CN107981405B - Preparation method and application of cigarette without burning by heating - Google Patents

Abstract

A method for preparing a cigarette without burning in heating and its application, adopt the new process of embossing roll, make the heating with certain thickness not burn the tobacco leaf surface of the remaking become uneven, increase the superficial area, strengthen the atomization effect, increase the surface friction, and use the compound aluminium foil cigarette paper of the emboss, when making the rolling up and connecting the machine to roll up and connect and start the car in the later stage, the remaking tobacco leaf and rolling up and connecting the aluminium foil pattern surface of the material compound aluminium foil cigarette paper, the friction is strengthened by a wide margin, easy to process, reduce the parking frequency of the apparatus, make the production go on continuously, raise the production efficiency, reduce material cost and production cost; the low-temperature cigarette has shorter tobacco shred sections, the friction is increased, the tobacco shred falling is reduced, and the problems that the friction force between the smooth surface of the cigarette making leaf which is not combusted after heating and the non-embossed aluminum foil paper of the wrapping material is small, the slipping is serious, the cigarette paper is not moved, the equipment is frequently stopped, and the production efficiency is influenced are overcome; and the low-temperature tobacco shreds of the low-temperature cigarette have short tobacco shred sections and small friction force and are easy to fall off.

Description

A kind of preparation method of heat not burn cigarette and application thereof

technical field

The invention relates to the field of heat-not-burn novel tobacco, in particular to a preparation method and application of a heat-not-burn cigarette.

Background technique

Heat-not-burn reconstituted tobacco leaf is a functional reconstituted tobacco leaf with tobacco components as the main body, loaded with a large dose of atomizing agent, and releasing the atomizing agent through high temperature heating to form a smoke effect. The heat-not-burn reconstituted tobacco is heated by an external heating element, so that the aerosol, tobacco and flavor components in the reconstituted tobacco are heated instead of burning to generate smoke, reducing the risk of burning and thermal cracking in traditional cigarettes. produced harmful components.

When the heat-not-burn reconstituted tobacco leaves are processed and rolled into cigarettes, the friction between the smooth surface of the heat-not-burn reconstituted tobacco leaves and the aluminum foil surface of the wrapping material aluminum foil paper is small, the slippage is serious, and the cigarette paper does not move, causing the equipment to stop frequently , affecting the production efficiency; and the low-temperature cigarettes have short cut tobacco segments, low friction, and the cut tobacco is easy to fall off.

SUMMARY OF THE INVENTION

According to above-mentioned deficiency and defect, the object of the present invention is to provide a kind of preparation method of heat not burn cigarette and its application, in the last step of rolling process of rolling method, one of the two pressing rollers adopts embossing roller, Embossing the heat-not-burn reconstituted tobacco leaves by rolling method to make the surface of the heat-not-burn reconstituted tobacco leaves with a certain thickness uneven, increase the surface area, enhance the atomization effect, increase the surface friction, and use the embossed composite aluminum foil cigarette paper Coiling, so that the friction between the sheet and the aluminum foil surface of the aluminum foil cigarette paper is greatly enhanced when the upper coiling machine is rolled and started, which is easy to process, reduces the frequency of equipment shutdown, enables continuous production, improves production efficiency, and reduces material costs and production costs And the low-temperature cigarette cut tobacco section is short, increasing the friction helps to reduce the drop of the cut tobacco, and overcomes the small friction between the smooth surface of the heat-not-burn reconstituted tobacco leaf and the non-embossed aluminum foil paper of the wrapping material, and the slippage is serious, and the cigarette paper is stripped. Immobility causes frequent shutdown of equipment, affecting production efficiency; and low-temperature cigarettes have short cut tobacco segments, low friction, and low-temperature cut tobacco is easy to fall.

