Aromatic plant endogenous fragrance, preparation method thereof and atomized fragrance

Abstract

The invention discloses an endogenous aromatic plant flavor and a preparation method thereof and an atomized flavor, belonging to the technical field of flavors and fragrances. The preparation method of the endogenous aromatic plant flavor comprises the following steps: providing aromatic plant dry powder; subjecting the aromatic plant dry powder to supercritical CO 2 Extraction to obtain Extract 1; freeze-drying, thermal cracking, molecular distillation of Extract 1, taking the distillate to obtain Extract 2; enzymatic hydrolysis of aromatic plant dry powder, filtration, and concentration to obtain Extract 3; Maillard reaction of Extract 3, membrane concentration to obtain Extract 4; Extract 1, Extract 2, Extract 3 and Extract 4 are mixed to obtain aromatic plant endogenous flavors. Through the directional extraction of important tobacco aroma precursors and combined with the thermal reaction process, the types of tobacco endogenous aroma are created and enriched, making up for the lack of aroma and poor richness of existing tobacco endogenous flavors.

Description

Technical Field

[0001] The invention relates to the technical field of flavors, and in particular to an endogenous flavor of aromatic plants, a preparation method thereof, and an atomized flavor. Background Art

[0002] Aromatic plants, in a narrow sense, can be understood as plants that can release fragrance, while in a broad sense, the scope of aromatic plants is relatively broad, and it is a general term for plants that have odor or can extract aromatic compounds. Because they are rich in alcohols, esters, ethers, ketones and other types of aromatic compounds, they often bring direct or indirect sensory pleasure to people.

[0003] Aromatic plants contain a wealth of chemical components, which can be roughly divided into four categories: aromatic components, medicinal components, nutritional components, and pigment components; in addition, there are some antioxidants and antibacterial components. Among them, aromatic components are the most important characteristics of aromatic plants, which can generally be used as raw materials in the spice industry.

[0004] Plants synthesize and release low-boiling-point, low-molecular-weight secondary metabolites in their natural state, collectively referred to as plant volatile organic compounds, which are a type of volatile organic compound emitted directly into the atmosphere. Different parts of plants, including flowers, fruits, stems, leaves, etc., can release volatile organic compounds. The composition of volatile organic compounds contains about tens of thousands of compounds, which can be roughly divided into three categories: terpenes (isoprene, monoterpenes and sesquiterpenes), phenyl / phenylpropanoids, and fatty acid derivatives.

[0005] However, some aromatic plants contain a considerable number of aroma precursors, which are generally not direct products of the metabolic process of carbon, nitrogen and other substances, but are first synthesized into non-volatile macromolecular compounds such as esters and terpenes, and then further decomposed under the action of enzymes or non-enzymes to form volatile and semi-volatile organic compounds. For example, in the aromatic plant tobacco, according to the relationship between aroma substances and aroma precursors, tobacco aroma substances can be divided into the following categories: glycoside compounds, sugar ester compounds, cypermethrin compounds, lysine compounds and Maillard reaction substances. Previous studies have shown that these aroma precursors will release a large number of aroma components during the production and processing of cigarettes and the smoking process, such as neophytadiene, nicotine, solanone, damascenone, geranyl acetone, megastigmatrienone, β-ionone, benzaldehyde, benzyl alcohol, dihydroactinolide and other key aroma components.

[0006] At present, the industrial extraction of endogenous flavors from aromatic plants can be mainly divided into water extraction to extract polar aroma substances; supercritical CO2 extraction to extract non-polar aroma substances; organic solvent extraction to extract medium-polar and weak-polar aroma substances, etc. These endogenous flavors are generally extracted from plant leaves or plant extracts by a single technical means, which cannot fully reflect the complex characteristics of the aromatic plant's own aroma substances. For example: ultrasonic extraction of nicotine, hemicellulose, lignin, and cellulose from tobacco leaves, although the extraction of substances is more thorough, but the process is complicated, the extraction materials are more complex and not conducive to subsequent further separation, and the introduction of more substances will also destroy the aroma of tobacco. Summary of the invention

[0007] The main purpose of the present invention is to provide a method for preparing endogenous aromatic plant spices, aiming to overcome the problems of insufficient aroma and more impurities in the prior art of endogenous aromatic plant spices.

[0008] To achieve the above object, the present invention provides a method for preparing endogenous fragrances from aromatic plants, comprising the following steps:

[0009] Provide aromatic plant dried powder;

[0010] The aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1;

[0011] The extract 1 is freeze-dried, thermally cracked, and molecularly distilled, and a distillate is taken to obtain an extract 2;

[0012] The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration and concentration to obtain extract three;

[0013] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four;

[0014] The extract one, the extract two, the extract three and the extract four are mixed to obtain the aromatic plant endogenous fragrance.

[0015] Optionally, the aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain an extract:

[0016] The extraction pressure is 10-40 MPa; and / or,

[0017] The extraction time is 0.5 to 6 hours; and / or,

[0018] The extraction temperature is 40-60°C; and / or,

[0019] The flow rate of CO2 is 6 to 10 L / h.

