CN113913244A - Preparation method of low-sugar high-aroma tobacco flavor and application of tobacco flavor - Google Patents

Preparation method of low-sugar high-aroma tobacco flavor and application of tobacco flavor Download PDF

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Publication number
CN113913244A
CN113913244A CN202111102484.7A CN202111102484A CN113913244A CN 113913244 A CN113913244 A CN 113913244A CN 202111102484 A CN202111102484 A CN 202111102484A CN 113913244 A CN113913244 A CN 113913244A
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tobacco
low
liquid
flavor
carrying
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CN113913244B (en
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万帅
席高磊
陈芝飞
刘前进
马波波
蔡莉莉
李耀光
王清福
杜佳
张世英
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China Tobacco Henan Industrial Co Ltd
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China Tobacco Henan Industrial Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • A24B15/26Use of organic solvents for extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

The invention discloses a preparation method of a low-sugar high-aroma type tobacco flavor and application of the tobacco flavor, wherein the method comprises the following steps: heating and extracting at the temperature of 100-120 ℃ for 6-10h according to the material-liquid ratio of the Brazilian tobacco fragments to the extracting agent of 1 (10-15) to obtain an extracting material; carrying out ultrasonic-assisted flash extraction treatment on the extract, filtering and concentrating the extract product to obtain a Brazilian tobacco extract; adding polysaccharase into the Brazilian tobacco extract, carrying out inactivation treatment after enzymolysis for a period of time, and carrying out reduced pressure distillation to obtain a feed liquid; mixing the Brazilian tobacco extract and the feed liquid according to the volume ratio of 3 to 5 to 10, uniformly mixing the mixture with amino acid, adjusting the pH value to 8 to 10, and carrying out high-temperature high-pressure reaction in an inert gas atmosphere to obtain a spice liquid; and (3) adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the low-sugar high-aroma cigarette spice. The prepared low-sugar high-odor type tobacco flavor can be well coordinated with the tobacco flavor of a cigarette which is not combusted by heating, the smoke concentration is improved, the characteristics of the sweet and baked smoke flavor are highlighted, and the smoke richness is improved.

Description

Preparation method of low-sugar high-aroma tobacco flavor and application of tobacco flavor
Technical Field
The invention relates to the field of preparation of tobacco flavors, in particular to a preparation method of a low-sugar high-aroma tobacco flavor and application of the tobacco flavor.
Background
With the continuous and deep promotion of harm and tar reduction engineering in the tobacco industry, novel tobacco products appear at home and abroad in succession, and the cigarette which is not combusted by heating is the fastest one of the tobacco products. The cigarette without burning is heated by a special heating source of the appliance, so that the nicotine and the flavor substances in the tobacco shred are volatilized, and the smoke is generated to meet the requirements of smokers. Because the heating temperature of the cigarette which is not burnt is far lower than the burning temperature of the traditional cigarette, the produced harmful substances are less, and the cigarette meets the requirements of the current consumers, thereby becoming a novel cigarette product which is sought by the consumers. However, because the cigarette is heated at a low temperature without burning, most of the non-volatile substances in the cigarette cannot enter smoke through combustion decomposition, so that the smoke concentration and the fragrance amount of the cigarette are reduced, and the problem needs to be compensated by adding flavoring.
The tobacco extract is one of the most important flavor raw materials for blending flavor of Chinese cigarettes, and has the effects of enhancing the characteristic flavor of the tobacco and improving the sensory quality of the cigarettes. The cigarette industry enterprises can relieve the contradiction of insufficient supply of high-quality tobacco leaf raw materials to a certain extent by reasonably utilizing the tobacco extracts. However, the existing tobacco flavor cannot meet the requirements of low sugar and high fragrance.
Therefore, the technical problem to be solved in the field is how to provide the cigarette flavor which has low sugar and high aroma and is suitable for heating non-burning cigarettes.
