g, purchased from Beijing Xiasheng Biotechnology Development Co., Ltd., the main component is mannanase, its function is to degrade hemicellulose. The patentee found that after it acts on the tobacco cell wall, the products are mainly mannooligosaccharides and a small amount of mannose, etc.

[0052] 3. Amylase: Activity 50000 U / g, purchased from Beijing Xiasheng Biotechnology Development Co., Ltd. It contains multiple bioactive components such as cellulase, β-glucanase and xylanase. The patentee has discovered that it can degrade non-starch polysaccharides in tobacco, rapidly disintegrate the structure of fiber, protein and starch that are intertwined, promote the separation of each component, and improve the content of residual starch in fiber.

[0053] 4. Cellulase: Activity 50000 U / g, purchased from Beijing Xiasheng Biotechnology Development Co., Ltd., Xiasheng Cellulase (CEL-01 type), mainly contains endonuclease (EG), and contains a small amount of exonuclease and a small amount of β-1,4 glucosidase.

[0054] III. Other Major Materials, Reagents and Instruments

[0055] Experimental water: Grade I water (resistivity > 18.2 MΩ·cm) as specified in GB / T 6682-2008.

[0056] Instruments: ME204 electronic balance (sensitivity 0.0001 g, Mettler Toledo, USA); A33 continuous flow analyzer (BRAN LUEBBE, Germany); Fibertec 2010 fiber analyzer (FOSS, Denmark); Helios NanoLab 600i dual-beam focused ion beam scanning electron microscope (FEI, USA); Spirit 120kV transmission electron microscope (FEI, USA); ICS-3000 multi-functional ion chromatograph (Dionex, USA); 6890N-5975C gas chromatograph-mass spectrometer (Agilent Technologies, USA); TGA / DSC 3+ thermogravimetric analyzer; IST 16 thermal analysis system (Mettler-Toledo, Switzerland); Milli-Q Reference ultrapure water system (Millipore, USA); KBF 720 constant temperature and humidity chamber (Binder, Germany).

[0057] Blank Example A: Enzymatic hydrolysis without the addition of exogenous biological enzymes

[0058] According to traditional processes, the raw tobacco leaves are rehydrated, cut into shreds to obtain tobacco shreds, and then subjected to low-loss permeability treatment and harm reduction treatment. Take 50 g of the shredded tobacco.

[0059] Take 50 g of high-purity water (without active enzyme composition) and place it in a laboratory sprayer, then spray it evenly onto the tobacco product. Seal the sprayed tobacco product and place it in a constant temperature and humidity chamber (temperature 55℃, relative humidity 25%) for 4 h. Then place the reacted tobacco in an oven at 80℃ for 20 min. Finally, dry the final tobacco in an oven at 50℃ for 20 min, and use it as a tobacco sample for later use.

[0060] Examples B1-B6: Pectinase hydrolysis

[0061] According to traditional processes, the raw tobacco leaves are rehydrated and then shredded to obtain tobacco shreds. Each batch of tobacco shreds weighs 50g and undergoes low-loss permeability treatment and harm reduction treatment.

[0062] Dilute the pectinase with ultrapure water to prepare a 200 U / g pectinase solution. Prepare the solution immediately before use and place it in a laboratory sprayer.

[0063] In Examples B1-B6, pectinase was uniformly sprayed onto the tobacco shreds according to the pectinase-to-tobacco mass ratio specified in Table 1. After spraying, the tobacco shreds were sealed and placed in a constant temperature and humidity chamber (set temperature 55℃, relative humidity 25%) for enzymatic hydrolysis for 4 hours. The hydrolyzed tobacco shreds were then placed in an oven to terminate the enzymatic hydrolysis reaction (set temperature 80℃, baking time 20 min). The finally hydrolyzed tobacco shreds were then dried in an oven (set temperature 50℃, baking time 20 min) and used as tobacco shred samples for later use.

[0064] Table 1: Mass ratio of pectinase and tobacco in each example

[0065]

[0066] Examples C1-C4: Enzymatic hydrolysis of hemicellulase

[0067] According to traditional processes, the raw tobacco leaves are rehydrated and then shredded to obtain tobacco shreds. Each batch of tobacco shreds weighs 50g and undergoes low-loss permeability treatment and harm reduction treatment.

[0068] Dilute the hemicellulase with ultrapure water to prepare a 200 U / g hemicellulase solution. Prepare the solution immediately before use and place it in a laboratory sprayer.