[0020] Optionally, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2:

[0021] The freeze drying temperature is -50 to -5°C; and / or,

[0022] The vacuum degree of freeze drying is 10-20 Pa; and / or,

[0023] The freeze drying time is 0.5 to 2.5 hours; and / or,

[0024] The temperature of thermal cracking is 100 to 300°C; and / or,

[0025] The heating rate of thermal cracking is 3 to 10°C / min; and / or,

[0026] The thermal cracking time is 0.2 to 1.5 hours; and / or,

[0027] The temperature of molecular distillation is 50-120°C; and / or,

[0028] The vacuum degree of molecular distillation is 0.5 to 50 mbar; and / or,

[0029] The feed flow rate of molecular distillation is 50-150 mL / h.

[0030] Optionally, the aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration, and concentration to obtain the following three extracts:

[0031] The enzyme for enzymatic hydrolysis comprises at least one of α-amylase and β-amylase; and / or,

[0032] The temperature of the enzymatic hydrolysis is 50-65°C; and / or,

[0033] The enzymatic hydrolysis time is 6 to 8 hours; and / or,

[0034] The pH value of the enzymatic hydrolysis is 5.4 to 5.8; and / or,

[0035] The mass ratio of the enzyme to the substrate in the enzymatic hydrolysis is (1-3): (5-10); and / or,

[0036] The temperature of vacuum concentration is 50-55°C; and / or,

[0037] The vacuum degree of vacuum concentration is 30-50 mbar; and / or,

[0038] The vacuum concentration time is 1.0 to 2.0 h.

[0039] Optionally, the extract three is subjected to a Maillard reaction and membrane concentration to obtain an extract four:

[0040] Extract three is subjected to a Maillard reaction with L-alanine; and / or,

[0041] The pH value of the Maillard reaction is 7.5 to 8.5; and / or,

[0042] The temperature of the Maillard reaction is 105-125°C; and / or,

[0043] The Maillard reaction time is 2 to 5 hours; and / or,

[0044] The water content during the Maillard reaction is 5 to 25%; and / or,

[0045] The pore size of the membrane concentration is 50 to 200 nm; and / or,

[0046] The molecular cutoff of the membrane concentration is greater than 25,000.

[0047] Optionally, the extract one, the extract two, the extract three and the extract four are mixed to obtain the aromatic plant endogenous fragrance:

[0048] The mass ratio of extract 1, extract 2, extract 3 and extract 4 is (0.5-1): (0.8-1): (1-2): (0.5-1.5).

[0049] Optionally, in the aromatic plant dry powder provided: the aromatic plant includes at least one of tobacco, thyme, gardenia, sage and lemon balm.

[0050] The invention also provides an aromatic plant endogenous fragrance, which is prepared by the preparation method of the aromatic plant endogenous fragrance.

[0051] The invention also provides an atomized essence, comprising the endogenous fragrance of the aromatic plant.

[0052] The preparation method of the aromatic plant endogenous fragrance of the present invention creates a rich variety of tobacco endogenous aroma by directional extraction of important tobacco aroma precursors and combining with a thermal reaction process, thereby making up for the problem of insufficient aroma richness of existing tobacco endogenous fragrances. Not only are the types of tobacco endogenous aromas rich, but they are also highly compatible with tobacco flavors or electronic atomization liquids. When it is configured into a tobacco flavor or added to an electronic atomization liquid, it has high solubility, low threshold, and rich tobacco flavor, which can significantly improve the taste of tobacco flavors or electronic atomization liquids. DETAILED DESCRIPTION

[0053] To make the purpose, technical scheme and advantages of the embodiment of the present invention clearer, the technical scheme in the embodiment of the present invention will be described clearly and completely below. If the specific conditions are not specified in the embodiment, it is carried out according to the normal conditions or the conditions recommended by the manufacturer. If the reagents or instruments used do not specify the manufacturer, they are all conventional products that can be purchased commercially. In addition, the meaning of "and / or" appearing in the full text includes three parallel schemes, taking "A and / or B" as an example, including scheme A, or scheme B, or schemes that A and B meet at the same time. In addition, the technical schemes between the various embodiments can be combined with each other, but must be based on the ability of ordinary technicians in the field to achieve. When the combination of technical solutions is contradictory or cannot be achieved, it should be considered that the combination of such technical solutions does not exist, and is not within the scope of protection required by the present invention. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in the field without making creative work belong to the scope of protection of the present invention.

[0054] Aromatic plants, in a narrow sense, can be understood as plants that can release fragrance, while in a broad sense, the scope of aromatic plants is relatively broad, and it is a general term for plants that have odor or can extract aromatic compounds. Because they are rich in alcohols, esters, ethers, ketones and other types of aromatic compounds, they often bring direct or indirect sensory pleasure to people.

[0055] Aromatic plants contain a wealth of chemical components, which can be roughly divided into four categories: aromatic components, medicinal components, nutritional components, and pigment components; in addition, there are some antioxidants and antibacterial components. Among them, aromatic components are the most important characteristics of aromatic plants, which can generally be used as raw materials in the spice industry.

[0056] Plants synthesize and release low-boiling-point, low-molecular-weight secondary metabolites in their natural state, collectively referred to as plant volatile organic compounds, which are a type of volatile organic compound emitted directly into the atmosphere. Different parts of plants, including flowers, fruits, stems, leaves, etc., can release volatile organic compounds. The composition of volatile organic compounds contains about tens of thousands of compounds, which can be roughly divided into three categories: terpenes (isoprene, monoterpenes and sesquiterpenes), phenyl / phenylpropanoids, and fatty acid derivatives.