Disclosure of Invention
The invention aims to provide a novel technical scheme for a preparation method of a cigarette flavor which has low sugar and high aroma and is suitable for heating non-combustible cigarettes.
According to a first aspect of the invention, a method for preparing a tobacco flavor from tobacco leaf residue is provided.
The preparation method of the low-sugar high-fragrance cigarette flavor comprises the following steps:
step (1): heating and extracting at the temperature of 100-120 ℃ for 6-10h according to the material-liquid ratio of the Brazilian tobacco fragments to the extracting agent of 1 (10-15) to obtain an extracting material, wherein the extracting agent comprises water and ethanol, the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL;
step (2): after the extraction material is balanced to room temperature, carrying out ultrasonic-assisted flash extraction treatment, and filtering and concentrating the extraction product to obtain the Brazilian tobacco extract, wherein the voltage of flash extraction is 150-;
and (3): adding polysaccharase into the Brazilian tobacco extract, carrying out inactivation treatment after enzymolysis for a period of time, and carrying out reduced pressure distillation to obtain a feed liquid;
and (4): mixing the Brazilian tobacco extract and the feed liquid according to the volume ratio of 3 to 5 to 10, uniformly mixing with amino acid, adjusting the pH to 8 to 10, reacting at high temperature and high pressure in an inert gas atmosphere to obtain the spice liquid,
wherein the temperature of the high-temperature high-pressure reaction is 150-;
and (5): and (3) adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the low-sugar high-aroma cigarette spice.
Optionally, the volume ratio of water to ethanol in the extractant in the step (1) is (1.5-2): 1.
Optionally, the step (1) is specifically as follows:
step (1-1): heating and extracting at 100-120 ℃ for 6-10h according to the material-liquid ratio of the Brazilian tobacco fragments to the extracting agent of 1 (10-15), and cooling to room temperature to obtain a pre-extracted material, wherein the extracting agent comprises water and ethanol, the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL;
step (1-2): and (3) carrying out ultrasonic treatment on the pre-extracted material, filtering and carrying out reduced pressure distillation to obtain an extracted material.
Optionally, the polysaccharidase in step (3) is at least one of alpha-amylase, cellulase, pectinase and glucoamylase.
Optionally, the enzymolysis parameters in step (3) are as follows:
the temperature is 30 ℃, the humidity is 68%, and the enzymolysis time is 4 h.
Optionally, the inactivation temperature in the step (3) is 60-80 ℃.
Optionally, the amino acid in the step (4) is at least one of proline, histidine, leucine and tryptophan, and the feed-liquid ratio of the amino acid to the sum of the volumes of the Brazilian tobacco extract and the feed liquid is 1 (20-50), wherein the unit of the feed in the feed-liquid ratio is g, and the unit of the liquid is mL.
Optionally, the feed-liquid ratio of the amino acid to the sum of the volumes of the Brazilian tobacco extract and the feed liquid is 1 (40-50).
Optionally, the parameters of the vacuum freeze-drying process in the step (5) are as follows:
the freezing temperature is-200 to-120 ℃, and the vacuum pressure is 10 to 100 Pa.
The invention also provides application of the tobacco leaf spice prepared by the preparation method of the low-sugar high-aroma type tobacco spice, wherein the addition amount of the low-sugar high-aroma type tobacco spice is 0.5-4 per mill.
The invention has the following advantages:
(1) the tobacco fragments are used as raw materials, a new idea is provided for fully utilizing a large amount of low-grade tobacco leaves and tobacco powder generated in the production of cigarette industry enterprises, the environmental pollution pressure can be reduced, the cost can be saved, and the industrial value is improved.
(2) After being concentrated and enriched, a large amount of saccharides contained in the tobacco leaves are subjected to Maillard reaction, so that the content of the saccharides is greatly reduced, the content of the fragrant substances is obviously increased, the fragrance intensity is higher, and the fragrance is richer.
(3) The inert gas is used for protection in the high-temperature high-pressure reaction stage, so that the oxidation deterioration of active fragrant compounds can be prevented, the loss of fragrant substances is reduced, and the quality of the perfume product is improved.