The present invention is achieved through the following technical solutions:

A preparation method of a heat-not-burn cigarette, comprising the steps:

(1) Preparation of raw materials: Prepare raw materials according to the percentage by mass: 50-70% of tobacco raw materials, 10-25% of atomizer, 3-10% of solid adhesive, 1-10% of cigarette additives, and 1-10% of fiber, Warm water 15-35%;

(2) Mixing and pulverizing of dry materials: put the tobacco raw material, solid adhesive and solid cigarette additive calcium salt into the pulverizer in proportion, pulverize to 40 meshes to 300 meshes, and mix them evenly through low temperature and high speed pulverization;

(3) The wet material is mixed and dispersed evenly: the fibers and warm water are poured into the material bucket in proportion, and at the same time of high-speed stirring, ultrasonic cavitation is used to assist the fibers to loosen and disperse more uniformly, and then add the mist of the above step 1) mass ratio Continue the ultrasonic-assisted high-speed stirring to disperse the fibers and the atomizing agent uniformly, and at the same time slowly add the wet material and the tobacco flavor to the uniformly mixed dry material powder in the above step 2), and stir together at a high speed evenly;

(4) Embossing and rolling: the reconstituted tobacco leaves are obtained by rolling for 3 to 9 times. In the last rolling process, the reconstituted tobacco leaves are embossed and rolled with an embossing pressing roller, and then heated and dried to obtain a thermally inert tobacco by rolling. Burn embossed reconstituted tobacco leaves;

(5) wrapping and wrapping: carry out wrapping and wrapping of the heat-not-burn embossed reconstituted tobacco leaves by the rolling method according to the cigarette process specification, and use the embossed composite aluminum foil cigarette paper, filter rods for cigarettes, etc. for wrapping and wrapping, which is the present invention The productivity-enhancing heat-not-burn cigarettes.

Further, the tobacco raw material is one of tobacco leaves and tobacco stems or a mixture thereof.

Further, the cigarette additive is a cigarette flavor and a calcium salt, and the calcium salt is a mixture of one or more of calcium carbonate, calcium lactate, calcium citrate, and calcium tartrate.

Further, the low-temperature pulverization is 0-4° C., 40-300 mesh.

Further, the solid adhesive is sodium alginate, potassium alginate, CMC (carboxymethyl cellulose), PAC (polyanionic cellulose), polyvinyl alcohol, casein gum, rosin, dextrin, chitosan , sodium glycerophosphate, etc. one or more of them.

Further, the fiber is a mixture of one or more of wood pulp, tobacco rod fiber, bagasse pulp, bamboo pulp, coconut fiber and the like.

Further, the temperature of the warm water is 30-60°C.

Further, the atomizing agent is one or a mixture of glycerol, propylene glycol and ethylene glycol.

Further, the speed of the high-speed stirring is 300-1200 r/min.

Further, the frequency of the ultrasound is 20-130KHz.

Further, the thickness of the heat-not-burn reconstituted tobacco leaf is 0.21-0.30 mm, the elongation at break is 1.0-1.6%, and the tensile strength is 300-450 N/m.

Further, the embossed composite aluminum foil cigarette paper is twill or random embossed composite aluminum foil cigarette paper, wherein the thickness of the embossed aluminum foil is 1-19 μm, and the thickness of the cigarette paper is 20-200 μm.

A heat not burn cigarette prepared by the above method is used in electric heating or carbon heating low temperature cigarettes.

The heat-not-burn cigarette with improved production efficiency of the invention has uneven surfaces of the reconstituted tobacco leaves, enhances the atomization effect, increases the surface friction, and uses the embossed composite aluminum foil cigarette paper as the rolling material, so that the upper rolling machine can be rolled in the later stage. When driving, the friction between the embossed aluminum foil surface of the thin sheet and the composite aluminum foil cigarette paper is greatly enhanced, which is easy to process, reduces the frequency of equipment shutdown, enables continuous production, improves production efficiency, and reduces material costs and production costs; Shorter, increasing the friction helps to reduce the drop of shredded tobacco at the end of the cigarette, and overcomes the small friction between the smooth surface of the heat-not-burn reconstituted tobacco leaf and the non-embossed aluminum foil paper of the wrapping material, which causes serious slippage and the cigarette paper does not move. The equipment is frequently stopped, which affects the production efficiency; and the low-temperature cigarette cut tobacco section is short, the friction force is small, and the low-temperature cut tobacco at the end is easy to fall and other defects.

The beneficial effects of the present invention are:

(1) Heat-not-burn reconstituted tobacco leaves are adopted by the rolling method, and applied to low-temperature cigarettes such as electric heating and charcoal heating. Compared with traditional cigarettes, the amount of tobacco raw materials used in each cigarette is reduced by 20-50%, and the cost of tobacco raw materials is reduced. , and the tobacco raw materials and tobacco flavors are heated and volatilized without combustion and thermal cracking, thereby reducing the harm of smoke.