[0069] Hemicellulase and tobacco were sprayed evenly onto the tobacco shreds according to the proportions shown in Table 2, corresponding to examples C1-C4 respectively. After spraying, the tobacco shreds were sealed and placed in a constant temperature and humidity chamber (set temperature 55℃, relative humidity 25%) for enzymatic hydrolysis for 4 hours. The enzymatically hydrolyzed tobacco shreds were then placed in an oven to terminate the enzymatic hydrolysis reaction (set temperature 80℃, baking time 20 min). Each group underwent three repeated spraying and enzymatic hydrolysis processes, for a total enzymatic hydrolysis reaction of 12 hours. The finally enzymatically hydrolyzed tobacco shreds were then dried in an oven (set temperature 50℃, baking time 20 min) as tobacco shred samples for later use.

[0070] Table 2: Mass ratio of hemicellulase and tobacco in each example

[0071]

[0072] Examples D1-D4: Amylase hydrolysis

[0073] According to traditional processes, the raw tobacco leaves are rehydrated and then shredded to obtain tobacco shreds. Each batch of tobacco shreds weighs 50g and undergoes low-loss permeability treatment and harm reduction treatment.

[0074] Dilute the amylase with ultrapure water to prepare a 200 U / g amylase solution. Prepare the solution immediately before use and place it in a laboratory sprayer.

[0075] Amylase and tobacco were sprayed evenly onto the tobacco shreds according to the proportions shown in Table 3, corresponding to examples D1-D4 respectively. After spraying, the tobacco shreds were sealed and placed in a constant temperature and humidity chamber (set temperature 55℃, relative humidity 25%) for enzymatic hydrolysis for 4 hours. The enzymatically hydrolyzed tobacco shreds were then placed in an oven to terminate the enzymatic hydrolysis reaction (set temperature 80℃, baking time 20 min). The finally enzymatically hydrolyzed tobacco shreds were then dried in an oven (set temperature 50℃, baking time 20 min) and used as tobacco shred samples for later use.

[0076] Table 3: Mass ratio of amylase and tobacco in each example

[0077]

[0078] Examples G1-G6: Enzymatic hydrolysis of enzyme compositions

[0079] According to traditional processes, the raw tobacco leaves are rehydrated and then shredded to obtain tobacco shreds. Each batch of tobacco shreds weighs 50g and undergoes low-loss permeability treatment and harm reduction treatment.

[0080] Prepare the enzyme composition according to the following weight ratio, dilute the enzyme composition with ultrapure water to prepare an enzyme composition solution of 200 U / g, and use it immediately. Put the enzyme composition solution into a laboratory sprayer.

[0081] The enzyme composition formulations are shown in Table 4, corresponding to examples G1-G6 of the tobacco shreds. The enzyme composition was uniformly sprayed onto the tobacco shreds at a ratio of 1.0% by mass of tobacco. After spraying, the tobacco shreds were sealed and placed in a constant temperature and humidity chamber (set temperature 55℃, relative humidity 25%) for enzymatic hydrolysis for 4 hours. The hydrolyzed tobacco shreds were then placed in an oven to terminate the enzymatic hydrolysis reaction (set temperature 80℃, baking time 20 min). The finally hydrolyzed tobacco shreds were then dried in an oven (set temperature 50℃, baking time 20 min) and used as tobacco shred samples for later use. Alternatively, replacing hemicellulase with cellulase yielded similar experimental results.

[0082] Table 4: Enzyme Composition Ratio

[0083]

[0084] Examples H1-H5: Different Nebulization Doses

[0085] Add 10%, 15%, 17.5%, 20%, and 25% of the tobacco weight of the tobacco shreds to the tobacco shreds obtained in Example B2, respectively, and then use them as tobacco shreds samples for Examples H1-H5.

[0086] Examples H6-H9: Different atomizing agent formulations

[0087] Add 15% by weight of atomizing agent, consisting of glycerol and propylene glycol, to the tobacco shreds obtained in Example B2. The formulation of the atomizing agent is shown in Table 5. Then, use them as tobacco shreds samples for Examples H6-H9.

[0088] Table 5: Proportion of atomizing agent in each embodiment

[0089]

[0090] To further demonstrate the beneficial effects of this patent, the tobacco samples from blank example A and examples B to H were tested using the following test examples.

[0091] Experimental Example 1: Scanning Electron Microscopy Experiment of Tobacco Slices

[0092] This experimental case was tested at the Protein Science Research Platform of the Institute of Biophysics, Chinese Academy of Sciences.

