CN113528240A - Preparation and application of novel spice with smoke regulation and control function for heating cigarette - Google Patents
Preparation and application of novel spice with smoke regulation and control function for heating cigarette Download PDFInfo
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- CN113528240A CN113528240A CN202110791676.7A CN202110791676A CN113528240A CN 113528240 A CN113528240 A CN 113528240A CN 202110791676 A CN202110791676 A CN 202110791676A CN 113528240 A CN113528240 A CN 113528240A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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Abstract
The invention belongs to the technical field of heated cigarettes, and particularly relates to a preparation method and application of novel spice with a smoke regulation function for heated cigarettes. The preparation method comprises the following steps: fermenting the mixed raw material of Zimbabwe flue-cured tobacco and tea leaves by using bacillus at 25-30 ℃, and after 5-10 days, taking out a fermentation substrate, and extracting the fermentation substrate by using an ethanol solution with the concentration of 60-80 wt% to obtain a crude extract; and filtering the crude extract by using an ultrafiltration membrane with the molecular weight of 1-3 ten thousand at the room temperature under the operating pressure of 0.16-0.18 MPa to obtain the novel spice. The invention utilizes the microbial fermentation technology and the novel extraction and separation technology to change the chemical components of the tobacco leaves and the tea leaves, extracts and separates novel latent fragrant substances from the tobacco leaves and adds the substances into the heated cigarette, thereby effectively reducing the release amount of harmful substances in the smoke of the heated cigarette, improving the smoking quality of the heated cigarette, enriching and plump the smoke, covering miscellaneous gas and wood gas and ensuring that the taste is more mellow.
Description
Technical Field
The invention belongs to the technical field of heated cigarettes, and particularly relates to a preparation method and application of a heated cigarette spice with a smoke regulation function.
Background
The literature reports that more than 6000 chemical compositions are identified in the traditional cigarette smoke, the chemical compositions are mainly generated by directly transferring related components in tobacco or through pyrolysis and thermal synthesis reactions, and part of harmful components can be pyrolyzed or thermally synthesized under high-temperature (combustion) conditions, so that the following can be known: the emission of harmful components in the smoke can be obviously reduced by reducing the heating or combustion temperature. In addition, sidestream smoke generated after the traditional cigarette is ignited (mainly smoke escaping from the smoldering cigarette ignition end in the smoking interval period) can cause non-people to passively smoke, and the unpleasant feeling of the non-smoking people is caused.
Smokers desire to smoke cigarettes with lower harm, non-smoking people want to avoid the harm of passive smoking, and the reasons boost the generation of novel herbal products. Currently, the new types of tobacco products appearing on the market include: heating cigarettes, smokeless tobacco products, and electronic cigarettes.
The heating of non-burning tobacco product (also known as cigarette) is a new type of tobacco product which is produced by heating tobacco material with special heating source, and the nicotine and flavor substance in the tobacco material are volatilized to produce smoke to meet the requirements of smokers. Different from the traditional cigarette, the cigarette is heated without being ignited, so that the harmful components generated by high-temperature combustion and cracking of tobacco are reduced as much as possible. But the tobacco substances are not ignited, a large amount of flavor components generated by thermal synthesis and thermal cracking are reduced, and the problems of poor oral comfort, bitter feeling, insufficient aroma and the like are inevitably generated in the process of heating cigarettes for smoking.
At present, the flavor is mainly added into the heated cigarette to enrich the taste of the smoke. The tobacco part of the heated cigarette is always in a heated state (about 200-350 ℃) in the smoking process, and the additional essence and flavor are easy to volatilize and completely disappear in the first mouth and the second mouth, so that the problems of uneven taste, unstable quality and the like are caused. The taste accompanied with strong flavor and chemical smell during smoking has certain gap with the smoking quality of cigarettes. And some flavors and fragrances added in the traditional cigarette, such as macromolecular organic substances, such as raspberry ketone, thymol and dihydrocoumarin, have boiling points of more than 200 ℃, and can generate fragrance components similar to flowery scent, fruity fragrance and bean fragrance only after high temperature, and can not be completely volatilized in a heating temperature range of the heated cigarette and can not bring expected effects, so that the flavors and fragrances can not be completely transplanted into the heated cigarette for application.