(4) The prepared low-sugar high-odor type tobacco flavor can be well coordinated with the tobacco flavor of a cigarette which is not combusted by heating, the smoke concentration is improved, the characteristics of the sweet and baked smoke flavor are highlighted, and the smoke richness is improved.
Detailed Description
Various exemplary embodiments of the present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
The preparation method of the low-sugar high-fragrance cigarette flavor comprises the following steps:
step (1): heating and extracting at 100-120 ℃ for 6-10h according to the material-liquid ratio of the Brazilian tobacco leaf fragments to the extracting agent of 1 (10-15) to obtain an extracting material, wherein the extracting agent comprises water and ethanol, the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL.
In order to improve the extraction efficiency, the volume ratio of water to ethanol in the extractant in the step (1) is (1.5-2): 1.
In order to ensure the content of effective components of the extracted product, the step (1) is specifically as follows:
step (1-1): heating and extracting at 100-120 ℃ for 6-10h according to the material-liquid ratio of the Brazilian tobacco leaf fragments to the extracting agent of 1 (10-15), and cooling to room temperature to obtain a pre-extracted material, wherein the extracting agent comprises water and ethanol, the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL.
Step (1-2): and (3) carrying out ultrasonic treatment on the pre-extracted material, filtering and carrying out reduced pressure distillation to obtain an extracted material.
Step (2): and (3) balancing the extraction material to room temperature, then carrying out ultrasonic-assisted flash extraction treatment, and filtering and concentrating the extraction product to obtain the Brazilian tobacco extract, wherein the flash extraction voltage is 150-.
And (3): adding polysaccharase into the Brazilian tobacco extract, carrying out inactivation treatment after enzymolysis for a period of time, and carrying out reduced pressure distillation to obtain a feed liquid.
In order to improve the polysaccharide decomposition efficiency, the polysaccharase in the step (3) is at least one of alpha-amylase, cellulase, pectinase and glucoamylase.
In order to ensure the decomposition effect, the enzymolysis parameters in the step (3) are as follows:
the temperature is 30 ℃, the humidity is 68%, and the enzymolysis time is 4 h.
The inactivation temperature in step (3) may be 60-80 ℃.
And (4): mixing the Brazilian tobacco extract and the feed liquid according to the volume ratio of 3 to 5 to 10, uniformly mixing with amino acid, adjusting the pH to 8 to 10, reacting at high temperature and high pressure in an inert gas atmosphere to obtain the spice liquid,
wherein the temperature of the high-temperature high-pressure reaction is 150-.
In specific implementation, 1-5mol/L aqueous solution of sodium hydroxide or potassium hydroxide can be used for adjusting the pH.
In order to ensure the effect of the Maillard reaction, the amino acid in the step (4) is at least one of proline, histidine, leucine and tryptophan, and the material-liquid ratio of the amino acid to the sum of the volumes of the Brazilian tobacco extract and the material liquid is 1 (20-50), wherein the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL.
In order to enhance the roasting sweet aroma of the low-sugar high-aroma type tobacco flavor, the feed-liquid ratio of the amino acid to the sum of the volumes of the Brazilian tobacco extract and the feed liquid is 1 (40-50).
Further, the feed-to-solution ratio of the amino acid to the sum of the volumes of the Brazilian tobacco extract and the feed solution was 1: 40.
And (5): and (3) adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the low-sugar high-aroma cigarette spice.
In specific implementation, the pH of the spice liquid can be adjusted by adopting citric acid aqueous solution, malic acid aqueous solution and tartaric acid aqueous solution.
The parameters of the vacuum freeze-drying treatment in the step (5) are as follows:
the freezing temperature is-200 to-120 ℃, and the vacuum pressure is 10 to 100 Pa.
The invention also provides application of the tobacco leaf spice prepared by the preparation method of the low-sugar high-aroma type tobacco spice, wherein the addition amount of the low-sugar high-aroma type tobacco spice is 0.5-4 per mill.
