Preparation method for atomized liquid flavor, atomized liquid flavor and atomized liquid

Abstract

Provided in the present disclosure are a preparation method for an atomized liquid flavor, an atomized liquid flavor, and an atomized liquid. The preparation method for an atomized liquid flavor comprises the following steps: step (1): adding a tobacco extract, an amino acid and a reducing sugar to a solvent for a hydrothermal reaction at 70°C-150°C for 2-5 h to obtain a Maillard reactant; and step (2): performing a distillation cracking reaction on the Maillard reactant at 180°C-300°C and the vacuum pressure of -0.06 Mpa-0.1 Mpa for 0.5-1.5 h to obtain a distillate as an atomized liquid flavor. The preparation method of the present disclosure can reduce the problems of burnt coils and carbon deposition, and improve the flavor richness of atomized liquids.

Description

Preparation method of atomized liquid flavor, atomized liquid flavor and atomized liquid

[0001] Cross-reference to related applications

[0002] The present disclosure is based on and claims priority to Chinese Patent Application No. 202411013061.1, filed on July 25, 2024, entitled “Preparation method of atomized liquid flavor, atomized liquid flavor and atomized liquid”, the entire contents of which are incorporated herein by reference. TECHNICAL FIELD

[0003] The present disclosure relates to the technical field of tobacco, in particular to a preparation method of atomized liquid flavor, atomized liquid flavor and atomized liquid. BACKGROUND

[0004] Electronic atomization devices have been widely reported as representatives of new types of tobacco products in recent years. Since it uses an atomizer to heat the atomized liquid to produce “vapor” for users to smoke, it does not produce a large amount of toxic and harmful substances generated by traditional tobacco combustion. Currently, atomized liquid flavors mainly use raw materials allowed by the national standard of electronic cigarettes and tobacco raw materials. With the rise of electronic atomization devices, users have increasingly increasing demand for the flavor and taste of atomized liquid.

[0005] Maillard reaction, as one of the main ways to produce important aroma components of tobacco, can produce important tobacco aroma components and potential aroma substances. However, the Maillard reaction process is complex, and the final product contains not only important small molecule aroma components, but also large molecule substances that cause negative sensory smoking. Therefore, the tobacco extract obtained after Maillard reaction is not effective in atomized liquid applications, and problems such as core paste and thick carbon deposition are prone to occur, which seriously affects product quality.

[0006] Therefore, it is necessary to develop a new preparation method of atomized liquid flavor, which can not only improve the richness of tobacco aroma of atomized liquid flavor, but also reduce the problems of core paste and carbon deposition when used in electronic atomization devices. SUMMARY

[0007] Therefore, the main purpose of the present disclosure is to provide a preparation method of atomized liquid flavor, atomized liquid flavor and atomized liquid. The preparation method provided by the present disclosure is simple in process, can improve the richness of tobacco aroma of atomized liquid flavor, and can reduce the problems of core paste and carbon deposition when used in electronic atomizers.

[0008] To this end, the first aspect of the present disclosure provides a preparation method of atomized liquid flavor, wherein the preparation method comprises the following steps:

[0009] Step (1): adding tobacco extract, amino acid and reducing sugar into a solvent, and performing hydrothermal reaction at 70-150℃ for 2-5h to obtain a Maillard reactant;

[0010] Step (2): performing distillation cracking reaction on the Maillard reactant at 180-300℃ under a vacuum pressure of-0.06Mpa to-0.1Mpa for 0.5-1.5h to obtain a distillate as an atomized liquid flavorant.

[0011] In some embodiments, in step (2), the distillation cracking reaction is sequentially performed at 1-5 gradient temperatures for 0.2-0.5h respectively to obtain a distillate as an atomized liquid flavorant.

[0012] In some embodiments, in step (2), the distillate at one or more of the 1-5 gradient temperatures is collected as an atomized liquid flavorant.

[0013] In some embodiments, in step (1), the tobacco extract∶solvent∶reducing sugar∶amino acid is 100∶40-400∶4-25∶1-13 by mass; and the pH of the hydrothermal reaction system is 4-10.

[0014] In some embodiments, the preparation method satisfies one or more of the following:

[0015] The tobacco extract is selected from one or more of flue-cured tobacco water extract, flue-cured tobacco alcohol extract, burley tobacco water extract and burley tobacco alcohol extract;

[0016] The amino acid is selected from one or more of proline, alanine, valine, tryptophan, histidine, glutamic acid and glycine;

[0017] The reducing sugar is selected from one or more of fructose syrup, fructose, glucose and xylose; and / or

[0018] The solvent is selected from a mixed solvent of propylene glycol and water.