[0057] However, some aromatic plants contain a considerable number of aroma precursors, which are generally not direct products of the metabolic process of carbon, nitrogen and other substances, but are first synthesized into non-volatile macromolecular compounds such as esters and terpenes, and then further decomposed under the action of enzymes or non-enzymes to form volatile and semi-volatile organic compounds. For example, in the aromatic plant tobacco, according to the relationship between aroma substances and aroma precursors, tobacco aroma substances can be divided into the following categories: glycoside compounds, sugar ester compounds, cypermethrin compounds, lysine compounds and Maillard reaction substances. Previous studies have shown that these aroma precursors will release a large number of aroma components during the production and processing of cigarettes and the smoking process, such as neophytadiene, nicotine, solanone, damascenone, geranyl acetone, megastigmatrienone, β-ionone, benzaldehyde, benzyl alcohol, dihydroactinolide and other key aroma components.

[0058] At present, the industrial extraction of endogenous flavors from aromatic plants can be mainly divided into water extraction to extract polar aroma substances; supercritical CO2 extraction to extract non-polar aroma substances; organic solvent extraction to extract medium-polar and weak-polar aroma substances, etc. These endogenous flavors are generally extracted from plant leaves or plant extracts by a single technical means, which cannot fully reflect the complex characteristics of the aromatic plant's own aroma substances. For example: ultrasonic extraction of nicotine, hemicellulose, lignin, and cellulose from tobacco leaves, although the extraction of substances is more thorough, but the process is complicated, the extraction materials are more complex and not conducive to subsequent further separation, and the introduction of more substances will also destroy the aroma of tobacco.

[0059] At present, low-boiling volatile substances are extracted from aromatic plants by a single technical means. A large number of aroma precursors contained in aromatic plants will produce a richer variety of aroma components under specific conditions such as relatively low-temperature Maillard reaction, high-temperature thermal cracking reaction, or microbial fermentation and enzymatic hydrolysis reaction. These aroma components and their application effects are closer to the original aroma of aromatic plants when they are burned. However, there has been no targeted research on the endogenous aroma components of important aroma precursors in aromatic plants during the thermal reaction process.

[0060] In view of this, the present invention proposes a method for preparing endogenous spices from aromatic plants, aiming to overcome the problems of insufficient aroma and excessive impurities in the prior art of endogenous spices from aromatic plants.

[0061] A method for preparing endogenous aromatic plant spices comprises the following steps:

[0062] Provide aromatic plant dried powder;

[0063] The aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1;

[0064] The extract 1 is freeze-dried, thermally cracked, and molecularly distilled, and a distillate is taken to obtain an extract 2;

[0065] The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration and concentration to obtain extract three;

[0066] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four;

[0067] The extract one, the extract two, the extract three and the extract four are mixed to obtain the aromatic plant endogenous fragrance.

[0068] The extract obtained by supercritical CO2 extraction is mainly carotenoids, such as α-carotene, β-carotene, violaxanthin and neoxanthin. These substances, as important aroma precursors, provide a rich variety of aroma components under specific conditions.

[0069] The first extract is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain a second extract, which mainly contains small molecular volatile substances, such as esters, acids, phenols, etc. These substances can provide rich top notes.

[0070] The aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, which mainly contains rich reducing sugar substances. On the one hand, sugar itself is a precursor for the formation of aroma. On the other hand, these substances can provide endogenous Maillard reaction substrates and promote the occurrence and progress of the Maillard reaction.

[0071] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four, which mainly contains substances mainly composed of heterocyclic compounds such as pyrazine and pyrrole, such as 2-methylpyrazine, 2,5-dimethylpyrazine, 2-ethylpyrazine, etc. These substances can provide roasted, nut-like flavor characteristics.

[0072] It should be noted that the aromatic plant dry powder can be purchased or prepared by oneself. In any embodiment of the present invention, taking tobacco leaves as an example, it can be prepared by oneself, and the following preparation method is adopted: use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, place the tobacco leaves in an oven at 50°C and bake for 3 to 4 hours, crush them with a pulverizer, pass through a 40-mesh sieve, collect the tobacco dry powder, and seal and store it.

[0073] It should be noted that the present invention does not limit the order of the preparation steps, and it is only necessary to prepare extracts 1 and 3 first, prepare extract 2 based on extract 1, and prepare extract 4 based on extract 3. In actual production, extracts 1 and 3 will not all be used to prepare extracts 2 and 4, and extracts 1 and 3 will also participate in the batching process of endogenous spices of aromatic plants.

[0074] Through the combined use of four extraction methods, namely supercritical CO2 extraction, thermal cracking, enzymatic hydrolysis and Maillard reaction, the richness of the aroma of endogenous tobacco spices can be improved and the types of endogenous tobacco aroma can be increased.