[0093] The tobacco samples were placed in phosphate buffer (0.1 MPB, pH 7.2-7.4) of 2.5% glutaraldehyde + 2% paraformaldehyde at 4°C for 3 days. They were then washed four times on ice with 0.1 M PB for 10 min each time. The samples were then fixed at 4°C for 2 h with 1% osmium tetroxide solution (0.1 MPB). They were then washed three times on ice with redistilled water for 10 min each time. Gradient dehydration was performed using ethanol solution according to the conditions in Table 6, and gradient osmosis was performed according to the conditions in Table 7.

[0094] Table 6: Gradient elution conditions

[0095]

[0096] Table 7: Gradient Permeability Conditions

[0097]

[0098] The tobacco samples, after being permeated with the enzyme solution, were placed in a mold filled with resin (+0.7% DMAE) and polymerized at 45°C for 12 h and 70°C for 24 h, respectively. The polymerized tobacco samples were then cut into 70 nm thick tobacco sheets using a Leica UC6 slicer, and the tobacco sheet samples were backscattered electron images performed using a scanning electron microscope.

[0099] The scanning electron microscopy results of tobacco samples B1, B3, B5, and B6 obtained using a Spirit 120kV transmission electron microscope show that ( Figure 1 (scale bar is 2μm), where Figure 1 In this context, A is a blank example A; Figure 1 In this context, B refers to Example B1 (treated with 0.5% pectinase). Figure 1 C in the example is Example B3 (treated with 1.0% pectinase); Figure 1 D in the text refers to Example B5 (treated with 1.5% pectinase). Figure 1 E in the example is Example B6 (treated with 2.0% pectinase);

[0100] Blank example A ( Figure 1 In A), the tobacco cells showed intact overall structure, with complete organelles and clear boundaries. However, with increasing pectinase concentration, the structures of the cells within the cells were significantly altered. Figure 1 C~ Figure 1 In the E-cell structure, cell wall rupture, organelle dissolution, and cell wall swelling were observed. The decomposition and rupture of the cell wall may be the mechanism by which heated cigarette tobacco-type smoke-generating media effectively adsorbs atomizing agents and releases flavor substances upon heating.

[0101] In addition, intercellular spaces and cell wall rupture rates can be obtained by measurement and statistics under an electron microscope.

[0102] The cell wall rupture rates of tobacco leaf cells after treatment with different concentrations of pectinase in Examples B1, B3, B5, and B6 are as follows: Figure 3 As shown, pectinase exhibits a clear dose-response relationship in disrupting cell walls. When the amount of pectinase added is greater than 1%, the cell wall rupture rate in the experimental group is significantly different from that in the control group A, indicating that under this concentration, pectinase can significantly disrupt the cell wall structure of tobacco leaves.

[0103] like Figure 2 (Scale bar is 10μm) and Figure 3 (As shown in the figure, scale bar is 2μm), where Figure 2 In this context, A is a blank example A; Figure 2 B in the example is Example C1 (treated with 0.5% hemicellulase); Figure 2 C in this context refers to 2 in Example C (treated with 1.0% hemicellulase). Figure 2 D in the example is Example C3 (treated with 1.5% hemicellulase); Figure 2 E in the example is Example C4 (treated with 2.0% hemicellulase);

[0104] in Figure 3 In this context, A is a blank example A; Figure 3 B in the example is Example C1 (treated with 0.5% hemicellulase); Figure 3 C in this context refers to Example C2 (treated with 1.0% hemicellulase). Figure 3 D in the example is Example C3 (treated with 1.5% hemicellulase); Figure 3 E in the example is Example C4 (treated with 2.0% hemicellulase).

[0105] Transmission electron microscopy (TEM) results of 10 μm and 2 μm intercellular gaps in tobacco samples treated with C1-C4 hemicellulase, compared with blank example A (…). Figure 2 Group A) and low concentration treatment group ( Figure 2 In B), the tobacco cells are arranged in an orderly and compact manner with clear cell wall boundaries. However, as the concentration of the gradient treatment increases, in Figure 2 In cell C, disordered cell arrangement, widened intercellular spaces, cell wall swelling, and further widening of intercellular spaces leading to cell detachment were observed. With increasing hemicellulase concentration, no obvious cell wall rupture was observed, the overall cell morphology changed from round to irregular, and organelles gradually dissolved. This indicates that although hemicellulase treatment did not cause cell wall rupture, it effectively penetrated the cell and destroyed organelles by disrupting the cell wall's microstructure, thus achieving the mechanism of effective adsorption and release of atomizing agents and flavoring substances upon heating.