[0019] In some embodiments, before step (2) is performed, the preparation method further comprises performing evaporation concentration on the Maillard reactant to obtain a concentrated Maillard reactant, and the density of the concentrated Maillard reactant is 1.15g / cm 3 -1.25g / cm 3 .

[0020] The second aspect of the present disclosure also provides an atomized liquid flavorant, which is obtained according to the preparation method of the first aspect described above, and the atomized liquid flavorant comprises nutty substances, roasty substances, floral substances, fresh substances, fruity substances and sweet substances.

[0021] In some embodiments, the nutty flavor substance includes one or more of 5-methyl-2-heptene-4-ketone, 5-methyl-2-acetylfuran, 2-propylpyrazine, 2,4,5-trimethylthiazole;

[0022] The roasty flavor substance includes one or more of 2-ethyl-6-methylpyrazine, 5-methylfurfural, maltol;

[0023] The floral flavor substance includes one or more of isobutyraldehyde, phenylacetaldehyde, benzyl alcohol, ethyl phenylacetate;

[0024] The fresh flavor substance includes one or more of neophytadiene, octyl acetate;

[0025] The fruity flavor substance includes one or more of ethyl acetate, methyl heptanoate, p-methylbenzaldehyde, dihydroactinidiolide; and

[0026] The sweet flavor substance includes one or more of hydroxyacetone, o-methylacetophenone, damascone, phenylacetic acid, ethyl phenylacetate.

[0027] The third aspect of the present disclosure also provides an atomized liquid including the atomized liquid flavor of the second aspect.

[0028] In some embodiments, the mass percentage of the atomized liquid flavor is 0.1-2% relative to the total mass of the atomized liquid.

[0029] The preparation method provided by the present disclosure promotes the occurrence of Maillard reaction by adding amino acids and reducing sugars in tobacco extract to produce important tobacco flavoring components and potential flavor substances. Then, through thermal cracking reaction, the potential flavor substances in the Maillard reaction products can be cracked to generate flavoring components, and at the same time, the macromolecular substances in the Maillard reaction products can be cracked to generate flavoring components and / or potential flavor substances, thereby enriching tobacco flavor substance components, thereby improving the richness of tobacco flavor in the atomized liquid flavor; in addition, the macromolecular substances in the Maillard reaction products are cracked into small molecular substances through thermal cracking reaction, which can reduce the problems of paste core and carbon deposition. The atomized liquid flavor prepared by the method of the present disclosure has rich tobacco flavor substances, which is beneficial to improve the sensory experience, and can reduce the problems of paste core and carbon deposition. BRIEF DESCRIPTION OF DRAWINGS

[0030] FIG. 1 is a paste core condition comparison chart of the atomized liquid flavor of the examples and the comparative examples of the present disclosure when used in an electronic atomizer. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present disclosure will be clearly and completely described in combination with the embodiments of the present disclosure and the drawings. Obviously, the described embodiments are only part of the embodiments of the present disclosure, rather than all the embodiments. Based on the embodiments in the present disclosure, all other embodiments obtained by those skilled in the art without creative effort fall within the scope of the present disclosure.

[0032] Throughout the specification, unless otherwise specifically indicated, the terms used herein are to be understood in the manner as commonly used in the art. Therefore, unless otherwise defined, all technical and scientific terms used herein have the same meaning as generally understood by those skilled in the art to which the present disclosure belongs. If there is a conflict, the present specification takes precedence.

[0033] It should be noted that in the embodiments of the present disclosure, the terms "comprise", "contain" or any other variants thereof are intended to cover non-exclusive inclusion, so that the method or device comprising a series of elements not only includes the elements explicitly recited, but also includes other elements not explicitly listed, or includes elements inherent to the implementation of the method or device. Without more limitation, the element defined by the sentence "comprises a" does not exclude the presence of other related elements in the method or device comprising the element.

[0034] In the present disclosure, the phrase "aerosol for inhalation by a user", "aerosol" or "smoke" can include, but is not limited to, aerosol, suspension liquid, low-temperature vapor and volatile gas.

[0035] Maillard reaction can be used to produce important tobacco aroma components and potential aroma substances. However, the Maillard reaction process is complex, and the final product has important small molecule aroma components and large molecule substances that cause negative sensory smoking. Therefore, the tobacco extract obtained after Maillard reaction has poor effect in the application of atomization liquid, and problems such as core paste and thick carbon deposition are easy to occur, which seriously affects the product quality.