[0075] In the technical solution of the present invention, by directional extraction of important tobacco aroma precursors and combining with the thermal reaction process, a rich variety of tobacco endogenous aromas is created to make up for the lack of aroma richness of existing tobacco endogenous spices. Not only are there rich varieties of tobacco endogenous aromas, but they are also highly compatible with tobacco flavors or electronic atomization liquids. It is configured into tobacco flavors or added to electronic atomization liquids, with high solubility, low threshold, and rich tobacco aroma, which can significantly improve the taste of tobacco flavors or electronic atomization liquids.

[0076] In any embodiment of the present invention, the aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1: the extraction pressure is 10-40 MPa. Within this pressure range, the yield of extract 1 can be increased.

[0077] In any embodiment of the present invention, the aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1: the extraction time is 0.5 to 6 hours. Within this time range, the yield of extract 1 can be increased.

[0078] In any embodiment of the present invention, the aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1: the extraction temperature is 40-60° C. Within this extraction temperature range, the yield of extract 1 is increased.

[0079] In any embodiment of the present invention, the aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain the extract 1: the flow rate of CO2 is 6 to 10 L / h. Within this flow rate range, the yield of the extract 1 is increased.

[0080] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, molecularly distilled, and the distillate is taken to obtain the extract 2: the freeze-drying temperature is -50 to -5° C. Within this freeze-drying temperature range, the yield of the extract 2 can be increased.

[0081] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2: the vacuum degree of freeze-drying is 10-20 Pa. Within this vacuum degree range, the yield of the extract 2 can be increased.

[0082] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2: the freeze-drying time is 0.5 to 2.5 hours. Within this freeze-drying time range, the yield of the extract 2 can be increased.

[0083] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2: the thermal cracking temperature is 100 to 300°C. Within this thermal cracking temperature range, the yield of the extract 2 can be increased. Specifically, the freeze-dried powder can be placed in a low-temperature aluminum retort pyrolysis furnace for thermal cracking treatment, and the volatile aroma components can be condensed and collected.

[0084] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2: the thermal cracking heating rate is 3 to 10°C / min. Within this thermal cracking heating rate range, the yield of the extract 2 can be increased.

[0085] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2: the thermal cracking time is 0.2 to 1.5 hours. Within this cracking time range, the yield of the extract 2 can be increased.

[0086] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, molecularly distilled, and the distillate is taken to obtain the extract 2: the temperature of the molecular distillation is 50 to 120°C. Within this molecular distillation range, the yield of the extract 2 can be increased. Specifically, propylene glycol can be added to the collected thermal cracking liquid, and the molecular distillation treatment can be performed after stirring. The heating temperature of the molecular distillation injector is 40 to 60°C, and the scraping speed is set to 150 to 350 rpm / min.

[0087] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2: the vacuum degree of the molecular distillation is 0.5 to 50 mbar. Within this molecular distillation vacuum degree range, the yield of the extract 2 can be increased.

[0088] In any embodiment of the present invention, the extract one is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract two: the feed flow rate of the molecular distillation is 50 to 150 mL / h. Within this feed flow rate range of the molecular distillation, the yield of the extract two can be increased.

[0089] In any embodiment of the present invention, the extract 1 is freeze-dried, thermally cracked, molecularly distilled, and the distillate is taken to obtain the extract 2: the molecular distillation time is 0.5 to 1.0 h. Within this molecular distillation time range, the yield of the extract 2 can be increased.

[0090] In any embodiment of the present invention, the aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration, and concentration to obtain extract three: the enzyme for enzymatic hydrolysis includes at least one of α-amylase and β-amylase. The use of at least one of the above enzymes can degrade the aroma precursor substances therein into monosaccharides, which is beneficial to the generation of aroma substances. Specifically, the aromatic plant dry powder can be mixed with a citric acid-sodium citrate buffer solution, and then the enzyme is added and stirred. After the enzymatic hydrolysis is stirred in a constant temperature water bath until the reaction is complete, it is stirred in a boiling water bath for 20 minutes to completely lose the enzyme activity, cooled, filtered, centrifuged in a centrifuge at 5000r / min for 5 minutes, the supernatant is combined, and vacuum concentrated.

[0091] In any embodiment of the present invention, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the enzymatic hydrolysis temperature is 50-65° C. Within this enzymatic hydrolysis temperature range, it is beneficial to exert maximum enzyme activity.

[0092] In any embodiment of the present invention, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the enzymatic hydrolysis time is 6 to 8 hours, and within this enzymatic hydrolysis time range, it can help to exert the maximum enzyme activity.

[0093] In any embodiment of the present invention, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the pH value of the enzymatic hydrolysis is 5.4-5.8. Within this pH value range of the enzymatic hydrolysis, it is beneficial to exert the maximum enzyme activity.

[0094] In any embodiment of the present invention, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the mass ratio of the enzymatic enzyme to the substrate is (1-3): (5--10). Within this mass ratio range, the biological activity of the enzyme and the substrate utilization rate can be effectively exerted.

[0095] In any embodiment of the present invention, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the temperature of vacuum concentration is 50-55°C. Within this vacuum concentration temperature range, a large loss of volatile and heat-sensitive components can be avoided.

[0096] In any embodiment of the present invention, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the vacuum degree of vacuum concentration is 30-50 mbar. Within this vacuum degree range of vacuum concentration, the concentration of the concentrate can be maximized.