Disclosure of Invention
Tobacco fermentation, also known as tobacco aging, is a key process performed after tobacco is baked (or aired) and threshed and redried, under artificial intervention or natural conditions. The tobacco has larger change of chemical components after being roasted, the sensory quality is improved, but the tobacco is still not suitable to be directly used as a raw material of a tobacco product because of large irritation, rough aroma, heavy miscellaneous gas and strong astringent taste, and the quality defects can be obviously improved by fermentation. The fermentation methods reported at present include natural fermentation, artificial fermentation, enzymatic fermentation and microbial fermentation. The microorganism fermentation method is a method for accelerating the fermentation speed of tobacco by artificially inoculating microorganisms under certain conditions, and in the fermentation process of the tobacco, the microorganisms grow and metabolize to degrade macromolecular substances in the tobacco and generate lipid, acid and other small molecular substances, so that the chemical components of the tobacco are improved.
At present, the microbial technology is mainly applied to the field of traditional cigarettes, and comprises the steps of shortening tobacco mellowing time by microbial fermentation, removing special chemical components of tobacco by microbial fermentation and the like. However, the invention utilizes the microbial fermentation technology to achieve the technical effect of regulating and controlling the smoke of the heated cigarette, thereby achieving the purposes of reducing harm and increasing flavor.
In order to improve the smoking quality of the heated cigarette and further achieve the aim of reducing harmful substances in the smoke. The invention extracts and separates the mixed raw materials of Zimbabwe tobacco leaves and tea leaves after fermentation, changes the chemical components of the tobacco leaves and the tea leaves, extracts and separates novel latent fragrant substances from the mixed raw materials, and adds the substances into the heated cigarettes, thereby effectively reducing the release amount of harmful substances in the smoke of the heated cigarettes, improving the smoking quality of the heated cigarettes, enriching and plump smoke, covering miscellaneous gas and wood gas and ensuring that the taste is more mellow.
The invention provides a preparation method and application of novel spice with smoke regulation and control function for heated cigarettes, wherein the preparation method comprises the following steps:
fermenting the mixed raw material of the Zimbabwe flue-cured tobacco leaves and the tea leaves which are naturally alcoholized for 1-2 years at 25-30 ℃ by using bacillus, and taking out a fermentation substrate after 5-10 days;
then extracting a fermentation substrate by using an ethanol solution with the concentration of 60-80 wt% to obtain a crude extract;
and filtering the crude extract by using an ultrafiltration membrane with the molecular weight of 1-3 ten thousand at the room temperature under the operating pressure of 0.16-0.18 MPa to obtain the novel spice.
Preferably, the mixed raw materials of the Zimbabwe flue-cured tobacco leaves and the tea leaves are crushed and sieved by a sieve with no less than 200 meshes.
Preferably, the tea leaves are one or more of black tea, green tea or dark tea.
Preferably, the mass ratio of the Zimbabwe flue-cured tobacco leaves to the tea leaves is 10: 1-1: 1.
Preferably, the bacillus is provided in the form of a bacillus liquid, and the concentration of the bacillus liquid is not less than 1010CFU/mL。
Preferably, the bacillus liquid is provided in the form of: the tobacco leaf spraying agent is sprayed on tobacco leaves and tea leaves, and the spraying proportion is 1-10 wt% (mass percentage of the tobacco leaves).
The second aspect of the invention provides the use of the novel spice of the first aspect, wherein the novel spice is added into the cut tobacco of the heated cigarette in a flavoring and feeding manner in a proportion of 1-5 wt% for smoking.