[0036] Therefore, the first aspect of the present disclosure proposes a preparation method of atomization liquid flavor, which comprises the following steps:

[0037] Step (1): adding tobacco extract, amino acid and reducing sugar into a solvent, and carrying out hydrothermal reaction at 70-150℃ for 2-5h to obtain Maillard reaction product;

[0038] Step (2): carrying out distillation cracking reaction of the Maillard reaction product at 180-300℃ under the condition of vacuum pressure of-0.06Mpa to-0.1Mpa for 0.5-1.5h to obtain distillate as atomization liquid flavor.

[0039] In the present disclosure, Maillard reaction is carried out by adding amino acids and reducing sugars in tobacco extract to promote the occurrence of Maillard reaction, to produce important tobacco aroma components and potential aroma substances. The Maillard reaction is realized in the form of hydrothermal reaction, so that the temperature is regulated by hydrothermal mode to realize Maillard reaction flavoring. The temperature of the hydrothermal reaction is 70-150℃, and the time of the hydrothermal reaction is 2-5h. The temperature of the hydrothermal reaction is within the above range, which is conducive to the Maillard reaction of the substances in the tobacco extract with amino acids and reducing sugars to generate aroma components and potential aroma substances. If the temperature is too low, the reaction between the substances is insufficient, and the generated tobacco aroma substances are less, and the effect of Maillard reaction flavoring is lower. If the temperature is too high, more macromolecular substances are generated by reaction, which is easy to cause problems such as core paste and carbon deposition. Illustratively, the temperature of the hydrothermal reaction can be 70℃, 80℃, 90℃, 100℃, 110℃, 120℃, 130℃, 140℃, 150℃ or a value between any two of them. Preferably, the temperature of the hydrothermal reaction can be 120-140℃. Illustratively, the time of the hydrothermal reaction can be 2h, 3h, 4h, 5h or a value between any two of them. Preferably, the time of the hydrothermal reaction can be 3-4h.

[0040] When the product of Maillard reaction is directly used in electronic atomizer, it is easy to cause the problems of core paste and carbon deposition of electronic atomizer. In the related art, in order to solve the problems of core paste and carbon deposition of electronic atomizer, an alcohol precipitation process is introduced to treat the product of Maillard reaction. However, after the alcohol precipitation process, the problem of high carbon deposition still exists, and the tobacco aroma intensity of the product of Maillard reaction is reduced, which weakens the effect of Maillard reaction flavoring.

[0041] The inventors have found that, through a thermal cracking reaction, the potential aroma substances in the Maillard reactants can be cracked to generate aroma components, and at the same time, the macromolecular substances in the Maillard reactants can be cracked to generate aroma components and / or potential aroma substances, thereby enriching the tobacco aroma components, and thus improving the richness of the tobacco aroma in the atomized liquid flavor. In addition, the macromolecular substances in the Maillard reactants are cracked into small molecular substances through the thermal cracking reaction, which can reduce the problems of paste core and carbon deposition. The present disclosure realizes the thermal cracking of the Maillard reactants by performing a distillation cracking reaction at a temperature of 180-300°C and a vacuum pressure of-0.06 to-0.1 MPa for 0.5-1.5 h. Under the above conditions, the macromolecular substances in the Maillard reactants can be fully cracked into small molecular substances, and the potential aroma substances can be cracked into aroma components, thereby improving the richness of the tobacco aroma in the atomized liquid flavor, and at the same time, reducing the problems of paste core and carbon deposition caused by the macromolecular substances. For example, the temperature of the distillation cracking reaction can be 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, or a value between any two of the above values. For example, the vacuum pressure can be-0.06 MPa, -0.07 MPa, -0.08 MPa, -0.09 MPa, -0.1 MPa, or a value between any two of the above values. For example, the reaction time can be 0.5 h, 0.8 h, 1.0 h, 1.2 h, 1.5 h, or a value between any two of the above values.

[0042] In some embodiments, in step (2), the distillation cracking reaction is sequentially performed at 1-5 gradient temperatures for 0.2-0.5 h, respectively, to obtain a distillate as the atomized liquid flavor. For example, the distillation cracking reaction can be performed at 1, 2, 3, 4, or 5 gradient temperatures. Each of the gradient temperatures is selected from the range of 180-300°C. For example, the gradient temperature is selected from 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, or a value between any two of the above values. In the present disclosure, the 1-5 gradient temperatures are different. For example, the distillation cracking reaction can be performed at one gradient temperature of 195°C for 0.75 h; or can be sequentially performed at two gradient temperatures of 190°C and 195°C for 0.2-0.5 h, respectively; or can be sequentially performed at three gradient temperatures of 190°C, 195°C, and 205°C for 0.2-0.5 h, respectively; or can be sequentially performed at five gradient temperatures of 180°C, 200°C, 220°C, 240°C, and 260°C for 0.2 h, 0.2 h, 0.2 h, 0.2 h, and 0.2 h, respectively.