[0097] In any embodiment of the present invention, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the vacuum concentration time is 1.5 to 3.0 hours. Within this vacuum concentration time range, the concentration effect can be maximized.

[0098] In any embodiment of the present invention, extract three is subjected to a Maillard reaction and membrane concentration to obtain extract four: extract three is subjected to a Maillard reaction with L-alanine. The use of L-alanine and extract three for the Maillard reaction can contribute to the formation of caramel aroma substances. In other embodiments of the present invention, extract three can also undergo a Maillard reaction with amino acids such as glycine, tyrosine, and valine. Specifically, extract three can be mixed with amino acids, mixed with an aqueous solution of propylene glycol, the pH is adjusted with 10% NaOH, a magnet is added, and the mixture is placed in a round-bottom flask equipped with a reflux condenser and a thermometer, and refluxed in a constant temperature magnetic stirrer. The reaction solution is filtered and concentrated to obtain extract four.

[0099] In any embodiment of the present invention, the extract three is subjected to Maillard reaction and membrane concentration to obtain extract four: the pH value of the Maillard reaction is 7.5-8.5. Within this pH value range of the Maillard reaction, it can help the formation of heterocyclic compounds.

[0100] In any embodiment of the present invention, the extract three is subjected to the Maillard reaction and membrane concentrated to obtain the extract four: the temperature of the Maillard reaction is 105-125°C. Within this temperature range of the Maillard reaction, it can help the formation of flavor substances. Too high a temperature will destroy amino acids and Maillard reaction substrates and even produce carcinogens; too low a temperature is not conducive to the Maillard reaction.

[0101] In any embodiment of the present invention, the extract three is subjected to Maillard reaction and membrane concentrated to obtain extract four: the time of the Maillard reaction is 2 to 5 hours, and within this time range of the Maillard reaction, the occurrence of the Maillard reaction can be facilitated.

[0102] In any embodiment of the present invention, the extract three is subjected to Maillard reaction and membrane concentration to obtain extract four: the water content in the Maillard reaction process is 5-25%. Within this water content range, the occurrence of the Maillard reaction can be facilitated.

[0103] In any embodiment of the present invention, the extract three is subjected to Maillard reaction and membrane concentration to obtain extract four: the membrane pore size of the membrane concentration is 50-200nm. Within this membrane pore size range, impurities with larger molecular weight can be filtered out, which is conducive to the collection of small molecular volatile aroma components.

[0104] In any embodiment of the present invention, the extract three is subjected to the Maillard reaction and membrane concentration to obtain the extract four: the molecular interception of the membrane concentration is greater than 25,000, and in this: within the molecular weight range of the membrane concentration, unnecessary aroma substances can be effectively intercepted. Specifically, the Maillard reaction liquid can be filtered through a ceramic membrane (primary membrane) with a pore size of 100nm. When the Maillard reaction liquid begins to bubble, 10% to 20% of the total weight of the Maillard reaction liquid is added. The solution passing through the membrane is called filtrate one, and the solution not passing through the membrane is called concentrated solution one; when no filtrate one flows out, the membrane treatment operation is stopped. The filtrate one is passed through an organic roll membrane (secondary membrane) with a molecular weight cutoff of 25,000. When the filtrate one system begins to bubble, 10% to 20% of the total weight of the filtrate one is added. The solution passing through the membrane is called filtrate two, and the solution not passing through the membrane is called concentrated solution two. When no filtrate two flows out, the membrane treatment operation is stopped, and the obtained filtrate two is extract four.

[0105] In any embodiment of the present invention, the mass ratio of extract 1, extract 2, extract 3 and extract 4 in the aromatic plant endogenous fragrance obtained by mixing extract 1, extract 2, extract 3 and extract 4 is (0.5-1): (0.8-1): (1-2): (0.5-1.5). Within this mass ratio range, aromatic plant endogenous fragrances with rich aromas can be created.

[0106] In any embodiment of the present invention, in the provision of aromatic plant dry powder, the aromatic plant includes at least one of tobacco, thyme, gardenia and sage. The selection of at least one of the above aromatic plants can provide a suitable aromatic smell.

[0107] The present invention also proposes an aromatic plant endogenous fragrance, which is prepared by the preparation method of the aromatic plant endogenous fragrance. The aromatic plant endogenous fragrance has all the technical solutions of the preparation method of the aromatic plant endogenous fragrance, and thus has all the beneficial effects of the preparation method of the aromatic plant endogenous fragrance, which will not be described in detail in the present invention.

[0108] The present invention also proposes an atomized flavor, comprising the aromatic plant endogenous flavor. The aromatic plant endogenous flavor is prepared by the preparation method of the aromatic plant endogenous flavor. The atomized flavor has all the technical solutions of the preparation method of the aromatic plant endogenous flavor, and thus has all the beneficial effects of the preparation method of the aromatic plant endogenous flavor, which will not be described in detail in the present invention.

[0109] The technical scheme of the present invention is further described in detail below in conjunction with specific examples. It should be understood that the following examples are only used to explain the present invention and are not used to limit the present invention. The aromatic plant tobacco is used as an example for description.