The novel spice is added into the heated cigarette leaf group to regulate and control the smoke of the heated cigarette, so that the release amount of harmful substances in the smoke of the heated cigarette is effectively reduced, and particularly, the reduction rate of the specific nitrosamine in the tobacco is not lower than 50%. Meanwhile, the fragrant substances in the smoke are increased, the smoking quality of the heated cigarette is improved, the smoke is enriched and full, miscellaneous gases and wood gases are covered, and the taste of the cigarette is more mellow.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention uses specific Zimbabwe flue-cured tobacco leaf and tea leaf raw materials, adopts microbial fermentation technology, changes the chemical compositions of the tobacco leaf and the tea leaf, leads the pectin, protein, amino acid and other components in the raw materials to have the functions of decomposition, degradation, oxidation, reduction, polymerization, coupling, conversion and the like, and forms complex low molecular compounds which comprise various fragrant compounds such as alcohols, aldehydes, ketones, acids, esters, phenols, furans, pyrazines, pyridines, terpenes and the like, and the fragrant substances improve the smoking quality of the heated cigarette, enrich and plump smoke, cover up miscellaneous gas and wood gas, and lead the taste to be more mellow. And the thermal weight loss experiment shows that the heated cigarette added with the novel spice can be largely pyrolyzed to generate volatile fragrant substances in the heating temperature range (compared with a blank sample).
2. With the increasing attention of the public on smoking and health problems, the reduction of the release amount of harmful ingredients in cigarette smoke has important practical significance. The invention uses specific tobacco leaf and tea raw materials, and adopts the technical combination of microbial fermentation, extraction, separation and the like, thereby changing the chemical components of the raw materials. The prepared novel spice is added into the heated cigarette, so that harmful ingredients such as nitric oxide, polycyclic aromatic hydrocarbon, N-nitrosamine, phenols and the like in the smoke of the heated cigarette can be selectively reduced, and the aim of reducing harm more obviously is fulfilled.
3. In particular, the invention uses specific tobacco leaves and tea raw materials, adopts technical combinations of microbial fermentation, extraction, separation and the like to prepare novel spices, and adds the novel spices into the heated cigarette, thereby solving the problems that the flavors and spices added in the process of smoking the heated cigarette are easy to volatilize and exhaust in the first mouth and the second mouth, so that the taste is not uniform, the quality is unstable, and the smoking is accompanied with stronger flavors and spices and chemical smell taste. The aroma of the heated cigarette is stably and uniformly released in the smoking process, and a certain characteristic aroma style is given to the product, so that the cigarette is a novel high-stability novel spice.
4. The method directionally enriches the tobacco components of Zimbabwe by a certain process means, thereby realizing the supplement and substitution of tobacco with a certain grade, a certain quality or a certain style, and playing an important role in relieving the contradiction of high-quality raw material requirements and improving the product quality.
5. The novel spice is prepared by using specific tobacco leaves and tea raw materials and adopting the technical combination of microbial fermentation, extraction, separation and the like, the extract is derived from natural materials, is not limited by a list of additives for cigarettes, and has guaranteed safety.
Drawings
Figure 1 is the total ion flow diagram of the novel perfume obtained in example 1.
Figure 2 is a total ion flow graph of the volatile components of the commercially available zimbabwe tobacco extract of example 1.
Fig. 3 is a Thermogravimetric (TG), Differential Thermal Gravimetries (DTG) -temperature (Temp) curve of a control of application example 4 pyrolyzed in air atmosphere.
Fig. 4 is a Thermogravimetric (TG), Differential Thermal Gravimetries (DTG) -temperature (Temp) curve of a novel fragrance addition sample obtained in application example 4 pyrolyzed in an air atmosphere.
FIG. 5 is a thermal cracking chromatogram of a control sample of application example 5 at 350 ℃.
FIG. 6 is a thermal cracking chromatogram at 350 ℃ of a novel flavor additive sample obtained in application example 5.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited to these examples. The experimental methods not specified in the examples are generally commercially available according to the conventional conditions and the conditions described in the manual, or according to the general-purpose equipment, materials, reagents and the like used under the conditions recommended by the manufacturer, unless otherwise specified. The starting materials required in the following examples and comparative examples are all commercially available.
Example 1
A preparation method of novel fractions with smoke regulation and control functions and application of the novel fractions in cigarette heating, wherein the preparation method comprises the following steps:
respectively crushing the cured tobacco leaves and the tea leaves which are naturally alcoholized for 2 years, sieving the crushed tobacco leaves and the tea leaves with a 200-mesh sieve, mixing the crushed tobacco leaves and the tea leaves according to the mass ratio of 5:1, fermenting the mixed raw materials by using bacillus at 25 ℃, and taking out a fermentation substrate after 7 days;
then extracting a fermentation substrate by using an ethanol solution with the concentration of 70 wt% to obtain a crude extract;
filtering the crude extract with ultrafiltration membrane with molecular weight of 3 ten thousand at room temperature and operating pressure of 0.18MPa to obtain novel perfume.
