Endogenous flavoring of aromatic plant and preparation method therefor, and e-liquid flavor concentrate

Abstract

A method for preparing an endogenous flavoring of an aromatic plant. The method comprises the following steps: providing the dry powder of an aromatic plant; subjecting the dry powder of the aromatic plant to supercritical CO2 extraction, so as to obtain an extract I; subjecting the extract I to freeze drying, thermal cracking and molecular distillation, and taking a distillate, so as to obtain an extract II; subjecting the dry powder of the aromatic plant to enzymolysis, filtration and concentration, so as to obtain an extract III; subjecting the extract III to the Maillard reaction and membrane concentration, so as to obtain extract IV; and mixing the extract I, the extract II, the extract III and the extract IV, so as to obtain an endogenous flavoring of the aromatic plant. In the preparation method, directional extraction of important aroma precursors of tobacco is conducted and is combined with a thermal reaction process, thereby creating new types of endogenous aroma of tobacco to enrich same and making up for the problems of insufficient aroma and poor abundance of existing endogenous flavorings for tobacco. In addition, provided are an endogenous flavoring of an aromatic plant prepared by using the preparation method and an E-liquid flavor concentrate comprising the endogenous flavoring of an aromatic plant.

Description

Aromatic plant endogenous fragrance, preparation method thereof, and atomized essence

[0001] This application claims priority to the Chinese patent application filed with the China Patent Office on February 20, 2024, with application number 202410189212.2, the entire contents of which are incorporated by reference into this application. Technical Field

[0002] The present application relates to the field of flavor technology, and in particular to an endogenous fragrance of an aromatic plant, a preparation method thereof, and an atomized flavor. Background Art

[0003] Aromatic plants, in a narrow sense, can be understood as plants that release fragrance. Broadly speaking, aromatic plants encompass a wider range of plants, encompassing those that have an odor or extractable aromatic compounds. These plants are rich in various aromatic compounds, including alcohols, esters, ethers, and ketones, and often provide direct or indirect sensory pleasure.

[0004] Aromatic plants contain a rich variety of chemical compounds, which can be broadly categorized into four main groups: aromatic compounds, medicinal compounds, nutritional compounds, and pigments. They also contain antioxidants and antimicrobial compounds. Aromatic compounds are their most significant characteristic and are often used as raw materials in the fragrance industry.

[0005] Plants naturally synthesize and release low-boiling-point, low-molecular-weight secondary metabolites, collectively known as plant volatile organic compounds (VOCs), which are emitted directly into the atmosphere. VOCs can be released from various plant parts, including flowers, fruits, stems, and leaves. VOCs comprise thousands of compounds, broadly categorized into three main groups: terpenes (isoprenes, monoterpenes, and sesquiterpenes), phenyl / phenylpropanoids, and fatty acid derivatives.

[0006] However, some aromatic plants contain a significant number of aroma precursors. These are generally not direct products of carbon or nitrogen metabolism, but are instead synthesized as non-volatile macromolecular compounds such as esters and terpenes. These compounds are then further decomposed by enzymes or non-enzymes to form volatile and semi-volatile organic compounds. For example, in the aromatic plant tobacco, aroma compounds can be divided into the following categories based on the relationship between aroma compounds and aroma precursors: glycosides, sugar esters, cypermethrin, lysine, and Maillard reaction products. Previous studies have shown that these aroma precursors release a large number of key aroma components during cigarette manufacturing, processing, and smoking, including neophytadiene, nicotine, solanone, damascenone, geranylacetone, megastigmatrienone, β-ionone, benzaldehyde, benzyl alcohol, and dihydroactinolactone.