[0110] Example 1

[0111] Purchase aromatic plant tobacco dry powder and pass it through a 40-mesh sieve;

[0112] The tobacco powder was subjected to supercritical CO2 extraction to obtain an extract 1, wherein the extraction pressure was 10 MPa, the extraction time was 6 h, the extraction temperature was 50° C., and the extraction flow rate was 8 L / h;

[0113] The extract 1 was freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2, wherein the freeze-drying conditions were -50°C, 10Pa, and 1.0h, the thermal cracking conditions were 180°C, 3°C / min, and 0.5h, and the molecular distillation parameters were main evaporation temperature 50°C, system vacuum 0.5mbar, feed rate 150mL / h, and condensation temperature 4°C.

[0114] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the conditions for enzymatic hydrolysis were α-amylase and β-amylase, 50°C, 6h, pH 5.4, and a mass ratio of enzyme to substrate of 1:2, and the conditions for vacuum concentration were 50°C, 30mbar, 1h, and 4°C cold cycle;

[0115] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four, wherein the conditions for the Maillard reaction are amino acid L-alanine, 105°C, pH value 7.5, 5h, and water content 5%, and the conditions for membrane concentration are 50nm ceramic membrane and 30,000 molecular cutoff membrane;

[0116] Extract one, extract two, extract three and extract four are mixed in a mass ratio of 0.8:0.9:1.6:1 to obtain tobacco endogenous flavor.

[0117] Example 2

[0118] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, place the tobacco leaves in a 50℃ oven for 4 hours, crush them with a crusher, pass them through a 40-mesh sieve, collect the tobacco powder, and seal it for storage;

[0119] The tobacco powder was subjected to supercritical CO2 extraction to obtain an extract 1, wherein the extraction pressure was 40 MPa, the extraction time was 0.5 h, the extraction temperature was 40° C., and the extraction flow rate was 10 L / h;

[0120] Extract 1 was freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain Extract 2, wherein the freeze-drying conditions were -5°C, 20Pa, and 1.2h, the thermal cracking conditions were 300°C, 10°C / min, and 0.5h, and the molecular distillation parameters were 120°C, 50mbar, and 50mL / h;

[0121] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the conditions for enzymatic hydrolysis were α-amylase and β-amylase, 65°C, 8 hours, pH value 5.8, and a mass ratio of enzyme to substrate of 1:10, and the conditions for vacuum concentration were 55°C, 50 mbar, and 1.2 hours;

[0122] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four, wherein the conditions for the Maillard reaction are amino acid L-alanine, 125°C, pH value 8.5, 2h, water content 25%, and the conditions for membrane concentration are 200nm ceramic membrane and 30,000 molecular cutoff membrane;

[0123] Extract one, extract two, extract three and extract four are mixed in a mass ratio of 0.5:0.8:1:0.5 to obtain tobacco endogenous flavor.

[0124] Example 3

[0125] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, place the tobacco leaves in a 50℃ oven for 3 hours, crush them with a crusher, pass them through a 40-mesh sieve, collect the tobacco powder, and seal it for storage;

[0126] The tobacco powder was subjected to supercritical CO2 extraction to obtain an extract 1, wherein the extraction pressure was 20 MPa, the extraction time was 3 h, the extraction temperature was 60° C., and the extraction flow rate was 6 L / h;

[0127] Extract 1 was freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain Extract 2, wherein the freeze-drying conditions were -30°C, 15Pa, and 1.0h, the thermal cracking conditions were 280°C, 5°C / min, and 1h, and the molecular distillation parameters were 100°C, 10mbar, and 100mL / h;

[0128] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the conditions for enzymatic hydrolysis were α-amylase and β-amylase, 55° C., 7 h, pH 5.5, and a mass ratio of enzyme to substrate of 1:8, and the conditions for vacuum concentration were 52° C., 40 mbar, and 2.0 h;

[0129] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four, wherein the conditions for the Maillard reaction are amino acid glycine, 110°C, pH value 8, 4h, and water content 10%, and the conditions for membrane concentration are 100nm ceramic membrane and 30,000 molecular cutoff membrane;

[0130] Extract one, extract two, extract three and extract four are mixed in a mass ratio of 1:1:2:1.5 to obtain tobacco endogenous flavor.

[0131] Example 4

[0132] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, place the tobacco leaves in a 50℃ oven for 3.5 hours, crush them with a crusher, pass them through a 40-mesh sieve, collect the tobacco powder, and seal them for storage;

[0133] The tobacco powder was subjected to supercritical CO2 extraction to obtain an extract 1, wherein the extraction pressure was 30 MPa, the extraction time was 2 h, the extraction temperature was 45° C., and the extraction flow rate was 7 L / h;

[0134] Extract 1 was freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain Extract 2, wherein the freeze-drying conditions were -30°C, 13 Pa, and 2.5 h, the thermal cracking conditions were 250°C, 6°C / min, and 1.5 h, and the molecular distillation parameters were 50°C, 0.5 mbar, and 150 mL / h;

[0135] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the conditions for enzymatic hydrolysis were α-amylase and β-amylase, 53°C, 6.5h, pH value 5.6, and a mass ratio of enzyme to substrate of 1:10, and the conditions for vacuum concentration were 52°C, 35mbar, and 2.0h;

[0136] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four, wherein the conditions for the Maillard reaction are amino acid tyrosine, 110°C, pH value 7.8, 3h, and water content 15%, and the conditions for membrane concentration are 150nm ceramic membrane and 30,000 molecular cutoff membrane;

[0137] Extract one, extract two, extract three and extract four are mixed in a mass ratio of 0.5:0.8:1:0.5 to obtain tobacco endogenous flavor.