The method for obtaining the bacillus can be used for purchasing conventional bacillus in the market or self-culturing. The bacillus of this example was purchased from the market. Providing Bacillus in the form of Bacillus liquid, and preparing to concentration of 1.5 x 1010CFU/mL of Bacillus strain solution. Then spraying the bacillus liquid on the tobacco leaves and the tea leaves,the spraying proportion is 5 wt% (the mass percentage of the bacillus liquid in the tobacco leaf).
Application example 1
Novel spice stability research
The novel perfume product is not easy to generate the phenomena of putrefaction and deterioration and the like. After the sample is placed for 6 months, the phenomenon of odor change does not occur to the sample, the appearance state is stable, and the quality of the sample is still stable after the sample is placed for 12 months, so that the quality guarantee period is determined to be 12 months. The reason for this is related to the raw materials and extraction process of the novel perfume.
Second, measurement of physical and chemical indexes
The appearance, clarity, relative density, miscibility (25 ℃), acid value, total amount of volatile components and the like of the novel perfume are measured according to the industry standard YC/T145.1-YC/T145.9. The heavy metal elements Pb and As in GB/T5009.74-2003 and GB/T5009.76-2003 are determined. XDS and HZS were determined in accordance with Q/HY.CJ.202-2009.
The specific results of the measurement of the physicochemical indexes of the novel spice are shown in the table 1, the detection results show that the product has better appearance quality and dissolution performance, and the contents of heavy metals Pb and As, XDS and HZS are also within the range of national food safety.
Novel physical Properties of fragrances
TABLE 1 novel physicochemical indices of spices
Detecting items | Novel perfume |
Appearance and clarity | Light yellow clear liquid |
Relative density d20 20 | 1.040±0.008 |
Refractive index nD 20 | 1.434±0.008 |
Degree of miscibility (25 ℃ C.) | 1 volume of sample was dissolved in 20 volumes of 70% ethanol solution |
Acid value | 6.8±2.5 |
Total amount of volatile component (m/m) | 88±4 |
Pb content (mg/kg) | ≤10.0 |
As content (mg/kg) | ≤3.0 |
XDS(mg/kg) | <100 |
HZS(mg/kg) | Is free of |
Analysis of fragrant components
The aroma components in the extract are measured by GC-MS according to the tobacco industry standard. Refer to the determination of aroma components of tobacco and tobacco products and the simultaneous distillation extraction-gas chromatography-mass spectrometry combination TCJC-ZY-IV-014-2012.
GC-MS analysis test conditions: a chromatographic column: HP-5MS (60 m.times.0.132 mm.times.0.125 μm); carrier gas: he; flow rate: 1 mL/min; sample introduction temperature: 240 ℃; interface temperature: 250 ℃; mass spectrum scanning range: 35 to 455 amu; an ion source: EI source, electron energy: 70 eV. According to the analysis and test conditions, the volatile components are subjected to GC-MS analysis, and the mass fraction of each compound is determined as an area normalization method. The qualitative analysis of the compound is to confirm the chemical components in the mass spectrum information obtained by GC-MS combination through comparison and analysis of a Wiley and NISt 98 spectral library and a standard spectrogram by a computer.
The total ion flow diagram of the volatile components of the commercially available Zimbabwe tobacco extract is shown in figure 2, the total ion flow diagram of the volatile aroma components of the novel spice product is shown in figure 1, and the specific analysis result is shown in table 2.