Furthermore, the addition amount of the low-sugar high-fragrance cigarette flavor is 3.5 per mill.
The experimental procedures used in the examples below are conventional unless otherwise specified, the materials and reagents used therein are commercially available, and the equipment used in the experiments are well known to those skilled in the art without otherwise specified.
Example 1
Weighing 40g of pulverized Brazilian tobacco leaf pieces, adding into a 500mL round-bottom flask, adding 400mL of an extractant (composed of water and ethanol in a volume ratio of 1.5: 1), heating and extracting at 120 deg.C for 6h in a heating mantle, and cooling to room temperature to obtain a pre-extract. And (3) carrying out ultrasonic treatment on the pre-extracted material, filtering and carrying out reduced pressure distillation to obtain an extracted material.
And (3) balancing the extraction material to room temperature, then carrying out ultrasonic-assisted flash extraction treatment, wherein the voltage of flash extraction is 150V, the rotating speed is 2500r/min, the extraction time is 3min, the ultrasonic power is 200W, and the extraction time is 10min, and filtering and concentrating the extraction product to obtain the Brazilian tobacco extract.
Taking part of Brazil tobacco extract, adding a certain amount of polysaccharase (comprising alpha-amylase, cellulase, pectinase and glucoamylase with a mass ratio of 1:2:1: 3) for treatment, carrying out enzymolysis at 30 ℃ and 68% humidity for 4h, inactivating at 60 ℃ after enzymolysis is finished, and carrying out reduced pressure distillation to obtain feed liquid.
Mixing the Brazilian tobacco extract and the feed liquid according to the volume ratio of 3:8, then mixing the mixture with amino acid (the volume ratio of the amino acid to the Brazilian tobacco extract to the feed liquid is 1:40) and pH regulating liquid (the pH is regulated to 9), adding the mixture into a 500mL autoclave type reactor, covering and sealing the reactor, opening an air inlet hole and an air outlet hole, filling nitrogen into the reactor through the air inlet hole, discharging the internal air through the air outlet hole, then closing the air outlet hole, and filling nitrogen again. Adjusting the temperature of the high-pressure kettle type reactor to 200 ℃, the pressure to 1.0MPa, reacting for 4 hours, and naturally cooling to room temperature.
And (3) adjusting the pH value of the reacted spice liquid to 6, and then freezing and drying at-150 ℃ and 25Pa to obtain the low-sugar high-aroma type tobacco spice.
Weighing a certain amount of low-sugar high-aroma type tobacco flavor, diluting the low-sugar high-aroma type tobacco flavor into a flavor solution with 5% (mass percent) by using ethanol and distilled water (the volume ratio is 1:4), uniformly spraying the flavor solution on reconstituted tobacco according to the addition amount of the tobacco flavor of 3.5 per mill, sealing and standing for 2 hours. Then the mixture is put into a baking oven at 100 ℃ for drying, is humidified by distilled water to reach the standard moisture (12 percent), and is rolled into a standard cigarette bullet for heating the non-combustible cigarette, and the balance time (the humidity is 50 percent +/-2 percent, and the temperature is 25 +/-1 ℃) is 48 hours. The smoke cartridge was heated by a special heating source of the appliance and the results of the smoke panel test are shown in table 1.
TABLE 1 results of the test
Figure BDA0003271367470000061
As can be seen from the smoking results in Table 1, the low-sugar high-aroma type tobacco flavor disclosed by the invention can better improve and modify the aroma of a cigarette which is not burned by heating, cover up miscellaneous gas, reduce the irritation of the cigarette, increase the smoke concentration and the sweet feeling, improve the aroma quality and the aroma quantity, increase the sensory comfort level and improve the smoking taste and aftertaste. The low-sugar high-aroma cigarette flavor disclosed by the invention is simple in preparation process, better in flavoring effect and suitable for flavoring heated cigarettes.
Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.

Claims (10)

1. A preparation method of a low-sugar high-fragrance cigarette flavor is characterized by comprising the following steps:
step (1): heating and extracting at the temperature of 100-120 ℃ for 6-10h according to the material-liquid ratio of the Brazilian tobacco fragments to the extracting agent of 1 (10-15) to obtain an extracting material, wherein the extracting agent comprises water and ethanol, the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL;
step (2): carrying out ultrasonic-assisted flash extraction treatment after the extraction material is balanced to room temperature, filtering and concentrating the extract product to obtain the Brazilian tobacco extract, wherein the flash extraction voltage is 150-;
and (3): adding polysaccharase into the Brazilian tobacco extract, carrying out inactivation treatment after enzymolysis for a period of time, and carrying out reduced pressure distillation to obtain a feed liquid;
and (4): according to the volume ratio of 3 (5-10), mixing the Brazilian tobacco extract and the feed liquid, uniformly mixing the mixture with amino acid, adjusting the pH value to 8-10, and carrying out high-temperature high-pressure reaction in an inert gas atmosphere to obtain the spice liquid, wherein the temperature of the high-temperature high-pressure reaction is 150-250 ℃, the pressure is 0.5-2.5MPa, and the reaction time is 2-4 h;
and (5): and (3) adjusting the pH value of the spice liquid to 5-7, and then carrying out vacuum freeze drying treatment to obtain the low-sugar high-aroma cigarette spice.
2. The preparation method of the low-sugar high-aroma cigarette flavor according to claim 1, wherein the volume ratio of water to ethanol in the extracting agent in the step (1) is (1.5-2): 1.
3. The preparation method of the low-sugar high-aroma cigarette flavor according to claim 1, wherein the step (1) is as follows:
step (1-1): heating and extracting at 100-120 ℃ for 6-10h according to the material-liquid ratio of the Brazilian tobacco fragments to the extracting agent of 1 (10-15), and cooling to room temperature to obtain a pre-extracted material, wherein the extracting agent comprises water and ethanol, the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL;
step (1-2): and (3) carrying out ultrasonic treatment on the pre-extracted material, filtering and carrying out reduced pressure distillation to obtain an extracted material.
4. The method for preparing the low-sugar high-flavor cigarette flavor according to claim 1, wherein the polysaccharidase in the step (3) is at least one of alpha-amylase, cellulase, pectinase and glucoamylase.
5. The preparation method of the low-sugar high-aroma cigarette flavor according to claim 1, wherein the enzymolysis parameters in the step (3) are as follows:
the temperature is 30 ℃, the humidity is 68%, and the enzymolysis time is 4 h.
6. The preparation method of the low-sugar high-flavor tobacco flavor according to claim 1, wherein the inactivation temperature in the step (3) is 60-80 ℃.
7. The preparation method of the low-sugar high-flavor tobacco flavor according to claim 1, wherein the amino acid in the step (4) is at least one of proline, histidine, leucine and tryptophan, and the material-liquid ratio of the amino acid to the sum of the volumes of the Brazilian tobacco extract and the material liquid is 1 (20-50), wherein the unit of the material in the material-liquid ratio is g, and the unit of the liquid is mL.
8. The preparation method of the low-sugar high-aroma type tobacco flavor according to claim 7, wherein the feed-liquor ratio of the amino acid to the sum of the volumes of the Brazilian tobacco extract and the feed liquor is 1 (40-50).
9. The preparation method of the low-sugar high-flavor tobacco flavor according to claim 1, wherein the parameters of the vacuum freeze drying treatment in the step (5) are as follows:
the freezing temperature is-200 to-120 ℃, and the vacuum pressure is 10 to 100 Pa.
10. The application of the tobacco leaf spice prepared by the preparation method of the low-sugar high-aroma type tobacco spice in any one of claims 1 to 9 is characterized in that the addition amount of the low-sugar high-aroma type tobacco spice is 0.5-4 per thousand.
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