[0043] In some embodiments, in step (2), distillates at one or more of the 1-5 gradient temperatures are collected as the atomized liquid flavorant. Illustratively, distillates at all of the 1-5 gradient temperatures can be collected as the atomized liquid flavorant, obtaining all aroma substances from Maillard reaction and thermal cracking reaction. Distillates at one or more of the gradient temperatures can also be collected as the atomized liquid flavorant, screening specific aroma substances, to obtain atomized liquid flavorants with specific aroma. Illustratively, taking the example of performing the distillation cracking reaction at gradient temperatures of 190°C, 195°C, and 205°C in sequence, only the distillate at 190°C can be collected as the atomized liquid flavorant; or only the distillate at 195°C can be collected; or only the distillate at 205°C can be collected; or the distillates at 190°C and 205°C can be collected as the atomized liquid flavorant; or the distillates at 190°C, 195°C, and 205°C can be collected as the atomized liquid flavorant.

[0044] In some embodiments, the tobacco extract: solvent: reducing sugar: amino acid = 100: 40-400: 4-25: 1-13 by mass. The tobacco extract, solvent, reducing sugar, and amino acid in the above mass ratio are conducive to generating Maillard flavoring components, improving the quality of Maillard reaction products, and reducing the negative effects of Maillard reaction.

[0045] In some embodiments, the tobacco extract is selected from one or more of flue-cured tobacco water extract, flue-cured tobacco alcohol extract, burley tobacco water extract, and burley tobacco alcohol extract. The flue-cured tobacco water extract, flue-cured tobacco alcohol extract, burley tobacco water extract, and burley tobacco alcohol extract can be obtained commercially.

[0046] In some embodiments, the amino acid is selected from one or more of proline, alanine, valine, tryptophan, histidine, glutamic acid, glycine, and lysine. Illustratively, the amino acid is selected from one or more of proline and valine. Illustratively, the amino acid consists of proline and valine. Illustratively, the amino acid consists of proline and valine in a mass ratio of 7:4. The amino acid includes one or more of the above-mentioned amino acids, which is conducive to reacting with the reducing sugar to generate roasted aroma substances, nutty aroma substances, and other aroma substances, thereby improving the richness of tobacco aroma.

[0047] In some embodiments, the reducing sugar is selected from one or more of high fructose corn syrup, fructose, glucose, and xylose. Preferably, the reducing sugar is high fructose corn syrup. The reducing sugar includes one or more of the above-mentioned reducing sugars, which is conducive to reacting with the above-mentioned amino acid to generate roasted aroma substances, nutty aroma substances, and other aroma substances, thereby improving the richness of tobacco aroma.

[0048] In some embodiments, the solvent is a mixed solvent of propylene glycol and water. In this way, the amino acid and reducing sugar in the reaction system can be sufficiently dissolved, and the mixed solvent is selected, the reaction is mild, which is conducive to controlling the speed of the reaction, and reducing energy consumption, and improving the reaction efficiency. In some embodiments, when the solvent is a mixed solvent of propylene glycol and water, the mass ratio of propylene glycol and water is 1:1-10. Illustratively, the mass ratio of propylene glycol and water is 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, or a value between any two of them.

[0049] In some embodiments, before step (2) is performed, the preparation method further comprises evaporating and concentrating the Maillard reactants to obtain concentrated Maillard reactants, the density of the concentrated Maillard reactants is 1.15 g / cm 3 -1.25 g / cm 3 . Preferably, the Maillard reactants are concentrated after the Maillard reaction is completed. In this way, after the subsequent thermal cracking reaction is completed, it is not necessary to concentrate again, which is conducive to reducing the loss of smoke flavor substances. Preferably, the Maillard reactants are concentrated to the above density range. In this way, it is conducive to reducing the problem of reducing the quality of the atomized liquid flavor due to the occurrence of scorching in the subsequent distillation cracking step. Illustratively, the density of the concentrated Maillard reactants is 1.15 g / cm 3 , 1.16 g / cm 3 , 1.17 g / cm 3 , 1.18 g / cm 3 , 1.19 g / cm 3 , 1.20 g / cm 3 , 1.21 g / cm 3 , 1.22 g / cm 3 , 1.23 g / cm 3 , 1.24 g / cm 3 , 1.25 g / cm 3 , or a value between any two of them. In some preferred embodiments, the density of the concentrated Maillard reactants is 1.19 g / cm 3 -1.22 g / cm 3 .