[0007] Currently, industrial extraction of endogenous aromatic plant flavors primarily involves water extraction for the targeted extraction of polar aroma compounds; supercritical CO2 extraction for the targeted extraction of non-polar aroma compounds; and organic solvent extraction for the targeted extraction of intermediate- and weak-polar aroma compounds. These endogenous flavors typically utilize a single technique to extract aroma components from plant leaves or extracts, failing to fully capture the complex characteristics of the aromatic plant's inherent aroma compounds. For example, ultrasonic extraction of nicotine, hemicellulose, lignin, and cellulose from tobacco leaves, while relatively thorough, results in a complex process and a complex extract that hinders subsequent separation. Furthermore, the introduction of these compounds can degrade the tobacco's flavor. Technical issues

[0008] The main purpose of this application is to propose a method for preparing endogenous spices from aromatic plants, aiming to overcome the problems of insufficient aroma and excessive impurities in the existing technology of endogenous spices from aromatic plants. Technical Solutions

[0009] To achieve the above objectives, the present application proposes a method for preparing endogenous fragrances from aromatic plants, comprising the following steps:

[0010] Provide aromatic plant dried powder;

[0011] The aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1;

[0012] The extract 1 is freeze-dried, thermally cracked, and molecularly distilled, and the distillate is taken to obtain the extract 2;

[0013] The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration, and concentration to obtain extract three;

[0014] Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain extract 4;

[0015] The extract one, the extract two, the extract three and the extract four are mixed to obtain the aromatic plant endogenous fragrance.

[0016] In one embodiment, the aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain an extract:

[0017] The extraction pressure is 10-40 MPa; and / or,

[0018] The extraction time is 0.5 to 6 hours; and / or,

[0019] The extraction temperature is 40-60°C; and / or,

[0020] The flow rate of CO2 is 6~10L / h.

[0021] In one embodiment, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the following extract:

[0022] The freeze-drying temperature is -50~-5°C; and / or,

[0023] The vacuum degree of freeze drying is 10-20 Pa; and / or,

[0024] The freeze drying time is 0.5 to 2.5 hours; and / or,

[0025] The temperature of thermal cracking is 100-300°C; and / or,

[0026] The heating rate of thermal cracking is 3-10°C / min; and / or,

[0027] The thermal cracking time is 0.2 to 1.5 hours; and / or,

[0028] The temperature of molecular distillation is 50-120°C; and / or,

[0029] The vacuum degree of molecular distillation is 0.5~50mbar; and / or,

[0030] The feed flow rate for molecular distillation was 50~150 mL / h.

[0031] In one embodiment, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain the following extracts:

[0032] The enzymatic enzyme comprises at least one of α-amylase and β-amylase; and / or,

[0033] The temperature of the enzymatic hydrolysis is 50-65°C; and / or,

[0034] The enzymatic hydrolysis time is 6 to 8 hours; and / or,

[0035] The pH value of the enzymatic hydrolysis is 5.4 to 5.8; and / or,

[0036] The mass ratio of enzyme to substrate in enzymatic hydrolysis is (1-3): (5-10); and / or,

[0037] The temperature of vacuum concentration is 50-55°C; and / or,

[0038] The vacuum degree of vacuum concentration is 30~50mbar; and / or,

[0039] The vacuum concentration time is 1.0~2.0h.

[0040] In one embodiment, the extract three is subjected to a Maillard reaction and membrane concentration to obtain the extract four:

[0041] Extract three is subjected to a Maillard reaction with L-alanine; and / or,

[0042] The pH value of the Maillard reaction is 7.5 to 8.5; and / or,

[0043] The temperature of the Maillard reaction is 105-125°C; and / or,

[0044] The Maillard reaction time is 2 to 5 hours; and / or,

[0045] The moisture content during the Maillard reaction is 5-25%; and / or,

[0046] The pore size of the membrane concentration membrane is 50-200 nm; and / or,

[0047] The molecular cutoff of the membrane concentration is greater than 25,000.

[0048] In one embodiment, the extract 1, the extract 2, the extract 3 and the extract 4 are mixed to obtain the aromatic plant endogenous fragrance:

[0049] The mass ratios of extract 1, extract 2, extract 3 and extract 4 are (0.5~1):(0.8~1):(1~2):(0.5~1.5).