[0106] Amylase, vitamin B complex, or enzyme combinations can also achieve similar effects in adsorbing atomizing agents and effectively releasing flavoring substances upon heating.

[0107] Test Example 2: Maximum Atomizing Agent Load Test

[0108] According to the products of Examples A, B1-B6, C1-C4, D1-D4, and G1-G6, a certain mass of tobacco samples were weighed and placed in a constant temperature and humidity chamber, and equilibrated for 4 hours at 25°C and 20% humidity. Using a tobacco filling value measuring instrument, 20g of equilibrated tobacco was accurately weighed, and 1% (by weight) of atomizing agent (100% glycerol) was evenly sprayed onto the tobacco. Meanwhile, tests were conducted separately for Examples A and B1-B6 using 100% propylene glycol as the atomizing agent.

[0109] like Figure 9 As shown, tobacco shreds 1 with 1% atomizing agent (relative to the initial tobacco mass) were placed in a compression container 2. The compression container 2 was a cylindrical barrel with a diameter of (60.0±0.1) mm and a height of not less than 100 mm. A force-applying probe 3 with a diameter of (55.0±0.1) mm and capable of generating a uniform pressure of (29.4±0.5) N on the sample was applied to the surface of the tobacco shreds. The pressure application speed of the force-applying probe was (19.5±0.5) mm / s, and the pressure application time was (30.0±0.5) s. After the pressure was applied, the tobacco shreds were poured out onto a flat piece of white paper and gently shaken. If the tobacco shreds could be dispersed well without obvious clumping, then 1% atomizing agent (relative to the initial tobacco mass) was applied again, and all other conditions remained unchanged, and the above experiment was repeated. The experiment was terminated when the tobacco shreds were poured onto a flat sheet of white paper and gently shaken. If the tobacco shreds could not be dispersed well and showed obvious clumping, it indicated that the atomizing agent had not been extracted. The amount of atomizing agent used at this point was recorded as B%. The maximum load of tobacco substances on the atomizing agent under these conditions was (B-1)%. The test results are shown in Tables 8 and 9.

[0110] Table 8: Maximum loading after different enzyme treatments

[0111]

[0112] Table 9: Maximum loading capacity after treatment with different enzyme compositions

[0113]

[0114] Based on scanning electron microscopy experiments and maximum atomizing agent loading experiments, it can be deduced that the maximum loading is determined by the cell wall rupture rate, intercellular space, and the viscosity of the atomizing agent. Table 10 shows the results of intercellular space, cell wall rupture rate, and maximum atomizing agent loading tests for Examples A, B1, B3, B5, and B6.

[0115] Table 10: Relationship between intercellular space, cell wall rupture rate and maximum atomizing agent load

[0116]

[0117] Furthermore, as can be seen from Example A, even without enzymatic degradation treatment, the intercellular spaces are sufficient to accommodate a certain amount of atomizing agent, thus exhibiting a maximum loading rate of 13% (L). 30 Therefore, in order to ensure that the nebulizer is absorbed as much as possible within the ruptured cells rather than remaining in the intercellular spaces, it is necessary to consider the intracellular loading (i.e., L3-L). 30 This is related to the degree of cell rupture; on the other hand, the actual intracellular loading (RL) should be below 80%, or below 70%, or below 60%, or even below 50%, so that the low atomizing agent extraction rate of tobacco will be significantly reduced.

[0118] Because propylene glycol and glycerol have different viscosities, propylene glycol appears to have a higher maximum loading rate, i.e., L0.05. 20 > L 30 Furthermore, L2 > L3. Aerosols are typically a combination of multiple aerosol-generating agents such as propylene glycol and glycerol, therefore the actual intracellular loading (RL) should be calculated for different aerosol-generating agents.

[0119]

[0120] Among them, L 30 The maximum glycerol loading of the natural plant material is L. 20 L1 represents the maximum propylene glycol loading of the natural plant material, L2 represents the maximum glycerol loading of the natural plant material after quantified cell wall disruption treatment, and L3 represents the maximum propylene glycol loading of the natural plant material after quantified cell wall disruption treatment.

[0121] Experimental Example 3: Thermogravimetric Analysis of Tobacco Shreds

[0122] This patent describes thermogravimetric analysis of tobacco leaves treated with 0-2.0% enzyme (Examples A and B1-B4) to investigate the effect of different cell wall rupture degrees on the heat release performance of tobacco leaves.