TABLE 2 comparison of the novel flavor product with the main ingredient of the commercially available Zimbabwe tobacco extract (peak area:%)
The detection results show that after the biological fermentation Zimbabwe-like characteristic cigarette cream obtained by biological fermentation treatment is subjected to membrane separation and refining, the main aroma components of the biological fermentation Zimbabwe characteristic cigarette cream are megastigmatrienone (A, B, C, D), beta-damascenone, dihydroactinidiolide, 3-oxo-alpha-ionol and the like which are obviously higher than those of the commercially available Zimbabwe tobacco extracts, and the biological fermentation Zimbabwe-like characteristic cigarette cream has more aroma components than the Zimbabwe tobacco extracts, so that the Zimbabwe tobacco extract forming the baking aroma of flue-cured tobacco has the advantage that the Zimbabwe characteristic cigarette cream is more than 20 times that of the Zimbabwe tobacco extracts.
Application example 2
The novel flavor obtained in example 1 was added to cigarette shreds of Yunan Zhongyan cigarette in a flavoring and feeding manner in an amount of 2 wt% of the novel flavor/mass of cigarette) to conduct a smoke aerosol analysis test. The heated cigarette without adding the novel flavor under the same conditions was used as a blank.
The aerosol inspection basis of the heated cigarette added with the novel spice and the blank sample is respectively as follows:
GB/T23203.1-2013; GB/T19609-2004; GB/T23356-; GB/T21130-2007; GB/T23355-2009; YC/T253-2019; YC/T255-; YC/T254-; YC/T377-2019; Q/CTQ5-2010 (laboratory method for determination of tobacco-specific nitrosamines in total particulate matter of mainstream smoke). The results are shown in Table 3.
TABLE 3 comparison of the principal ingredients of the heated cigarette aerosols for the novel flavor and blank
As can be seen from Table 3, the novel spice obtained by fermenting, extracting and separating specific tobacco leaves and tea leaves by adopting a biological fermentation technology can change the chemical components of the raw materials, and can be added into a heated cigarette for smoking so as to selectively reduce harmful components such as aldehydes, nitrogen oxides, polycyclic aromatic hydrocarbons, N-nitrosamine, phenols and the like in the smoke of the heated cigarette. Particularly, the effect on reducing the tobacco specific nitrosamine is obvious, NNN is reduced by 64 percent, NNK is reduced by 66 percent, and NAT is reduced by 61 percent.
Application example 3
The novel flavor obtained in example 1 was added to cigarette shreds heated in Yunan tobacco in a flavoring and casing manner at 1 wt%, 2 wt% and 3 wt% (wt%: novel flavor mass/cigarette mass) to conduct tests.
The novel spice obtained in the embodiment is applied to a heated cigarette for evaluation, and the evaluation standard is QYNZY.J07.604-2017 part 4 sensory technical requirements of an electric heating non-combustible cigarette, and the evaluation result is shown in Table 4.
TABLE 4 results of the test
From the test results it can be seen that: the novel spice is added into the formula of the cigarette heated by the Yunnan Zhongyan cigarette in a feeding mode according to the proportion of 2 wt%, so that the richness of the cigarette fragrance of the heated cigarette is further increased, the fragrance is sufficient, the sweet feeling is increased, no wood gas and miscellaneous gas exist, and the baking fragrance is prominent.
Application example 4 thermal analysis
The novel spice product obtained in example 1 is added into cigarette tobacco shreds heated by Yunan tobacco in a flavoring and feeding mode at a proportion of 2 wt% to prepare a raw material, and a blank leaf group without any novel spice is used as a control.
Before sample analysis, a thermogravimetric analyzer is set to be kept for 10min at 800 ℃ so as to completely discharge impurities in the furnace body. The sensitivity of the thermobalance was 1. mu.g, with an empty crucible as reference. A typical heated cigarette tobacco material (5.00. + -. 0.05) mg was weighed into a hot platinum crucible. At the air flow rate of 80mL/min, the temperature rising programs are respectively as follows: 30 ℃ 10 ℃/min 800 ℃ (10 min).
FIG. 3 is a thermal analysis curve of a control sample at a temperature rise rate of 10 ℃/min and an air flow rate of 80 mL/min. As can be seen from the figure, the thermal weight loss is divided into four stages: firstly, the weight loss is 19.62 percent at the temperature of 50-237 ℃, which is a first weight loss stage; 243-352 ℃ weightlessness is 28.96 percent, which is the second weightlessness stage and has the most weightlessness; and 382 and 487 ℃ weight loss is 25.14 percent, which is a third weight loss stage. 568 and 734 ℃ weight loss of 4.74 percent are the fourth weight loss stage.