[0050] In one embodiment, the aromatic plant dry powder provided includes at least one of tobacco, thyme, gardenia, sage and lemon balm.

[0051] The present application also proposes an aromatic plant endogenous fragrance, which is prepared by the preparation method of the aromatic plant endogenous fragrance.

[0052] The present application also proposes an atomized essence, comprising the endogenous fragrance of the aromatic plant. Beneficial effects

[0053] The preparation method of aromatic plant endogenous fragrances of the present application creates a rich variety of tobacco endogenous aromas through the targeted extraction of important tobacco aroma precursors, combined with a thermal reaction process, to make up for the lack of aroma richness of existing tobacco endogenous fragrances. Not only is the variety of tobacco endogenous aroma rich, but it also has great adaptability with tobacco flavors or electronic atomization liquids. When it is configured into tobacco flavors or added to electronic atomization liquids, it has high solubility, low threshold, and rich tobacco aroma, which can significantly improve the taste of tobacco flavors or electronic atomization liquids. Modes for Carrying Out the Invention

[0054] In order to make the purpose, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. If specific conditions are not specified in the embodiments, they are carried out according to conventional conditions or the conditions recommended by the manufacturer. If the reagents or instruments used are not specified by 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, it includes scheme A, or scheme B, or schemes that A and B meet simultaneously. In addition, the technical solutions between the various embodiments can be combined with each other, but must be based on the ability of those of ordinary skill in the art 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 this application. Based on the embodiments in this application, all other embodiments obtained by those of ordinary skill in the art without making creative work are within the scope of protection of this application.

[0055] Aromatic plants, in a narrow sense, can be understood as plants that release fragrance. Broadly speaking, aromatic plants encompass a wider range of plants, encompassing those that have an odor or extractable aromatic compounds. These plants are rich in various aromatic compounds, including alcohols, esters, ethers, and ketones, and often provide direct or indirect sensory pleasure.

[0056] Aromatic plants contain a rich variety of chemical compounds, which can be broadly categorized into four main groups: aromatic compounds, medicinal compounds, nutritional compounds, and pigments. They also contain antioxidants and antimicrobial compounds. Aromatic compounds are their most significant characteristic and are often used as raw materials in the fragrance industry.

[0057] Plants naturally synthesize and release low-boiling-point, low-molecular-weight secondary metabolites, collectively known as plant volatile organic compounds (VOCs), which are emitted directly into the atmosphere. VOCs can be released from various plant parts, including flowers, fruits, stems, and leaves. VOCs comprise thousands of compounds, broadly categorized into three main groups: terpenes (isoprenes, monoterpenes, and sesquiterpenes), phenyl / phenylpropanoids, and fatty acid derivatives.

[0058] However, some aromatic plants contain a significant number of aroma precursors. These are generally not direct products of carbon or nitrogen metabolism, but are instead synthesized as non-volatile macromolecular compounds such as esters and terpenes. These compounds are then further decomposed by enzymes or non-enzymes to form volatile and semi-volatile organic compounds. For example, in the aromatic plant tobacco, aroma compounds can be divided into the following categories based on the relationship between aroma compounds and aroma precursors: glycosides, sugar esters, cypermethrin, lysine, and Maillard reaction products. Previous studies have shown that these aroma precursors release a large number of key aroma components during cigarette manufacturing, processing, and smoking, including neophytadiene, nicotine, solanone, damascenone, geranylacetone, megastigmatrienone, β-ionone, benzaldehyde, benzyl alcohol, and dihydroactinolactone.