[0138] Example 5

[0139] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, place the tobacco leaves in a 50℃ oven for 3 hours, crush them with a crusher, pass them through a 40-mesh sieve, collect the tobacco powder, and seal it for storage;

[0140] The tobacco powder was subjected to supercritical CO2 extraction to obtain an extract 1, wherein the extraction pressure was 25 MPa, the extraction time was 5 h, the extraction temperature was 55° C., and the extraction flow rate was 9 L / h;

[0141] Extract 1 was freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain Extract 2, wherein the freeze-drying conditions were -40°C, 18 Pa, and 0.5 h, the thermal cracking conditions were 250°C, 7°C / min, and 0.2 h, and the molecular distillation parameters were 90°C, 40 mbar, and 120 mL / h;

[0142] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the conditions for enzymatic hydrolysis were α-amylase and β-amylase, 60°C, 7.5h, pH value 5.7, and a mass ratio of enzyme to substrate of 2:9, and the conditions for vacuum concentration were 54°C, 45mbar, and 1.5h;

[0143] Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four, wherein the conditions of Maillard reaction are amino acid tyrosine, 115°C, pH value 7.9, 4h, water content 18%, and the conditions of membrane concentration are 80nm ceramic membrane and 30,000 molecular cutoff membrane;

[0144] Extract one, extract two, extract three and extract four are mixed in a mass ratio of 1:1:2:1.5 to obtain tobacco endogenous flavor.

[0145] Comparative Example 1

[0146] The preparation method of the aromatic plant endogenous flavor of Comparative Example 1 is the same as that of Example 1 except that the first extract is freeze-dried, thermally cracked, molecularly distilled, and the distillate is taken to obtain the second extract.

[0147] Comparative Example 2

[0148] The preparation method of the aromatic plant endogenous flavor of Comparative Example 2 is the same as that of Example 1 except that the extract three is subjected to Maillard reaction and membrane concentration to obtain the extract four.

[0149] Comparative Example 3

[0150] The preparation method of endogenous aromatic plant flavors of Comparative Example 3 is the same as Example 1 except that "subjecting supercritical CO2 extraction to aromatic plant dry powder to obtain extract one; freeze-drying, thermal cracking, molecular distillation of extract one, and taking the distillate to obtain extract two".

[0151] Comparative Example 4

[0152] The preparation method of endogenous aromatic plant flavors in Comparative Example 4 is the same as Example 1 except that the steps of "enzymatically hydrolyzing the aromatic plant dry powder, filtering, and concentrating to obtain Extract 3; and subjecting Extract 3 to Maillard reaction and membrane concentration to obtain Extract 4" are omitted.

[0153] Comparative Example 5

[0154] The preparation method of endogenous fragrances of aromatic plants in Comparative Example 5 is the same as that in Example 1 except that “extract one is freeze-dried, thermally cracked, molecularly distilled, and the distillate is taken to obtain extract two; extract three is subjected to Maillard reaction and membrane concentration to obtain extract four”.

[0155] Performance Testing

[0156] 1. Analysis of aroma components of endogenous spices from aromatic plants

[0157] The endogenous fragrances of aromatic plants prepared in Examples 1 to 5 and Comparative Examples 1 to 5 were analyzed by GC-MS. The GC-MS test conditions were as follows: HP-INNOWAX capillary column, 30 m×0.2 mm (id)×0.33 μm (df), carrier gas was He, column flow rate was 0.6 mL / min, injection port temperature was 250° C.; programmed temperature, 60° C. (1 min)--210° C. (50 min); injection volume was 2 μL, split ratio was 10:1, ionization voltage was 70 eV, ionization mode was EI, ion source temperature was 200° C., transmission line temperature was 280° C., mass number range was 30-40 amu, Wiley spectral library was used for spectral retrieval and qualitative analysis, and gas chromatography area normalization method was used for quantitative analysis.

[0158] Among them, the types and contents of the endogenous aromatic plant spices prepared in Examples 1 to 5 and Comparative Examples 1 to 5 are shown in Table 1:

[0159] Table 1 Types of endogenous aromatic plant spices prepared in Examples 1 to 5 and Comparative Examples 1 to 5

[0160] Esters Aldehydes Ketones Acids Alcohols Phenols Heterocyclic Example 1 24 12 12 15 21 15 37 Example 2 19 13 7 7 16 12 29 Example 3 18 10 6 7 14 12 22 Example 4 22 14 9 9 19 14 24 Example 5 23 16 7 6 19 14 32 Comparative Example 1 5 9 3 3 9 4 22 Comparative Example 2 7 5 3 4 7 8 21 Comparative Example 3 11 6 5 2 4 8 16 Comparative Example 4 12 7 5 0 0 7 18 Comparative Example 5 5 3 4 5 10 2 8

[0161] From Table 1, we can see that:

[0162] Compared with Example 1, the contents of various volatile components in Comparative Example 1 are lower, among which the content of heterocyclic substances has the largest difference, indicating that thermal cracking treatment can enrich the content of heterocyclic substances in Example 1.