(2) the feature of the technology of the present invention is to adopt tobacco raw material, solid adhesive, solid calcium salt to mix and pulverize to fine powder (40-300 mesh), so that tobacco raw material, adhesive, solid calcium salt (including calcium carbonate, calcium lactate, lemon One or more of calcium acid, calcium tartrate, etc.) are dispersed and mixed evenly, increase the specific surface area and generate a new microporous structure, effectively improve its absorption of the atomizing agent, improve the looseness and increase of the reconstituted tobacco leaves. Thickness increases the comfort of suction; while the fibers are pre-mixed with water, dissociated, and then mixed with the atomizer, using high-speed stirring to achieve the homogenization effect, so that the fibers are fully swelled in the water-atomizer system, and between the fibers Effectively interweave, and then slowly pour the wet material of fiber-water-atomizer into the fine powder of tobacco-adhesive-calcium salt for high-speed stirring evenly, so that the fine tobacco powder, the adhesive and the fiber are completely dispersed and mixed, and the fibers are mixed. , The fiber and the surrounding adhesive are well bonded, so that the reconstituted tobacco leaves have a certain strength, reduce the crushing rate, enhance the processing resistance, shorten the time of mixing and stirring processes, and overcome the ordinary rolling method to prepare the rolling method. Heat not burn When reconstituting tobacco leaves, after the fibers are defibrated in water, they are first mixed with tobacco powder, and then mixed with the remaining materials. The fibers cannot be uniformly dispersed and are easy to form agglomerates. The fibers, atomizers, and tobacco in the reconstituted tobacco leaves are extremely uneven. Defects;

(3) Solid adhesives are sodium alginate, potassium alginate, CMC (carboxymethyl cellulose), PAC (polyanionic cellulose), polyvinyl alcohol, casein gum, rosin, dextrin, chitosan, glycerophosphoric acid Sodium can help the fiber and tobacco raw materials to be closely combined, and improve the tensile strength of heat-not-burn reconstituted tobacco leaves, and the mixture of chitosan-sodium glycerophosphate and so on has a synergistic effect to increase adhesion; natural fibers can increase the strength of reconstituted tobacco leaves , Improve the effect of processing resistance;

(4) The present invention is rolled for 3 to 9 times, so that the fibers and tobacco are dispersed more evenly, the density, strength and thickness of the heat-not-burn reconstituted tobacco leaf are increased, the tensile strength and elongation at break are improved, and the In the last pressing roller process, the reconstituted tobacco leaves are embossed and rolled by an embossing pressing roller, and then heated and dried to obtain heat-not-burn embossed reconstituted tobacco leaves by rolling method. The surface of the reconstituted tobacco leaves is uneven and the atomization effect is enhanced. Increase surface friction;

(5) The twill or disorderly embossed composite aluminum foil cigarette paper, cigarette filter rod, etc. are used for rolling and packaging, so that when the upper rolling machine is rolled and driven, the patterned aluminum foil surface of the sheet and the embossed composite aluminum foil cigarette paper The friction is greatly enhanced, making it easy to process, reducing the frequency of equipment shutdown, enabling continuous production, improving production efficiency, and reducing material costs and production costs; and low-temperature cigarettes have shorter cut tobacco segments, increasing friction helps reduce cigarette ends. , to overcome the small friction between the smooth surface of the heat-not-burn reconstituted tobacco leaf and the non-embossed aluminum foil paper of the wrapping material, the slippage is serious, and the cigarette paper does not move, causing the equipment to stop frequently, affecting the production efficiency; and the low-temperature cigarette cut tobacco section is short, The friction force is small, and the cut tobacco at the end of the low-temperature cigarette is easy to fall off and other defects.

In addition, the embossed composite aluminum foil cigarette paper of the present invention is relatively thin, wherein the thickness of the embossed aluminum foil is 1-19 μm, and the thickness of the cigarette paper is 20-200 μm. In contrast, the comparative invention is that the thickness of the metal foil is 20-60 μm, and the thickness of the cigarette paper is 40-100 μm. In contrast, in the composite aluminum foil cigarette paper of the present invention, the thickness of the aluminum foil is significantly reduced, and the thinner the aluminum foil, the better the composite The less aluminum foil per unit area of aluminum foil paper is used, the lower the cost of aluminum foil cigarette paper, the softer the composite aluminum foil cigarette paper, the less the wear of the cutting tool used in production, the smoother the cigarette stick overlap, and the excessively thick aluminum foil. The mouth will be deformed by the soldering iron and cannot rebound, which will affect the appearance of the cigarette.