[0059] Currently, industrial extraction of endogenous aromatic plant flavors primarily involves water extraction for the targeted extraction of polar aroma compounds; supercritical CO2 extraction for the targeted extraction of non-polar aroma compounds; and organic solvent extraction for the targeted extraction of intermediate- and weak-polar aroma compounds. These endogenous flavors typically utilize a single technique to extract aroma components from plant leaves or extracts, failing to fully capture the complex characteristics of the aromatic plant's inherent aroma compounds. For example, ultrasonic extraction of nicotine, hemicellulose, lignin, and cellulose from tobacco leaves, while relatively thorough, results in a complex process and a complex extract that hinders subsequent separation. Furthermore, the introduction of these compounds can degrade the tobacco's flavor.

[0060] Currently, a single technique is used to extract low-boiling-point, volatile compounds from aromatic plants. Aromatic plants contain numerous aroma precursors that, under specific conditions such as the relatively low-temperature Maillard reaction, high-temperature thermal cracking, or microbial fermentation and enzymatic hydrolysis, produce a richer and more diverse array of aroma components. These aroma components and their application effects more closely resemble the natural aroma of aromatic plants during combustion. However, there has been no targeted research on the endogenous aroma components of important aroma precursors in aromatic plants during thermal reactions.

[0061] In view of this, the present application proposes a method for preparing endogenous spices from aromatic plants, aiming to overcome the problems in the prior art of insufficient aroma and excessive impurities in endogenous spices from aromatic plants.

[0062] A method for preparing endogenous aromatic plant spices comprises the following steps:

[0063] Provide aromatic plant dried powder;

[0064] The aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain extract 1;

[0065] The extract 1 is freeze-dried, thermally cracked, and molecularly distilled, and the distillate is taken to obtain the extract 2;

[0066] The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration, and concentration to obtain extract three;

[0067] Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain extract 4;

[0068] The extract one, the extract two, the extract three and the extract four are mixed to obtain the aromatic plant endogenous fragrance.

[0069] The extracts obtained by supercritical CO2 extraction are mainly carotenoids, such as α-carotene, β-carotene, violaxanthin and neoxanthin. These substances are important aroma precursors and provide a rich variety of aroma components under specific conditions.

[0070] The first extract is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the second extract. The obtained extract mainly contains small molecular volatile substances, such as esters, acids, phenols and other substances, which can provide rich top notes.

[0071] 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, sugars themselves are the precursors for the formation of aroma. On the other hand, these substances can provide endogenous Maillard reaction substrates, thereby promoting the occurrence and progress of the Maillard reaction.

[0072] Extract three is subjected to a 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, and 2-ethylpyrazine, which can provide roasted, nutty flavor characteristics.

[0073] It should be noted that the aromatic plant dry powder can be purchased or prepared by oneself. In any embodiment of the present application, taking tobacco leaves as an example, it can be prepared by oneself using the following preparation method: use a soft brush to clean off 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 grinder, pass them through a 40-mesh sieve, collect the tobacco dry powder, and seal and store them.

[0074] It should be noted that the present application does not limit the order of the preparation steps. 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. Extracts 1 and 3 will also participate in the ingredient process of endogenous aromatic plants.

[0075] By combining supercritical CO2 extraction, thermal cracking, enzymatic hydrolysis, and Maillard reaction, the richness of tobacco's endogenous spice aroma can be improved and the types of tobacco's endogenous aroma can be increased.

[0076] In the technical solution of this application, through the targeted extraction of important tobacco aroma precursors and combined with a thermal reaction process, a rich variety of endogenous tobacco aromas is created, compensating for the lack of aroma richness of existing endogenous tobacco spices. Not only is the variety of endogenous tobacco aroma rich, but it also has great compatibility with tobacco flavors or electronic atomization liquids. When configured into tobacco flavors or added to electronic atomization liquids, it has high solubility, low threshold, and rich tobacco aroma, which can significantly improve the taste of tobacco flavors or electronic atomization liquids.

[0077] In any embodiment of the present application, 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.

[0078] In any embodiment of the present application, 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.

[0079] In any embodiment of the present application, 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.