FIG. 4 is a thermal analysis curve of the novel flavor additive sample obtained in example 1 under the same conditions. As can be seen from fig. 2, the thermal weight loss is divided into four stages: 103-202 ℃ weight loss is 8.68 percent, which is a first weight loss stage; 225-370 ℃ weight loss of 35.50 percent is the second weight loss stage, the weight loss is the most and more violent in the stage, a larger peak is also presented on the DTG curve, and the weight loss reaches 0.205mg/min at 300.72 ℃; 391-491 ℃ weight loss is 26.28 percent, which is the third weight loss stage, the weight loss is most violent in the stage, a large peak is also shown on the DTG curve, and the peak reaches 0.922mg/min at 441.00 ℃. 592 and 723 ℃ weight loss of 4.06 percent, which is the fourth weight loss stage. Thermogravimetric analysis was performed on the samples and control samples to which the novel perfume of example 1 was added, and the results showed that:
(1) the sample added with the novel perfume is the same as a control sample, the thermal weight loss is divided into four stages, the thermal weight loss is larger in the second and third stages, the weight loss is stronger in the second weight loss stage, a larger peak is presented on a DTG curve, the weight loss is most violent in the third weight loss stage, and a large peak is presented on the DTG curve.
(2) The weight loss temperature range of the comparison sample in the first stage is 50-237 ℃, the first stage is delayed to 103-202 ℃ after the novel spice is added, and the thermal stability of the micromolecule substance which is very volatile is increased. The second stage is a most main weightlessness section in a heating temperature range of the heated cigarette, the weightlessness is changed from 28.96% at the temperature of 352 ℃ of a comparison sample to 35.30% at the temperature of 370 ℃ of the sample, the temperature range is wider, the pyrolysis substance is more, after the novel spice is added, more substances are pyrolyzed and volatilized in the working temperature range of the heated cigarette, the smoke chemical substance is added, the smoke substance is fuller and richer, the characteristic fragrance of the tobacco is increased, the fragrance is rich and elegant, the texture is good, and the fragrance increasing effect is maximally played.
Application example 5 thermal cracking study
(1) Preparation of samples and controls
The low-temperature spice obtained in example 1 is diluted to 5 wt%, and the diluted material is added into cut tobacco of cigarette heated by Yunnan Zhongyan tobacco in a flavoring and feeding manner according to the proportion of 2 wt% to prepare a raw material, and meanwhile, a blank leaf group without any low-temperature spice is used as a control sample. The electric heating temperature for heating the cigarette is lower than 350 ℃, so the experiment is carried out in the temperature rise range of 50-350 ℃ for carrying out the research on the thermal cracking behavior.
(2) GC-MS conditions
Instrument GC/MS (HP6890N/5973N, Agilent, USA)
Chromatographic mass spectrum conditions: capillary column: HP-5MS (30m 0.25mm 0.25m), injection port temperature: 240 ℃, carrier gas: he, flow rate: 1mL/min, GC-MS interface temperature: temperature gradient at 250 ℃ is as follows: 50 ℃ (1min) -2 ℃/min-100 ℃ (1min) -8 ℃/min-260 ℃ (5min), ion source: EI source, electron energy: 70eV, scanning range: 35-455amu, standard atlas library: NIST, willey spectral library.
(3) Conditions of thermal cracking
The instrument comprises the following steps: PYROPROBE 2000(CDS, USA)
Conditions are as follows: initial temperature: temperature rise rate at 30 ℃: 20.00 ℃/ms, cracking temperature: 350 ℃, duration: 10s, cracking atmosphere: 10% oxygen, atmospheric air or nitrogen (gas flow: 2.5 ml/s).
(4) Solid phase micro-extraction conditions
When the incense raw materials and the additives are subjected to thermal cracking in an atmospheric environment, a black extraction head is adopted to extract a cracking product from a self-designed cracking bottle, the extraction time is 10min, the extraction temperature is 70 ℃, and then an SPME sample injection needle is inserted into a gas chromatography high-temperature vaporization chamber for desorption, wherein the desorption time is 2 min.