[0123] Approximately 5 mg of tobacco sample treated with enzyme solution was weighed, and 18% of atomizing agent (100% glycerol) was added. The sample was then placed in an alumina crucible and subjected to thermogravimetric analysis (TGA). Since the heating temperature of the cigarette core segment did not exceed 400℃, the heating program was selected to increase the temperature from 30℃ to 400℃ at a rate of 20℃ / min; gas flow rate: 40 mL / min; ambient gas: air. Each parallel sample was repeated three times.

[0124] The results of tobacco leaves treated with different concentrations of pectinase in Examples A and B1-B4 are as follows: Figure 5A and Figure 5B As shown in the figure, when the temperature is between 30 and 125°C, the weight loss ratio of tobacco leaves treated with different concentrations of pectinase is relatively small, ranging from 5% to 10%, and the corresponding weight loss rate of the DTG curve is also low. It is noteworthy that the temperature at which the maximum weight loss rate of tobacco leaves treated with pectinase occurs within this temperature range is 25°C lower than that of blank example A, suggesting that cell wall rupture within this temperature range promotes the evaporation and premature release of water and some small molecule chemical substances. When the temperature is between 125 and 250°C, the TG curve gradually becomes the stage of maximum weight loss of tobacco leaves with increasing pectinase concentration, with a weight loss ratio of 25% to 35%. The corresponding DTG curve shows a larger weight loss rate, with the maximum weight loss rate occurring at 210°C. When the pectinase treatment concentration exceeds 50 U / g, this stage becomes the range of maximum weight loss rate, and the weight loss ratio increases with increasing pectinase concentration. The inventors believe that this stage may be the release range of the main small molecule aroma substances. When the temperature was between 250 and 350℃, the TG curve showed that the weight loss percentage of the tobacco leaves was between the first two temperature ranges, ranging from 15% to 25%. The corresponding DTG curve showed the maximum weight loss rate at 310℃, and the weight loss percentage decreased with increasing pectinase concentration. The inventors believe that the weight loss at this stage may be due to the decomposition of large, non-volatile macromolecules in the tobacco. The enzymatic hydrolysis of pectin reduces the substrate in this stage, leading to a slight decrease in the weight loss percentage. With increasing enzyme addition, the proportion of weight loss due to heat in the tobacco-type smoking medium continuously increased. Compared to blank example A, the total weight loss of the experimental groups with enzyme additions of 0.5%, 1%, 1.5%, and 2% increased by 4.09%, 5.03%, 7.08%, and 10.06%, respectively, and the weight loss range was mainly between 170 and 220℃.

[0125] Thermogravimetric analysis was performed on tobacco samples treated with the enzyme compositions in Examples G1-G6 as follows: Figure 6A and Figure 6B As shown. The tobacco samples treated with various enzyme compositions also exhibited a first thermal weight loss temperature range, which included the peak of the maximum weight loss rate, with the corresponding temperature T1 ranging from [180℃, 190℃], [190℃, 198℃], [198℃, 210℃], [210℃, 225℃], or [225℃, 250℃].

[0126] Example G2: Thermogravimetric analysis was performed on tobacco samples from conventional tobacco shreds and tobacco sheets as follows: Figure 7A and Figure 7B As shown. Only enzymatically hydrolyzed tobacco exhibits the first thermal weight loss temperature range [T] under thermal weight loss testing. 1L , T1H In this region [180℃, 250℃], such enzymatically hydrolyzed tobacco can produce an aerosol volume comparable to that of sheet-heated cigarettes at 300℃ even at a preheating temperature of less than 250℃, significantly reducing the preheating time.

[0127] In the above embodiments, the DTG value corresponding to the maximum weight loss rate peak of the enzymatically hydrolyzed tobacco within the first thermal weight loss temperature range is V1, which satisfies: V1 ≤ -0.30 s -1 V1≤-0.35 s -1 V1≤-0.40 s -1 V1≤-0.45 s -1 Or V1≤-0.48s -1 This enzymatic hydrolysis of tobacco, even with a preheating time of only 10 seconds, can produce an aerosol volume comparable to that of a sheet-heated cigarette preheated for 25 seconds, significantly shortening the preheating time. 1L The corresponding DTG value is V 1L T 1H The corresponding DTG value is V 1H Satisfying: V 1L = V 1H =90% × V1, and T 1L - T 1H ≤50℃, T 1L - T 1H ≤40℃, T 1L - T 1H ≤35℃, T 1L - T 1H ≤30℃, T 1L -T 1H ≤27.5℃, T 1L - T 1H ≤25℃ or T 1L - T 1H ≤22.5℃.