The invention has simple and mild process conditions, can realize the production of heat-not-burn reconstituted tobacco leaf cigarettes, has high production efficiency, and has great industrial application prospects in electric heating and charcoal heating new tobacco products.

Description of drawings

Fig. 1 is the structural representation of the heat-not-burn cigarette of the present invention;

Fig. 2 is the measurement schematic diagram of the amount of cut tobacco dropped from the end of the heat-not-burn cigarette;

Figure 3 is a total ion chromatogram of volatile components in 65μm PDMS/DVB solid-phase microextraction rolling method heat-not-burn reconstituted tobacco leaves.

Detailed ways

The present invention will be described in detail below with reference to specific embodiments.

Example 1

A preparation method of heat-not-burn cigarette, comprising the following technical steps:

(1) Preparation of raw materials: Prepare raw materials according to the percentage by mass: 50% of tobacco raw materials, 25% of glycerol as atomizer, 5% of solid adhesive (sodium alginate, potassium alginate, CMC, PAC), 5% of tobacco additives ( Solid calcium salt 3%, tobacco flavor 2%), fiber (wood fiber and coconut fiber, by mass ratio 4:1) 2%, 45 ℃ warm water 18%;

(2) Mixing and pulverizing dry materials: put the tobacco raw materials, solid adhesive and solid cigarette additives (calcium carbonate, calcium lactate, 2% and 1% by mass) into a low-temperature pulverizer in proportion, and pulverize to 200°C at 2°C. Mesh, mix evenly;

(3) The wet material is mixed and dispersed evenly: the fibers and 45°C warm water are poured into the material bucket in proportion, and while stirring at a high speed of 400r/min, 50KHz ultrasonic cavitation is used to assist the fibers to disperse and disperse more uniformly, and then add the above step 1 ) mass ratio of atomizer, continue 50KHz ultrasonic-assisted 400r/min high-speed stirring to uniformly disperse the fiber and atomizer, and at the same time slowly add wet material and tobacco flavor to the dry material powder mixed uniformly described in the above step 2). , stir at a high speed of 400r/min at the same time;

(4) Embossing rolling: the reconstituted tobacco leaves are obtained by 5 times of tanning roll pressing, and during the 6th rolling process, the reconstituted tobacco leaves are embossed and rolled with an embossing pressing roll, and then heated and dried at 70° C. to obtain a rolling method. Heat not burn embossed reconstituted tobacco leaves;

(5) Wrapping and wrapping: carry out wrapping and wrapping of the heat-not-burn embossed reconstituted tobacco leaves by the rolling method according to the cigarette process specification, and adopt twill embossed composite aluminum foil cigarette paper (wherein the thickness of the embossed aluminum foil is 10 μm, and the thickness of the cigarette paper is 100 μm), filter rods for cigarettes, etc. to be rolled and packaged, that is, the heat-not-burn cigarettes with improved production efficiency of the present invention, as shown in FIG. 1 .

The heat-not-burn reconstituted tobacco leaves have good strength, strong friction between the reconstituted tobacco leaves and the aluminum foil during rolling, good process continuity, and high production efficiency. Low-temperature cigarettes have uniform smoke release, large smoke volume, strong sense of satisfaction, and have the original aroma of tobacco, and the effect of simulating the sense of smoking is good.

Example 2

A preparation method of heat-not-burn cigarette, comprising the following technical steps:

(1) Preparation of raw materials: Prepare raw materials by mass percentage: 65% of tobacco raw materials, 11% of atomizer (glycerol, propylene glycol, and ethylene glycol are 6%, 3%, and 2% by mass respectively), solid adhesive 4 %, tobacco additive 3.5% (solid calcium salt 3%, tobacco spice mint 0.5%), fiber 1.5% (tobacco stem fiber and bagasse pulp are 1% and 0.5% by mass respectively), 55 ℃ warm water 15%;

(2) Mixing and pulverizing dry materials: put tobacco raw materials, solid adhesives and solid tobacco additives (calcium carbonate, calcium citrate, and calcium tartrate are respectively 1% by mass percentage) into a liquid nitrogen low-temperature pulverizer in proportion to 3 ℃ Pulverized to 240 mesh, and then mixed evenly by low-temperature high-speed pulverization;