[0163] Compared with Example 1, the contents of various volatile aroma components in Comparative Example 2 were reduced, among which the content of heterocyclic substances was reduced the most, indicating that the Maillard reaction can significantly increase the content of heterocyclic aroma components in the product.

[0164] Compared with Example 1, the contents of various volatile aroma components in Comparative Example 3 were significantly reduced, indicating that the aroma precursors extracted by supercritical carbon dioxide and the Maillard reaction can significantly enrich the aroma of the product.

[0165] Compared with Example 1, the contents of various volatile aroma components in Comparative Example 4 were reduced, indicating that enzymatic hydrolysis and Maillard reaction can significantly increase the types and contents of aroma components.

[0166] Compared with Example 1, Comparative Example 5 only used supercritical carbon dioxide extraction and enzymatic hydrolysis technology to obtain Extract 1 and Extract 3, respectively, and the types of aroma components in the products were significantly reduced, especially phenolic substances and heterocyclic substances. This shows that the synergistic effect of thermal cracking technology and Maillard reaction can significantly increase the types and contents of aroma substances.

[0167] The above are only preferred embodiments of the present invention, and do not limit the patent scope of the present invention. For those skilled in the art, the present invention may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the patent protection scope of the present invention.

Claims

1. A method for preparing endogenous fragrances from aromatic plants, characterized in that: The following steps are involved: Provide aromatic plant dried powder; The aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1; The extract 1 is freeze-dried, thermally cracked, and molecularly distilled, and a distillate is taken to obtain an extract 2; The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration and concentration to obtain extract three; Extract three is subjected to Maillard reaction and membrane concentration to obtain extract four; The extract one, the extract two, the extract three and the extract four are mixed to obtain an aromatic plant endogenous flavor; In the step of freeze-drying, thermal cracking, molecular distilling, and taking the distillate to obtain the second extract, the thermal cracking temperature is 180-300°C; the thermal cracking heating rate is 3-10°C / min; and the thermal cracking time is 0.2-1.5 h; In the step of enzymatically hydrolyzing the aromatic plant dry powder, filtering, and concentrating to obtain the extract, the enzyme for enzymatic hydrolysis includes at least one of α-amylase and β-amylase; the mass ratio of the enzyme for enzymatic hydrolysis to the substrate is (1-3): (5-10); In the step of subjecting the extract three to Maillard reaction and membrane concentration to obtain the extract four, the extract three is subjected to a Maillard reaction with L-alanine; In the step of mixing extract one, extract two, extract three and extract four to obtain endogenous fragrance of aromatic plants, the mass ratio of extract one, extract two, extract three and extract four is (0.5-1): (0.8-1): (1-2): (0.5-1.5).

2. The method for preparing endogenous aromatic plant spices according to claim 1, characterized in that: The aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain an extract: The extraction pressure is 10-40 MPa; and / or, The extraction time is 0.5~6h; and / or, The extraction temperature is 40-60°C; and / or, The flow rate of CO2 is 6~10L / h.

3. The method for preparing endogenous aromatic plant spices according to claim 1, characterized in that: The extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the extract 2: The freeze-drying temperature is -50~-5°C; and / or, The vacuum degree of freeze drying is 10~20Pa; and / or, The freeze drying time is 0.5 to 2.5 h; and / or, The temperature of molecular distillation is 50-120°C; and / or, The vacuum degree of molecular distillation is 0.5~50mbar; and / or, The feed flow rate for molecular distillation is 50~150 mL / h.

4. The method for preparing endogenous aromatic plant spices according to claim 1, characterized in that: The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration, and concentration to obtain the following three extracts: The temperature of the enzymatic hydrolysis is 50-65°C; and / or, The enzymatic hydrolysis time is 6 to 8 hours; and / or, The pH value of the enzymatic hydrolysis is 5.4 to 5.8; and / or, The temperature of vacuum concentration is 50-55°C; and / or, The vacuum degree of vacuum concentration is 30~50mbar; and / or, The vacuum concentration time is 1.0~2.0h.

5. The method for preparing endogenous aromatic plant spices according to claim 1, characterized in that: The extract three is subjected to Maillard reaction and membrane concentration to obtain extract four: The pH value of the Maillard reaction is 7.5 to 8.5; and / or, The temperature of the Maillard reaction is 105-125°C; and / or, The Maillard reaction time is 2 to 5 hours; and / or, The moisture content during the Maillard reaction is 5-25%; and / or, The pore size of the membrane concentration is 50-200 nm; and / or, The molecular cutoff of the membrane concentration is greater than 25,000.

6. The method for preparing endogenous aromatic plant spices according to claim 1, characterized in that: In the aromatic plant dry powder provided, the aromatic plant includes at least one of tobacco, thyme, gardenia, sage and lemon balm.

7. An endogenous aromatic plant flavor, characterized in that: The aromatic plant endogenous fragrance is prepared by the preparation method of any one of claims 1 to 6.

8. An atomized flavor, characterized in that: The method comprises the endogenous fragrance of aromatic plants as described in claim 7.