(5) Test method
Weighing a certain amount of sample (about 2mg) and adding the sample into a quartz tube special for cracking, then placing the quartz tube into a heating wire of a thermal cracking instrument, respectively carrying out thermal cracking at three set temperatures of 350 ℃ in different cracking atmospheres, placing a solid phase micro-extraction head into a self-designed cracking bottle to extract a cracking product, wherein the extraction time is 10min, the extraction temperature is 70 ℃, then inserting an SPME sample injection needle into a high-temperature vaporizing chamber of a gas chromatograph for desorption for 2min, and separating and identifying the cracking product in the gas chromatograph/mass spectrometer (GC/MS) to carry out standard library retrieval, wherein if the matching degree of the cracking product is not particularly specified to be more than 60.
The comparison and the heating cigarette thermal cracking chromatograms with the low-temperature spice of the invention are shown in figures 5 and 6. The substances detected are shown in Table 5. After the low-temperature spice is added, the quantity of pyrolysis substances is increased compared with that of a reference sample, wherein 20 substances, mainly furfural, 5-methyl-2-furfural, nicotine and the like, are detected by the reference sample; 55 substances, mainly nicotine, furfural, tea polyphenol, beta-damascenone, megastigmatrienone, neophytadiene and the like, are detected in the heated cigarette added with the novel spice. Therefore, the addition of the volatile micromolecule tobacco flavor product can increase the richness of the smoke of the heated cigarette, thereby improving the sensory quality of the cigarette.
TABLE 5 comparison of thermolysis products of novel flavor products after addition to heated cigarettes (blank boxes are not detected)
Claims (9)
1. A preparation method of a heated cigarette spice with a smoke regulation function is characterized by comprising the following steps:
fermenting the mixed raw material of the Zimbabwe flue-cured tobacco leaves and the tea leaves which are naturally alcoholized for 1-2 years at 25-30 ℃ by using bacillus, and taking out a fermentation substrate after 5-10 days;
then extracting a fermentation substrate by using an ethanol solution with the concentration of 60-80 wt% to obtain a crude extract;
and filtering the crude extract by using an ultrafiltration membrane with the molecular weight of 1-3 ten thousand at the room temperature under the operating pressure of 0.16-0.18 MPa to obtain the novel spice.
2. The preparation method according to claim 1, wherein the mixed raw material of Zimbabwe flue-cured tobacco leaf and tea leaf is sieved with a sieve of not less than 200 meshes after being crushed.
3. The method of claim 1, wherein the tea leaves are one or more of black tea, green tea or dark tea.
4. The preparation method according to claim 1, wherein the mixed raw materials of Zimbabwe flue-cured tobacco leaf and tea leaf are as follows: the mass ratio of Zimbabwe flue-cured tobacco leaves to tea leaves is 10: 1-1: 1.
5. The method according to claim 1, wherein the Bacillus is provided in the form of a Bacillus strain solution at a concentration of not less than 10%10CFU/mL。
6. The method according to claim 5, wherein the bacillus liquid is provided in the form of: the composition is sprayed on the mixed raw material of the Zimbabwe flue-cured tobacco leaves and the tea leaves, wherein the spraying proportion is 1-10 wt%, and the weight of the Zimbabwe flue-cured tobacco leaves is taken as a reference.
7. The use of the novel flavor obtained by the preparation method according to claim 1, wherein the novel flavor is added to the cut tobacco of the heated cigarette in a flavoring manner in a proportion of 1 to 5 wt% for smoking.
8. The use according to claim 7, wherein the novel spice is added into the tobacco shreds of the heated cigarette to regulate and control the smoke of the heated cigarette, so that the release amount of harmful substances in the smoke of the heated cigarette is effectively reduced, and particularly, the reduction rate of the specific nitrosamine in the tobacco is not less than 50%.
9. The application of claim 7, wherein the novel spice is added into the tobacco shreds of the heated cigarette to regulate and control the smoke of the heated cigarette, increase the fragrant substances in the smoke, improve the smoking quality of the heated cigarette, enrich and plump the smoke, cover up miscellaneous gas and wood gas and enable the taste of the cigarette to be more mellow.
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