[0050] In some embodiments, in step (2), propylene glycol is supplemented to the concentrated Maillard reactant. Preferably, the mass ratio of the concentrated Maillard reactant to propylene glycol is 1:0.01-0.2. The supplementation of propylene glycol in step (2) as a Maillard reactant protective agent is conducive to delaying the high-temperature carbonization time of the Maillard reactant and reducing the negative effects of thermal cracking reactions. On the other hand, the supplemented propylene glycol can act as an entraining agent to carry the aroma-producing substances out during the distillation process in step (2), which is conducive to enriching the aroma-producing substances in the Maillard reactant, improving the richness of the smoke aroma of the atomized liquid flavor, and improving the quality of the atomized liquid flavor.

[0051] The second aspect of the present disclosure also provides an atomized liquid flavor prepared according to the preparation method of the first aspect.

[0052] In some embodiments, the atomized liquid flavor comprises nutty substances, roasted substances, floral substances, fresh substances, fruity substances, and sweet substances.

[0053] The nutty substances comprise one or more of 5-methyl-2-heptene-4-ketone, 5-methyl-2-acetylfuran, 2-propylpyrazine, 2,4,5-trimethylthiazole, and other pyrazine, furan substances.

[0054] The roasted substances comprise one or more of 2-ethyl-6-methylpyrazine, 5-methylfurfural, maltol, and other pyrazine, aldehyde substances.

[0055] The floral substances comprise one or more of isobutyraldehyde, phenylacetaldehyde, benzyl alcohol, ethyl phenylacetate, and other aldehyde, alcohol, ester substances.

[0056] The fresh substances comprise one or more of neophytadiene and octyl acetate.

[0057] The fruity substances comprise one or more of ethyl acetate, methyl heptanoate, p-methylbenzaldehyde, dihydroactinidiolide, and other ester, aldehyde substances.

[0058] The sweet substances comprise one or more of hydroxyacetone, o-methylacetophenone, damascone, phenylacetic acid, ethyl phenylacetate, and other ketone, acid, ester substances.

[0059] In some embodiments, the atomized liquid flavor further comprises other substances, which are mainly tobacco substances in tobacco extracts, such as 2-acetylfuran, nicotine, guaiacol, macones, palmitic acid, and the like.

[0060] The third aspect of the present disclosure also provides an atomized liquid, which comprises the atomized liquid flavor of the present disclosure.

[0061] In some embodiments, the mass percentage of the atomized liquid flavoring in the atomized liquid is 0.1% to 2% relative to the total mass of the atomized liquid. Since the atomized liquid flavoring of the present disclosure is rich in aroma substance components, the atomized liquid can be flavored and supplemented with smoke aroma in a lower concentration range to improve the richness of smoke aroma. For example, the mass percentage of the atomized liquid flavoring in the atomized liquid can be 0.1%, 0.5%, 1.0%, 1.5%, 2.0%, or a value within a range between any two of the values.

[0062] In some embodiments, the atomized liquid of the present disclosure further comprises a solvent. The solvent is selected from one or more of propylene glycol (PG) or glycerol (VG). The mass percentage of the solvent in the atomized liquid is 98% to 99.9% relative to the total mass of the atomized liquid.

[0063] The present disclosure will be described in further detail below with reference to specific examples, which are merely illustrative and not intended to limit the scope of the present disclosure.

[0064] Examples

[0065] Example 1

[0066] The cloud tobacco extract, fructose-glucose syrup, and propylene glycol used in the following examples were purchased from Yunnan Mailang Biotechnology Co., Ltd., wherein the cloud tobacco extract was a liquid substance. Proline and valine were purchased from Henan Wanbang Chemical Technology Co., Ltd. Sodium hydroxide was purchased from Shanghai Titan Science and Technology Co., Ltd.

[0067] 1) Maillard reaction

[0068] Take 100 g of cloud tobacco extract, add 12 g of fructose-glucose syrup, 0.7 g of proline, 0.4 g of valine, and 13 g of propylene glycol (PG), and dissolve in 42 g of purified water to obtain a mixture. Then use a saturated sodium hydroxide solution to adjust the pH of the mixture to 8.5. Add the mixture to a sealed pressure-resistant reaction kettle, heat to 140°C, and react for 3 h to obtain a Maillard reaction product.

[0069] 2) Concentration

[0070] Concentrate the above Maillard reaction product at 60°C and 100 mbar using a rotary evaporator to remove the solvent, obtaining 110 g of concentrated Maillard reaction product. The density of the concentrated Maillard reaction product is 1.20 g / cm 3 .

[0071] 3) Distillation cracking

[0072] To the above concentrated Maillard reactants, 11 g of propylene glycol was added and mixed uniformly. Distillation and cracking were carried out under the conditions of a vacuum pressure of -0.07 Mpa and gradient temperatures of 190°C, 195°C and 205°C for 15 min, respectively. All the distillates obtained at 190°C, 195°C and 205°C were collected as an atomized liquid flavor.