[0128] The narrower the maximum peak of the weight loss rate of enzymatically hydrolyzed tobacco, the more significant the heating and smoking effect at a specific temperature. When blended with tobacco sheets with a wider maximum peak of weight loss rate or traditional tobacco that does not have a first thermal weight loss temperature range, the amount of smoke and aroma in the first and last puffs can be more consistent with the middle puffs.

[0129] Test Example 4: Whole Filament Rate Test

[0130] The whole-shred rate and broken-shred rate of tobacco shreds in the above examples were determined according to YC / T 178-2003, "Determination Method of Whole Shred Rate and Broken Shred Rate of Tobacco Shreds". For other forms of plant materials such as tobacco, tobacco sheets, and cloves, the whole-shred rate can also be measured and corresponding test results obtained after shredding in a conventional manner. The experiments showed that the whole-shred rate C of Example A was 81%, the whole-shred rate C of Examples B1 and B2 remained at 80%, the whole-shred rate C of Examples B3 and B4 decreased to approximately 77-79%, while that of Example B5 decreased to 75%, and that of Example B6 was close to 70%.

[0131] Test Example 5: Production Line Test

[0132] like Figure 10 As shown, the tobacco shreds and formulation of this invention can be produced using a conventional cigarette production line. The production line includes: a tobacco sheet processing section 100, a tobacco shred processing section 200, a blending and flavoring device 250, a cigarette rolling section 300, and a production line control system. The production line control system includes one or more processors (CPUs), input / output devices or interfaces, wired or wireless network interfaces, and memory. The input devices include human-machine interface devices to receive control information from operators, including cigarette type and formula. The memory stores computer programs and / or computer instructions, which, when executed by the processor, control the production line.

[0133] The tobacco leaf processing section 100 includes an unpacking device, a metering device, a slicing device, a loosening and rehydration device, a tobacco leaf pre-mixing device, a screening device, a feeding device, and a leaf storage device. After the tobacco leaves have been threshed, re-dried, and aged, they are sent to the reuse production line in boxes and need to go through the following processes: unpacking and metering, slicing, loosening and rehydration, tobacco leaf pre-mixing, screening and feeding, leaf mixing and storage. First, according to the leaf group formula requirements of the product, the tobacco leaves are prepared for feeding. The unpacking device 110 is used to unpack the tobacco leaves through the unpacking process. After removing the outer packaging, the tobacco sheets are cut into several pieces of a specified thickness using a slicing device 130. Then, they are loosened and rehydrated using a loosening and rehydration device 150 and a tobacco sheet pre-mixing device to improve the processing resistance of the tobacco sheets and to initially and evenly mix the tobacco sheets. Then, a screening device is used to remove fragments, and tobacco slurry is sprayed onto the tobacco sheets using a feeding device 170. Finally, the selected tobacco sheets are evenly mixed and stored in a leaf storage device 180 for use in the next process stage.

[0134] The feeding device 170 includes a liquid source containing an enzyme combination (with the same ratio as in Example G2) and an atomizing agent composed of glycerol, propylene glycol, and water as the solvent. The feeding device 170 has a nozzle connected to the liquid source, allowing it to selectively spray the liquid onto the tobacco sheets according to instructions from the production line control system. Because the aerosol is added before the enzymatic reaction, the aerosol can quickly fill the interior of the tobacco cell walls after enzymatic hydrolysis, ensuring full absorption of the aerosol by the tobacco and preventing clumping or failure to disperse during subsequent shredding by the shredder 210. The near absence of aerosol residue on the tobacco surface avoids contamination of the production line, particularly preventing the cigarette rolling section 300 from rolling. Furthermore, the glycerol and propylene glycol in the cigarette product are absorbed into the cell walls, reducing their probability of contact with moisture in the air and decreasing apparent water absorption, thereby improving shelf life.

[0135] The leaf storage device 180 can be a leaf storage cabinet. The tobacco leaves sprayed with liquid will be sent into the leaf storage cabinet for enzymatic degradation reaction. The temperature of the leaf storage cabinet is 28-33℃ and the relative humidity is 67-75%. The leaf storage time can be selected as needed.