(3) The wet material is mixed and dispersed evenly: the fibers and warm water are poured into the material bucket in proportion, and at the same time of high-speed stirring at 500r/min, 80KHz ultrasonic cavitation is used to assist the fibers to loosen and disperse more uniformly, and then add the above step 1) Mass Proportion of the atomizer, continue 80KHz ultrasonic-assisted 500r/min high-speed stirring to uniformly disperse the fiber and atomizer, and at the same time slowly add the wet material and tobacco flavor to the dry material powder mixed uniformly in the above step 2), Stir together at a high speed of 500r/min;

(4) Embossing and rolling: the reconstituted tobacco leaves are obtained after 6 times of tanning roll pressing, and during the 7th rolling process, the reconstituted tobacco leaves are embossed and rolled with an embossing roll, and then heated and dried at 60° C. to obtain a rolling method. Heat not burn embossed reconstituted tobacco leaves;

(5) Rolling packaging: carry out the rolling and packaging of the heat-not-burn embossed reconstituted tobacco leaves by the rolling method according to the cigarette process specification, and use disorderly embossed composite aluminum foil cigarette paper (wherein the thickness of the embossed aluminum foil is 8 μm, the thickness of the cigarette paper 120 μm), filter rods for cigarettes, etc. to be rolled and packaged, that is, the heat-not-burn cigarettes with improved production efficiency of the present invention.

The heat-not-burn reconstituted tobacco leaves have good strength, strong friction between the reconstituted tobacco leaves and the aluminum foil during rolling, good process continuity, and high production efficiency. Low-temperature cigarettes have uniform smoke release, large smoke volume, strong sense of satisfaction, with tobacco original fragrance and mint cool feeling, comfortable throat, and good effect of simulated smoking.

Example 3

A preparation method of heat-not-burn cigarette, comprising the following technical steps:

(1) Preparation of raw materials: Prepare raw materials according to the percentage by mass: 70% of tobacco raw materials, 10% of atomizer (glycerol and propylene glycol account for 8% and 2% by mass respectively), 3% of solid adhesive (rosin, chitosan) , Sodium glycerophosphate is equal mass ratio), cigarette additives 1% (calcium carbonate 0.5%, tobacco extract 0.5%), fiber 1% (mass ratio of wood pulp, bamboo pulp, etc.), 60 ℃ warm water 15%;

(2) Mixing and pulverizing of dry materials: put the tobacco raw material, solid adhesive and solid cigarette additive calcium salt in a liquid nitrogen low-temperature pulverizer in proportion, pulverize to 300 mesh at 4°C, and then mix uniformly through low-temperature and high-speed pulverization;

(3) The wet material is mixed and dispersed evenly: the fibers and warm water are poured into the material bucket in proportion, and while stirring at a high speed of 600r/min, 120KHz ultrasonic cavitation is used to assist the fibers to loosen and disperse more uniformly, and then add the above step 1) Mass Proportion of the atomizer, continue 120KHz ultrasonic-assisted 600r/min high-speed stirring to uniformly disperse the fiber and atomizer, and at the same time slowly add the wet material and tobacco flavor to the dry material powder mixed uniformly in the above step 2), Stir together at a high speed of 600r/min;

(4) Embossing and rolling: the reconstituted tobacco leaves are obtained by 8 times of tanning roll pressing, and during the 9th rolling process, the reconstituted tobacco leaves are embossed and rolled with an embossing pressing roll, and then heated and dried at 65° C. to obtain a rolling method. Heat not burn embossed reconstituted tobacco leaves;

(5) Rolling packaging: carry out the rolling and packaging of the heat-not-burn embossed reconstituted tobacco leaves according to the cigarette process specification, and adopt the embossed composite aluminum foil cigarette paper with staggered pattern (wherein the thickness of the embossed aluminum foil is 6 μm, and the thickness of the cigarette paper is 6 μm). The thickness is 80 μm), cigarette filter rods, etc. are wrapped in disordered shredded tobacco, which is the heat-not-burn cigarette with improved production efficiency of the present invention.

The heat-not-burn reconstituted tobacco leaves have good strength, strong friction between the reconstituted tobacco leaves and the aluminum foil during rolling, good process continuity, and high production efficiency. Low-temperature cigarettes have uniform smoke release, large smoke volume, strong sense of satisfaction, high smoke concentration, tobacco aroma, comfortable throat, and good effect of simulated smoking.