[0073] The atomized liquid flavor obtained above was tested according to the following method.

[0074] Paste core test experiment

[0075] According to a 2% addition amount, the atomized liquid flavor was added to a mixed solvent of PG:VG = 6:4 (solvent accounted for 98%), to obtain an atomized liquid. The atomized liquid was loaded into an electronic atomizer, a smoking machine was used for simulated smoking, the heating body of the electronic atomizer was disassembled, and the paste core condition of the heating body was observed by an optical microscope. The smoking machine smoking parameters were set as 800 puffs, the paste core appeared, and the test was no longer continued; the preheating time was 0.05 s; the smoking time was 3 s; the rest time was 15 s; and the smoking capacity was 55 ml.

[0076] Sensory evaluation

[0077] According to a 2% addition amount, the atomized liquid flavor was added to a mixed solvent of PG:VG = 6:4 (solvent accounted for 98%), to obtain an atomized liquid. The atomized liquid was loaded into an electronic atomizer. Seven evaluators were invited to perform sensory evaluation of smoking, and sensory evaluation was performed from the aspects of comfort, richness, irritation, smoke, and odor, etc. The sensory evaluation was mainly based on GB5606.4-2005 as the evaluation standard, combined with the sensory characteristics of electronic cigarettes to give the sensory evaluation. The sensory evaluation scoring standard is shown in Table 1.

[0078] Table 1: Sensory evaluation scoring standard

[0079] Analysis of aroma components and flavor substances

[0080] The analysis was performed by using a solid phase microextraction-gas chromatography mass spectrometry (SPME-GC / MS) analysis method, and the classification and number of aroma components and flavor substances of the atomized liquid flavor were compared. The more the number of aroma components and flavor substances, the richer the aroma, and the better the characteristic aroma effect.

[0081] Comparative example 1

[0082] 1) Maillard reaction

[0083] Take 100 g of Yunyan tobacco extract, add 12 g of fructose syrup, 0.7 g of proline, 0.4 g of valine, 13 g of propylene glycol (PG), and dissolve in 42 g of purified water, stir uniformly to obtain a mixed solution. Then use saturated sodium hydroxide solution to adjust the pH of the mixed solution to 8.5. Add the mixed solution to a sealed pressure-resistant reaction kettle, heat to 140°C and react for 3h to obtain a Maillard reaction liquid.

[0084] 2) Concentration

[0085] Concentrate the above Maillard reaction product at 60°C and 100 mbar using a rotary evaporator to remove the solvent to obtain 110 g of concentrated Maillard reaction product as an atomized liquid flavorant. The density of the concentrated Maillard reaction product is 1.20 g / cm 3 .

[0086] The atomized liquid flavorant of Comparative Example 1 was subjected to paste core testing, sensory evaluation, aroma component analysis, and note substance analysis according to the test method of Example 1 described above.

[0087] Comparative Example 2

[0088] 1) Concentration

[0089] Take 150 g of Yunyan tobacco extract, concentrate it at 60°C and 100 mbar using a rotary evaporator to remove the solvent to obtain 125 g of concentrated Yunyan extract. The density of the concentrated Yunyan extract is 1.20 g / cm 3

[0090] 2) Distillation cracking

[0091] Add 10 g of PG to 100 g of the above concentrated Yunyan extract and mix uniformly. Distill and crack under the conditions of a vacuum pressure of -0.07 Mpa and gradient temperatures of 190°C, 195°C, and 205°C for 15 min each, and collect all the distillates obtained at 190°C, 195°C, and 205°C as an atomized liquid flavorant.

[0092] The atomized liquid flavorant of Comparative Example 2 was subjected to paste core testing, sensory evaluation, aroma component analysis, and note substance analysis according to the test method of Example 1 described above.

[0093] Comparative Example 3

[0094] 1) Maillard reaction and 2) Concentration

[0095] The Maillard reaction and concentration were carried out in the same way as in Example 1 to obtain a concentrated Maillard reaction product.

[0096] 3) Distillation cracking reaction

[0097] A distillation pyrolysis reaction was performed in the same manner as in Example 1, except that the distillation pyrolysis was performed at 160°C for 45 min, and the distillate was collected as an atomized liquid flavorant.

[0098] The atomized liquid flavorant was subjected to the core test, sensory evaluation, analysis of aroma- contributing components, and analysis of note substances in the same manner as in Example 1.

[0099] Comparative Example 4

[0100] 1) Maillard reaction and 2) concentration

[0101] A Maillard reaction and concentration were performed in the same manner as in Example 1 to obtain a concentrated Maillard reactant.