[0136] Because the enzymatically hydrolyzed tobacco sheets of this invention have high processability, they can be directly processed into heated tobacco shreds through the tobacco processing section 200 of a traditional tobacco production line, including shredding and other processes. The tobacco processing section 200 includes a shredding device, a drying device, and a blending and flavoring device. First, the shredding device shreds the tobacco sheets 21 to form heated tobacco shreds of a certain width. Then, the drying device dries the tobacco shreds. This step, in addition to drying the heated tobacco shreds to remove some of the moisture (to achieve a specified moisture content, for example, 11.5%~14.0%), thereby improving the filling capacity and sensory quality of the shreds, also includes a high-temperature rapid drying process (temperature 200-250℃, preferably 235℃; time 1-10s, preferably 3-5s) to inactivate residual enzyme combinations. Finally, the blending and flavoring device further adds flavorings and additives suitable for heated tobacco to the tobacco shreds, which are then sent to the cigarette rolling section 300.

[0137] The cigarette rolling section 300 includes a cigarette rolling device and a feeding device. The cigarette rolling device rolls heated cigarette tobacco into heated cigarette tobacco segments, and the feeding device feeds heated cigarette tobacco segments and heated cigarette filter segments into heated cigarettes 61.

[0138] Production line experiments revealed that while increased cell rupture can improve intracellular loading and reduce propellant extraction, thus increasing the yield of finished tobacco products, excessively high cell rupture can decrease the whole tobacco yield, ultimately lowering the overall yield. This is because a balance must be struck between maintaining processability and achieving a high whole tobacco yield and propellant extraction rate.

[0139] Experiment Example 6: Sensory Evaluation Experiment

[0140] The tobacco samples from Examples H1-H5 were made into cigarettes, and the cigarette tasters used F5202-JS3 heating devices to heat and smoke them. Referring to GB5606.4-2005 Cigarettes Part 4 Sensory Technical Requirements, YC / T 564-2018 Sensory Evaluation Method for Chinese Cigarettes Based on Consumer Experience, and YC / T 497-2014 Sensory Evaluation Method for Chinese Cigarette Style, and in combination with the characteristics of heated cigarette smoke, key evaluation indicators were formulated, sensory evaluation was conducted, and the evaluation scores were recorded according to Table 11.

[0141] Table 11: Sensory Evaluation Record Form for Tobacco-Based Heated Cigarettes

[0142]

[0143] The sensory evaluation results of the heated cigarettes made from the tobacco shreds in Examples H1-H5 are shown in Table 12:

[0144] Table 12: Sensory Evaluation Record Table for Examples H1-H5

[0145]

[0146] Based on sensory evaluation, adding 15% (by weight) of atomizing agent to the tobacco sample yields the best cigarette production. This amount of atomizing agent ensures sufficient smoke output while maintaining a relatively balanced performance across other indicators, thus effectively achieving the desired smoke production. Furthermore, according to... Figure 6A and Figure 6B Thermogravimetric analysis revealed that as the amount of atomizing agent added increased, the weight loss (smoke production) of the tobacco-type smoke-generating medium gradually increased. However, when the amount added reached 20% or 25%, although the weight loss still increased, the intensity was slightly insufficient. Moreover, the tobacco sticking was more severe at this point, affecting large-scale production.

[0147] The sensory evaluation results of the heated cigarettes made from the tobacco shreds in Examples H6-H9 are shown in Table 13:

[0148] Table 13: Sensory Evaluation Record Table for Examples H6-H9

[0149]

[0150] Glycerin and propylene glycol are the two most common components of atomizing agents. Glycerin provides a better smoke sensation, while propylene glycol provides sweetness and improves smoke characteristics. Based on the sensory evaluation in Table 14, a 4:6 ratio of the two atomizing agents is the preferred formulation.

[0151] According to Table 8, the initial maximum glycerol loading of the tobacco in Example B2 is L. 30The maximum loading of glycerol after quantified cell disruption was 36%, which was 13%. The difference was L3 - L. 30 It was 23%; the initial maximum propylene glycol loading was L. 20 The maximum loading of propylene glycol after quantified cell disruption was 14%, and the maximum loading L2 was 59%, with a difference of L2 – L. 20 The actual load factor RL for embodiments H1-H9 is 45%. Therefore, the actual load factor RL for embodiments H1-H9 is shown in Table 14.

[0152] Table 14: Actual Load R of Examples H1-H9

[0153]

[0154] As can be seen, when the actual loading degree RL is greater than the whole tobacco yield C, the atomizing agent cannot be effectively absorbed by the tobacco and has a high probability of extraction, which affects both the sensory experience and the production of heated cigarettes. Therefore, in order to achieve a balance in various dimensions of tobacco yield, aroma, aerosol extraction rate, and processability, based on the above experimental examples, we can conclude that the actual intracellular loading degree RL and the whole tobacco yield C of the atomizing agent should satisfy the following relationship:

[0155]

[0156] The better option, the better, is to satisfy the following:

[0157]

[0158] Wherein, C represents the whole tobacco shred rate of the enzymatically modified tobacco shreds.