Test Example 1: Comparison of Application Effects

The heat-not-burn reconstituted tobacco leaves prepared by the rolling method in Examples 1-3 were compared with the heat-not-burn reconstituted tobacco leaves manufactured by the conventional rolling process. When the content of the agent is high, the distribution is uniform, the surface is not sticking, and the fiber content is increased, and the reconstituted tobacco is evenly pulverized, the strength of the reconstituted tobacco is improved, the processing resistance is good, the strength improvement rate is as high as 35.71%, and the production efficiency is improved compared to the control. The smoking rate is more than 25%; the smoking is smoother, the satisfaction is strong, and the tobacco has the original aroma, and the sensory effect of simulated smoking is better;

(1) Intensity detection of the reconstituted tobacco leaf of the heat-not-burn cigarette of the present invention

The strength is an important indicator for the roll forming of reconstituted tobacco leaves with high atomization amount.

For the detection method, refer to GB/T 12914-2008 Determination of Tensile Strength of Paper and Cardboard.

Detection principle: Under the condition of constant speed stretching, the sample of specified size is stretched to break, and its tensile strength is measured. If desired, the elongation of the specimen can be measured and its maximum tensile strength recorded.

Instrument: TTM-30 computer tensile testing machine.

Grips: Two, in order to clamp the specimen of the specified width, each clamp should firmly clamp the full width of the specimen along a straight line, and should not damage or slide the specimen. The collet shall be equipped with means to adjust the clamping force.

Test steps:

1. Cut the sheet into 15mm wide and 200mm long.

2. Measure according to GB/T 12914.

3. The test samples that are not firmly adhered, fall off, and are not integrally broken are excluded from the measurement results.

The test results are as follows:

Table 1 Intensity of heat-not-burn reconstituted tobacco leaves by rolling method

sample Gram weight g/m² Tensile strengthN/m Elongation at break% Example 1 184 312 1.1 Example 2 201 328 1.2 Example 3 220 380 1.3 control 160 280 0.8

(2) Sensory evaluation of heat-not-burn cigarettes of the present invention

The sensory quality of the heat-not-burn cigarette of the present invention was compared and evaluated with its reference. The reference sample cigarette was prepared from heat-not-burn reconstituted tobacco leaves and glossy composite aluminum foil cigarette paper by ordinary rolling method. The results are shown in Table 2.

Table 2 Sensory evaluation of heat-not-burn cigarettes of the present invention

The results show that the heat-not-burn cigarette of the present invention has a large amount of smoke, a uniform release, a strong sense of satisfaction, and the original aroma of tobacco, and the sensory effect of simulated smoking is good.

(3) Test comparison of cut tobacco drop test at the end of heat-not-burn cigarette of the present invention

The current method for testing cigarette end drop, ISO3550-1 "Determination of cigarette end drop - Part 1: Rotating cage method" is used to measure the end drop of heat-not-burn cigarettes.

Apparatus: YDZ-II cigarette end shredding measuring instrument (vibration method), E44 cigarette end shredding measuring instrument (rotating cage method).

Method: According to the requirements of ISO3402, the sample should be equilibrated in the environment of (22+1)℃ and RH(60+3)% for more than 48h and within 10d.

Parameter setting: The ISO3550-2 measuring instrument rotates at a speed of 60rpm and rotates for 2min.

Determination of shredded tobacco from the end of cigarettes: The test was repeated 40 times for each cigarette sample using ISO3550-2. The test results are shown in Table 3 and Figure 2.

Table 3 Determination of the amount of shredded tobacco dropped from the end of heat-not-burn cigarettes

sample The amount of silk at the end of the cigarette (mg/cig) Example 1 8 Example 2 7 Example 3 6 control 10

The results are shown in Table 3 and Figure 2. Compared with the control, the amount of shredding at the end of the heat-not-burn cigarette of the present invention is reduced by 20-40%.

Test Example 2: HS-SPME-GC/MS Analysis of Volatile Chemical Components of Heat-Not-Burn Reconstituted Tobacco Leaves Using the Improved Rolling Process of the Present Invention

The heat-not-burn reconstituted tobacco leaves prepared by the improved rolling method of the present invention were detected and analyzed by gas mass spectrometry using a solid-phase microextraction head of 65 μm PDMS/DVB (polydivinylbenzene).