[0102] 3) distillation pyrolysis reaction

[0103] A distillation pyrolysis reaction was performed in the same manner as in Example 1, except that the distillation pyrolysis was performed at 320°C for 45 min, and the distillate was collected as an atomized liquid flavorant.

[0104] The atomized liquid flavorant was subjected to the core test, sensory evaluation, analysis of aroma- contributing components, and analysis of note substances in the same manner as in Example 1.

[0105] Comparative Example 5

[0106] 1) Maillard reaction and 2) concentration

[0107] A Maillard reaction and concentration were performed in the same manner as in Example 1 to obtain a concentrated Maillard reactant.

[0108] 3) microwave pyrolysis

[0109] A microwave pyrolysis was performed on 40 g of the concentrated Maillard reactant in a 100 mL microwave reaction vessel to obtain a microwave pyrolysis product. The microwave pyrolysis was performed at a power of 900 W for 120 s to obtain the microwave pyrolysis product as an atomized liquid flavorant.

[0110] Comparative Example 6

[0111] 1) Maillard reaction and 2) concentration

[0112] A Maillard reaction and concentration were performed in the same manner as in Example 1 to obtain a concentrated Maillard reactant.

[0113] 3) microwave pyrolysis and solvent extraction

[0114] A microwave pyrolysis was performed on 40 g of the concentrated Maillard reactant in a 100 mL microwave reaction vessel to obtain a microwave pyrolysis product. The microwave pyrolysis was performed at a power of 900 W for 120 s.

[0115] The 40 g of the microwave cleavage product was extracted with 400 ml of anhydrous ethanol to obtain an extract. The extract was then concentrated under reduced pressure to obtain an extract product as an atomizing liquid flavorant.

[0116] The atomizing liquid flavorant was subjected to the plug test, sensory evaluation, analysis of aroma components and note substances according to the test method of Example 1 described above.

[0117] Blank Example

[0118] The Virginia tobacco extract material which was not subjected to the Maillard reaction and the distillation cleavage reaction was used as a blank for the plug test, sensory evaluation, analysis of aroma components and note substances.

[0119] The plug test heating element plug condition is shown in FIG. 1, the plug condition and the carbon deposit thickness are shown in Table 2, the sensory evaluation results are shown in Table 3, the analysis results of aroma components and note substances are shown in Tables 4 and 5.

[0120] Table 2: Plug Test Results

[0121] Table 3: Sensory Evaluation Results

[0122] Table 4: Classification of Aroma Components and Number of Kinds

[0123] Table 5: Classification of Note Substances and Number of Kinds

[0124] From the paste core test results shown in Table 2 and the sensory evaluation results of Table 3 above, it can be seen that in the present disclosure, the atomized liquid flavor obtained by treating the Maillard reaction and distillation cracking process not only has rich tobacco aroma, clean aftertaste, and obvious aroma characteristics, but also can eliminate the negative effects brought by the Maillard reaction, reduce the risk of paste core and carbon deposition, and effectively improve the quality of the atomized liquid product. From the results of the aroma components and aroma substances analysis of Tables 4-5, it can be seen that the atomized liquid flavor prepared in Example 1 has obvious nutty aroma, roasting aroma, fresh aroma, floral aroma, fruity aroma, sweet aroma, and other aromas, and the aroma is the most abundant. Comparative Example 1 did not perform the distillation cracking step, and the atomized liquid flavor obtained had paste core and serious carbon deposition. In the sensory evaluation, the tobacco aroma components were reduced, the odor was heavy, and there was residual aftertaste, and the types of aroma components and aroma substances were reduced. Comparative Example 2 did not perform the Maillard reaction step. Due to the distillation cracking reaction, the atomized liquid obtained did not have the problems of paste core and carbon deposition, but in the sensory evaluation, the richness of tobacco aroma was low, the odor was heavy, and the types of aroma components and aroma substances were significantly reduced. Comparative Example 3 performed distillation cracking at a lower temperature, and the atomized liquid obtained had heavy odor, low richness of tobacco aroma, and significantly reduced types of aroma components and aroma substances. Comparative Example 4 performed distillation cracking at a higher temperature, and the atomized liquid obtained had more types of aroma components and aroma substances, but the burnt paste feeling was heavy, affecting the sensory evaluation. Comparative Example 5 treated the Maillard reaction product by microwave cracking, and the atomized liquid flavor obtained had low richness of tobacco aroma and odor, and fewer types of aroma components and aroma substances. Comparative Example 6 further enriched the aroma components and aroma substances in the cracking product by using ethanol extraction based on microwave cracking, and the number of types of aroma components and aroma substances was significantly increased, but due to the introduction of solvent extraction, the electronic atomizer flavor was prone to paste core and serious carbon deposition.