[0080] In any embodiment of the present application, the aromatic plant dry powder is subjected to supercritical CO2 extraction to obtain Extract 1: the CO2 flow rate is 6-10 L / h. Within this flow rate range, the yield of Extract 1 is improved.

[0081] In any embodiment of the present application, the first extract is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the second extract: the freeze-drying temperature is -50 to -5° C. Within this freeze-drying temperature range, the yield of the second extract can be increased.

[0082] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the extract 2: the vacuum degree of freeze-drying is 10~20Pa. Within this vacuum degree range, the yield of the extract 2 can be improved.

[0083] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the extract 2: the freeze-drying time is 0.5~2.5h. Within this freeze-drying time range, the yield of the extract 2 can be improved.

[0084] In any embodiment of the present application, extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain extract 2. The thermal cracking temperature is 100-300°C. Within this thermal cracking temperature range, the yield of extract 2 can be increased. Specifically, the freeze-dried powder can be placed in a low-temperature aluminum retort pyrolysis furnace for thermal cracking, and the volatile aroma components can be condensed and collected.

[0085] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the extract 2: the thermal cracking heating rate is 3~10℃ / min. Within this thermal cracking heating rate range, the yield of the extract 2 can be improved.

[0086] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the extract 2: the thermal cracking time is 0.2~1.5h. Within this cracking time range, the yield of the extract 2 can be improved.

[0087] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the extract 2: the molecular distillation temperature is 50-120°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, stirred, and then molecularly distilled. The heating temperature of the molecular distillation injector is 40-60°C, and the scraping speed is set to 150-350 rpm / min.

[0088] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain the extract 2: the vacuum degree of the molecular distillation is 0.5~50mbar. Within this molecular distillation vacuum degree range, the yield of the extract 2 can be improved.

[0089] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate to obtain an extract 2: the feed flow rate of the molecular distillation is 50~150 mL / h. Within this feed flow rate range of the molecular distillation, the yield of the extract 2 can be improved.

[0090] In any embodiment of the present application, the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain a distillate 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.

[0091] In any embodiment of the present application, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated 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 production of aroma-producing 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, and centrifuged in a centrifuge at 5000 r / min for 5 minutes. The supernatants are combined and concentrated in vacuo.

[0092] In any embodiment of the present application, 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 conducive to exerting maximum enzyme activity.

[0093] In any embodiment of the present application, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the enzymatic hydrolysis time is 6 to 8 hours, which can help to maximize the enzyme activity within this enzymatic hydrolysis time range.

[0094] In any embodiment of the present application, 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 conducive to exerting maximum enzyme activity.

[0095] In any embodiment of the present application, 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.

[0096] In any embodiment of the present application, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the vacuum concentration temperature is 50~55°C. Within this vacuum concentration temperature range, a large loss of volatile and heat-sensitive components can be avoided.

[0097] In any embodiment of the present application, 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.

[0098] In any embodiment of the present application, the aromatic plant dry powder is enzymatically hydrolyzed, filtered, and concentrated to obtain extract three: the vacuum concentration time is 1.5~3.0h. Within this vacuum concentration time range, the concentration effect can be maximized.

[0099] In any embodiment of the present application, extract three is subjected to a Maillard reaction and membrane concentration to obtain extract four: extract three undergoes a Maillard reaction with L-alanine. Selecting L-alanine for the Maillard reaction with extract three can facilitate the production of caramel-like aroma substances. In other embodiments of the present application, 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 adjusted with 10% NaOH, a magnet added, and 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.

[0100] In any embodiment of the present application, the extract three is subjected to a Maillard reaction and membrane concentrated to obtain an 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 be conducive to the formation of heterocyclic compounds.

[0101] In any embodiment of the present application, the extract three is subjected to a Maillard reaction and membrane concentrated to obtain an 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 progress of the Maillard reaction.