1 Materials and methods

1.1 Medicines and Instruments

The heat-not-burn reconstituted tobacco leaves prepared by the improved rolling method of the present invention;

Digital display constant temperature water bath AHYQ HH-6: Changzhou Aohua Instrument Co., Ltd.; balance CP2202S-OCE: Sartorius AG Germany; manual SPME injection handle, manual extraction fiber head (65μm PDMS/DVB polydivinylbenzene, 15mL special top Empty extraction sample bottle: American Supelco company; TRACE GC Ultra-DSQ II gas chromatography/mass spectrometry (GC/MS) combined instrument: American Thermoelectric Technology Co., Ltd.

1.2 Methods

1.2.1 SPME conditions

Weigh 1 g of the heat-not-burn reconstituted tobacco leaf sample prepared by the improved rolling method of the present invention, cut it into pieces with a diameter of 0.2 cm, place it in a 15 mL special headspace extraction sample bottle, insert the aged extraction head, and pre-heat it at a certain temperature. Equilibrate for 10min, and extract for a certain period of time. Aging of extraction head: Aging of injection port at 250℃ for 30min.

1.2.2 GC/MS analysis conditions

1.2.1.1 Chromatographic conditions

The initial temperature of the column was 50 °C, maintained for 2 min, heated to 180 °C at a rate of 8 °C/min, held for 1 min, and then heated to 280 °C at a rate of 18 °C/min, maintained for 30 min; the carrier gas was helium (He, purity 99.99 %), constant flow mode, flow rate is 1.0mL/min; split injection mode, split ratio 1:10, no solvent delay; injection port temperature 250°C.

1.2.1.2 Mass spectrometry conditions

Ionization method: EI source; electron energy: 70eV; multiplier tube voltage: 1.2kV; ion source temperature: 230℃; quadrupole temperature: 150℃; interface temperature: 280℃, transmission line 280℃; scanning range: 33m/z～ 350m/z. The NIST standard spectral library was used for search and analysis, and the relative percentage of compounds was calculated according to the peak area normalization method.

2 Results and Analysis

Taking the heat-not-burn reconstituted tobacco leaves prepared by the improved rolling method of the present invention as the research object, the extraction head 65 μm PDMS/DVB was used for HS-SPME-GC-MS detection and analysis. The total ion chromatogram is shown in Figure 3, and the volatile chemical components Mainly concentrated in 14 ~ 25min, see Table 4 for details. Table 4 HS-SPME-GC/MS of the volatile components of the heat-not-burn reconstituted tobacco leaves prepared by the improved rolling method of the present invention

analyze

As shown in Table 4 above, the heat-not-burn reconstituted tobacco leaves prepared by the improved rolling method of the present invention were detected by headspace-solid phase microextraction-gas chromatography mass spectrometry, and 84 volatile components were identified, and the total relative percentage was 97.91 %, including 10 kinds of alkenes (64.15%), 19 kinds of esters (9.41%), 19 kinds of ketones (7.45%), 11 kinds of alcohols (1.84%), 3 kinds of acids (0.45%), 3 kinds of aldehydes species (0.34%), 2 kinds of alkanes (0.21%), and 19 kinds of other heterocyclic compounds. In terms of single component, the highest relative percentage is neophytadiene (63.74%). Neophytadiene is a C20 cluster isoprene, which has the highest content in the neutral volatiles of tobacco, which is the highest in tobacco leaves. An important aroma substance, this component is formed by the degradation of chlorophyll contained in tobacco leaves during the ripening and modulation process to form leaf alcohol, which is further dehydrated by leaf alcohol. Neophytadiene itself has a fresh aroma and is less irritating, while chlorophyll and phytol have green miscellaneous gas. During the modulation process, as chlorophyll and phytol are converted into neophytadiene, the green miscellaneous gas of tobacco leaves. Eliminated, resulting in a clear aroma. Neophytadiene can directly enter the smoke when tobacco is burned, and has the effect of reducing irritation, alcohol and smoke. As a carrier for capturing aroma substances in smoke aerosols, neophytadiene has the ability to carry volatile aroma substances and aroma components in tobacco leaves into smoke, so it is also an important aroma enhancer for tobacco leaves; the second is á-nicotine. (11.73%), an important active ingredient in tobacco, with a pungent smell and acrid taste, giving people a sense of satisfaction; again, methyl palmitate (3.61%); fourth, geranyl acetone (1.94%) , and the fifth is methyl linolenic acid (1.92%). All these aldehydes, alcohols, ketones, esters, alkanes, heterocyclic compounds, aromatic hydrocarbons and other tobacco aroma components bring the heat-not-burn reconstituted tobacco by rolling method to rich and harmonious tobacco flavor, good satisfaction, and simulated cigarettes The suction effect is good.