[0159] This invention utilizes cell wall-degrading enzymes to quantitatively and controllably modify traditional cigarette tobacco, enabling it to absorb more aerosols and release more aroma compounds during heating while maintaining its original processability (especially the whole tobacco yield). This allows traditional cigarette production lines to be reused with heated tobacco with only minor modifications. By selecting specific enzyme compositions, the enzymatic degradation reaction can be carried out in the existing leaf storage environment without the need for additional high-temperature reaction equipment.

[0160] The terminology and expressions used herein are for descriptive purposes only, and the invention should not be limited to these terms and expressions. The use of these terms and expressions does not imply the exclusion of any illustrative and descriptive equivalents (or parts thereof), and it should be recognized that various modifications that may exist should also be included within the scope of the claims. Other modifications, variations, and substitutions may also exist. Accordingly, the claims should be considered to cover all such equivalents.

[0161] Similarly, it should be noted that although the present invention has been described with reference to the specific embodiments described above, the present invention is not limited to the detailed methods described above, that is, it does not mean that the present invention must rely on the detailed methods described above to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A modified natural plant aerosol generating matrix containing an atomizing agent, characterized in that, The aerosol generating matrix is ​​used in electric heating smokers and includes: natural plant materials that have undergone quantified cell wall disruption treatment and an exogenous atomizing agent loaded within the natural plant materials; The exogenous atomizing agent accounts for M% of the natural plant raw material. The exogenous atomizing agent includes glycerol and propylene glycol. The weight percentage of glycerol in the exogenous atomizing agent is m3, and the weight percentage of propylene glycol in the exogenous atomizing agent is m2, satisfying the following: Among them, L 30 The maximum glycerol loading of the natural plant material is L. 20 L3 is the maximum propylene glycol loading of the natural plant material, L2 is the maximum propylene glycol loading of the natural plant material after quantified cell wall disruption treatment, and C is the filament ratio of the modified natural plant aerosol generation matrix. The quantitative cell wall disruption treatment includes 1 to 5 enzymatic cell wall disruption steps, each of which includes: Step (1): Spray the active cell wall breaking enzyme solution evenly onto the natural plant material; Step (2): Seal the sprayed natural plant material and carry out enzymatic hydrolysis and cell wall breaking reaction under constant temperature and humidity conditions; In step (1), the active cell wall breaking enzyme includes any one or a combination of at least two of pectinase, hemicellulase, cellulase and amylase.

2. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, The natural plant aerosol generating matrix exhibits a first thermal weight loss temperature range [T] under thermal weight loss testing. 1L , T 1H The first thermal weight loss temperature range includes [180℃, 250℃].

3. The modified natural plant aerosol generating matrix according to claim 2, characterized in that, The first thermal weight loss temperature range includes the maximum weight loss rate peak, and the temperature T1 corresponding to the maximum weight loss rate peak is in the range of [180℃, 250℃].

4. The modified natural plant aerosol generating matrix according to claim 3, characterized in that, The DTG value corresponding to the maximum weightlessness rate peak is V1, which satisfies: V1 ≤ -0.30 s -1 .

5. The modified natural plant aerosol generating matrix according to claim 4, characterized in that, The T 1L The corresponding DTG value is V 1L The T 1H The corresponding DTG value is V 1H Satisfying: V 1L = V 1H = 90% × V1, and T 1L - T 1H ≤50℃.

6. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, The natural plant aerosol generation matrix satisfies the following: .

7. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, The filament ratio (C) of the modified natural plant aerosol generating matrix is ​​above 60%.

8. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, The proportion (M) of the exogenous atomizing agent in the natural plant raw material is 7.5%-30.0%.

9. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, The following condition is satisfied between m2 and m3: 6:4≤m3:m2≤2:

8.

10. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, The condition m2 and m3 satisfy the following relationship: m3 + m2 = 100%.

11. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, In step (1), the weight ratio of the active cell wall breaking enzyme to the natural plant raw material is 0.5-3.0%.

12. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, In step (2), the conditions for the enzymatic hydrolysis and cell wall breaking reaction are: temperature 25-60℃, relative humidity 15-80%; and the time for a single enzymatic hydrolysis and cell wall breaking reaction is 0.5-24 h.

13. The modified natural plant aerosol generating matrix according to claim 1, characterized in that, The active cell-wall-breaking enzyme solution comprises the active cell-wall-breaking enzyme and the exogenous atomizing agent.

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