[0102] In any embodiment of the present application, the extract three is subjected to a Maillard reaction and membrane concentrated to obtain an extract four: the Maillard reaction time is 2 to 5 hours. Within this Maillard reaction time range, the occurrence of the Maillard reaction can be facilitated.

[0103] In any embodiment of the present application, the extract three is subjected to a Maillard reaction and membrane concentrated to obtain an 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.

[0104] In any embodiment of the present application, the extract three is subjected to a Maillard reaction and membrane concentrated 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.

[0105] In any embodiment of the present application, extract three is subjected to a Maillard reaction and membrane concentration to obtain extract four: the molecular weight cutoff of the membrane concentration is greater than 25,000. Here, within the molecular weight range of the membrane concentration, unnecessary aroma substances can be effectively intercepted. Specifically, the Maillard reaction solution can be filtered through a ceramic membrane with a pore size of 100 nm (primary membrane). When the Maillard reaction solution begins to bubble, 10% to 20% of the total weight of the Maillard reaction solution is added. The solution that passes through the membrane is called filtrate one, and the solution that does not pass through the membrane is called concentrate one. When no filtrate one flows out, the membrane treatment operation is stopped. Filtrate one is passed through an organic spiral membrane with a molecular weight cutoff of 25,000 (secondary membrane). When the filtrate one system begins to bubble, 10% to 20% of the total weight of the filtrate one is added. The solution that passes through the membrane is called filtrate two, and the solution that does not pass through the membrane is called concentrate two. When no filtrate two flows out, the membrane treatment operation is stopped, and the resulting filtrate two is extract four.

[0106] In any embodiment of the present application, the mass ratio of extract 1, extract 2, extract 3, and extract 4 to obtain the aromatic plant endogenous fragrance is (0.5-1): (0.8-1): (1-2): (0.5-1.5). Within this mass ratio range, an aromatic plant endogenous fragrance with a rich variety of aromas can be created.

[0107] In any embodiment of the present application, in the aromatic plant dry powder provided, 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.

[0108] This application also proposes an aromatic plant endogenous fragrance, produced by the aforementioned method for preparing an aromatic plant endogenous fragrance. The aromatic plant endogenous fragrance incorporates all the technical solutions of the aforementioned method for preparing an aromatic plant endogenous fragrance, and thus possesses all the beneficial effects of the aforementioned method for preparing an aromatic plant endogenous fragrance. This application will not further elaborate on these details.

[0109] This application also provides an atomized flavoring agent comprising the aforementioned endogenous aromatic plant fragrance. The endogenous aromatic plant fragrance is produced by the aforementioned method for preparing endogenous aromatic plant fragrances. This atomized flavoring agent incorporates all the technical aspects of the aforementioned method for preparing endogenous aromatic plant fragrances, and thus possesses all the beneficial effects of the aforementioned method. This application will not further elaborate on these aspects.

[0110] The technical solution of the present application will be further described in detail below with reference to specific examples. It should be understood that the following examples are only used to explain the present application and are not intended to limit the present application.

[0111] Example 1

[0112] Purchase aromatic plant tobacco dry powder and pass it through a 40-mesh sieve;

[0113] 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;

[0114] 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, 10 Pa, and 1.0 h, the thermal cracking conditions were 180°C, 3°C / min, and 0.5 h, and the molecular distillation parameters were main evaporation temperature 50°C, system vacuum 0.5 mbar, feed rate 150 mL / h, and condensation temperature 4°C.

[0115] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain an extract three, wherein the enzymatic hydrolysis conditions were α-amylase and β-amylase, 50°C, 6 hours, pH 5.4, and a mass ratio of enzyme to substrate of 1:2, and the vacuum concentration conditions were 50°C, 30 mbar, 1 hour, and a cold cycle of 4°C;

[0116] Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain Extract 4, wherein the Maillard reaction conditions were as follows: amino acid L-alanine, 105°C, pH 7.5, 5h, and 5% water content; and the membrane concentration conditions were a 50nm ceramic membrane with a 30,000 molecule cut-off capacity.