The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, All should be included within the protection scope of the present invention.

Claims (10)

1. a preparation method of heat-not-burn cigarette, is characterized in that comprising the steps: (1) Preparation of raw materials: Prepare raw materials according to the percentage by mass: 50-70% of tobacco raw materials, 10-25% of atomizer, 3-10% of solid adhesive, 1-10% of cigarette additives, and 1-10% of fiber, Warm water 15-35%; (2) Mixing and pulverizing of dry materials: put the tobacco raw materials, solid adhesive and solid cigarette additive calcium salt in a low-temperature pulverizer in proportion, and pulverize to 40 meshes to 300 meshes at a low temperature, and at this time, they are uniformly mixed by low-temperature and high-speed pulverization; (3) The wet material is mixed and dispersed evenly: the fibers and warm water are poured into the material bucket in proportion, and at the same time of high-speed stirring, ultrasonic cavitation is used to assist the fibers to loosen and disperse more uniformly, and then add the above-mentioned step (1) mass ratio. Atomizer, continue ultrasonic-assisted high-speed stirring to disperse the fiber and the atomizer evenly, and at the same time slowly add the wet material and tobacco flavor to the uniformly mixed dry material powder in the above step (2), and stir together at a high speed to be uniform; (4) Embossing and rolling: the reconstituted tobacco leaves are obtained by rolling for 3 to 9 times. In the last rolling process, the reconstituted tobacco leaves are embossed and rolled with an embossing pressing roller, and then heated and dried to obtain a thermally inert tobacco by rolling. Burn embossed reconstituted tobacco leaves; (5) wrapping and wrapping: carry out wrapping and wrapping of the heat-not-burn embossed reconstituted tobacco leaves by the rolling method according to the cigarette process specification, and adopt the embossed composite aluminum foil cigarette paper and the filter rod for cigarettes for wrapping and wrapping, namely the present invention. Heat-not-burn cigarettes that improve productivity. 2 . The method for preparing heat-not-burn cigarettes as claimed in claim 1 , wherein the tobacco raw material is one of tobacco leaves and tobacco stems or a mixture thereof. 3 . 3. The preparation method of heat-not-burn cigarette as claimed in claim 1, it is characterized in that: described cigarette additive is tobacco flavor and calcium salt, and described calcium salt is calcium carbonate, calcium lactate, calcium citrate, One or a combination of calcium tartrate. 4. The method for preparing heat-not-burn cigarettes according to claim 1, wherein the low-temperature pulverization is 0-4°C, 40-300 mesh. 5. The preparation method of heat not burn cigarette as claimed in claim 1, is characterized in that: described solid adhesive is sodium alginate, potassium alginate, carboxymethyl cellulose, polyanionic cellulose, polyvinyl alcohol, One or a combination of casein gum, rosin, dextrin, chitosan, and sodium glycerophosphate. 6. The preparation method of heat-not-burn cigarette as claimed in claim 1, it is characterized in that: described fiber is one or more mixing in wood pulp, tobacco rod fiber, bagasse pulp, bamboo pulp, coconut fiber . 7 . The method for preparing heat-not-burn cigarettes according to claim 1 , wherein the temperature of the warm water is 30-60° C. 8 . 8 . The method for preparing heat-not-burn cigarettes according to claim 1 , wherein the atomizing agent is a mixture of one or more of glycerol, propylene glycol and ethylene glycol. 9 . 9 . The method for preparing heat-not-burn cigarettes according to claim 1 , wherein the embossed composite aluminum foil cigarette paper is twill or disorderly pre-embossed aluminum foil paper, wherein the embossed aluminum foil has a thickness of 1 to 10 . 19 μm, and the thickness of the cigarette paper is 20 to 200 μm. 10. A heat-not-burn cigarette prepared by the method according to any one of claims 1-9 is used in electric heating or carbon heating low temperature cigarettes.

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