[0125] Examples 2-3

[0126] The atomized liquid flavor was prepared according to the method of Example 1 above, except that the distillation cracking reaction was performed according to the parameters of Table 6 below. The atomized liquid flavor of Examples 2-3 was subjected to sensory evaluation, paste core test, and aroma component and aroma substance analysis according to the test methods of Example 1 above. The paste core test results are shown in Table 7 and Figure 1, the sensory evaluation results are shown in Table 8, and the aroma component analysis results are shown in Tables 9 and 10.

[0127] Table 6: Maillard reaction and distillation cracking reaction conditions

[0128] Table 7: Paste core test results

[0129] Table 8: Sensory evaluation results

[0130] Table 9: Substance classification and number of categories of aroma ingredients

[0131] Table 10: Substance classification and number of categories of aroma notes

[0132] From the above test results, it can be seen that the atomized liquid flavor obtained by distillation cracking at different temperature gradients significantly reduces the problems of paste core and carbon deposition, and the atomized liquid flavor has rich tobacco aroma, good taste, clean aftertaste, and good comprehensive sensory evaluation, effectively improving the quality of the atomized liquid product.

[0133] The above only describes the preferred embodiments of the present disclosure, and does not limit the patent scope of the present disclosure, and any equivalent structural transformation made under the inventive concept of the present disclosure, or direct / indirect application in other related technical fields, is included in the patent protection scope of the present disclosure.

Claims

1. A process for the preparation of an atomized liquid fragrance wherein, The preparation method comprises the following steps: Step (1): adding tobacco extract, amino acid and reducing sugar into a solvent, and performing hydrothermal reaction at 70-150°C for 2-5h to obtain a Maillard reactant; Step (2): performing distillation cracking reaction on the Maillard reactant at 180-300°C under the condition of vacuum pressure of-0.06 to-0.1Mpa for 0.5-1.5h to obtain a distillate as an atomized liquid flavor.

2. The production process according to claim 1, wherein In step (2), the distillation cracking reaction is sequentially performed at 1-5 gradient temperatures for 0.2-0.5h respectively to obtain a distillate as an atomized liquid flavor.

3. The production process according to claim 2, wherein, In step (2), the distillate at one or more of the 1-5 gradient temperatures is collected as an atomized liquid flavor.

4. The production process according to claim 1 or 2, wherein In step (1), the mass ratio of tobacco extract:solvent:reducing sugar:amino acid is 100:40-400:4-25:1-13; and the pH of the hydrothermal reaction system is 4-10.

5. The production process according to claim 1 or 2, wherein The preparation method satisfies one or more of the following: The tobacco extract is selected from one or more of flue-cured tobacco water extract, flue-cured tobacco alcohol extract, burley tobacco water extract and burley tobacco alcohol extract; The amino acid is selected from one or more of proline, alanine, valine, tryptophan, histidine, glutamic acid and glycine; The reducing sugar is selected from one or more of fructose-glucose syrup, fructose, glucose and xylose; and / or The solvent is selected from a mixed solvent of propylene glycol and water.

6. The production process according to claim 1 or 2, wherein Before performing step (2), the preparation method further comprises evaporating and concentrating the Maillard reactants to obtain concentrated Maillard reactants, the density of the concentrated Maillard reactants being 1.15 g / cm 3 ~ 1.25 g / cm 3 .

7. An atomized liquid fragrance prepared according to the method of any one of claims 1 to 6, wherein, The atomized liquid flavor comprises nutty substance, roasty substance, floral substance, fresh substance, fruity substance and sweet substance.

8. The atomized liquid flavor according to claim 7, wherein, The nutty substance comprises one or more of 5-methyl-2-heptene-4-ketone, 5-methyl-2-acetyl furan, 2-propyl pyrazine and 2,4,5-trimethyl thiazole; The roasty substance comprises one or more of 2-ethyl-6-methyl pyrazine, 5-methyl furfural and maltol; The floral substance comprises one or more of isobutyraldehyde, phenylacetaldehyde, benzyl alcohol and ethyl phenylacetate; The fresh substance comprises one or more of neophytadiene and octyl acetate; The fruity substance comprises one or more of ethyl acetate, methyl heptanoate, p-methyl benzaldehyde and dihydroactinidiolide; and The sweet substance comprises one or more of hydroxyacetone, o-methyl acetophenone, damascone, phenylacetic acid and ethyl phenylacetate.

9. An atomized liquid, comprising the atomized liquid flavor of claim 7 or 8.

10. The atomized liquid according to claim 9, wherein, The mass percentage content of the atomized liquid flavor in the atomized liquid is 0.1-2% relative to the total mass of the atomized liquid.

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