[0117] 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.

[0118] Example 2

[0119] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, bake the tobacco leaves in a 50℃ oven for 4 hours, crush them with a grinder, pass them through a 40-mesh sieve, collect the tobacco powder, and seal it for storage;

[0120] 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;

[0121] 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, 20 Pa, and 1.2 h, the thermal cracking conditions were 300°C, 10°C / min, and 0.5 h, and the molecular distillation parameters were 120°C, 50 mbar, and 50 mL / h;

[0122] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the enzymatic hydrolysis conditions were α-amylase and β-amylase, 65°C, 8 hours, pH 5.8, and a mass ratio of enzyme to substrate of 1:10, and the vacuum concentration conditions were 55°C, 50 mbar, and 1.2 hours;

[0123] Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain Extract 4, wherein the Maillard reaction conditions were as follows: amino acid L-alanine, 125°C, pH 8.5, 2h, and a water content of 25%, and the membrane concentration conditions were a 200nm ceramic membrane with a 30,000 molecule cut-off capacity.

[0124] 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.

[0125] Example 3

[0126] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, bake the tobacco leaves in a 50℃ oven for 3 hours, crush them with a grinder, pass them through a 40-mesh sieve, collect the tobacco powder, and seal it for storage;

[0127] 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;

[0128] 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, 15 Pa, and 1.0 h, the thermal cracking conditions were 280°C, 5°C / min, and 1 h, and the molecular distillation parameters were 100°C, 10 mbar, and 100 mL / h;

[0129] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the enzymatic hydrolysis conditions were α-amylase and β-amylase, 55°C, 7 hours, pH 5.5, and a mass ratio of enzyme to substrate of 1:8, and the vacuum concentration conditions were 52°C, 40 mbar, and 2.0 hours;

[0130] Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain extract 4, wherein the Maillard reaction conditions were as follows: amino acid glycine, 110°C, pH 8, 4h, and a water content of 10%, and the membrane concentration conditions were a 100nm ceramic membrane with a 30,000 molecule cut-off capacity membrane;

[0131] 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.

[0132] Example 4

[0133] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, bake the tobacco leaves in a 50℃ oven for 3.5 hours, crush them with a grinder, pass them through a 40-mesh sieve, collect the tobacco powder, and seal it for storage;

[0134] 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;

[0135] 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;

[0136] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain extract three, wherein the enzymatic hydrolysis conditions were α-amylase and β-amylase, 53°C, 6.5h, pH 5.6, and a mass ratio of enzyme to substrate of 1:10, and the vacuum concentration conditions were 52°C, 35mbar, and 2.0h;

[0137] Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain extract 4, wherein the conditions for the Maillard reaction were as follows: amino acid tyrosine, 110°C, pH 7.8, 3h, and a water content of 15%, and the conditions for membrane concentration were a 150nm ceramic membrane with a 30,000 molecule cut-off capacity.

[0138] 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.

[0139] Example 5

[0140] Use a soft brush to clean the dust, sand and other impurities on the tobacco leaves, bake the tobacco leaves in a 50℃ oven for 3 hours, crush them with a grinder, pass them through a 40-mesh sieve, collect the tobacco powder, and seal it for storage;

[0141] 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;

[0142] 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;

[0143] The tobacco powder was enzymatically hydrolyzed, filtered, and concentrated to obtain an extract three, wherein the enzymatic hydrolysis conditions were α-amylase and β-amylase, 60°C, 7.5 hours, pH 5.7, and a mass ratio of enzyme to substrate of 2:9, and the vacuum concentration conditions were 54°C, 45 mbar, and 1.5 hours;

[0144] Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain Extract 4, wherein the conditions for the Maillard reaction were as follows: amino acid tyrosine, 115°C, pH 7.9, 4 hours, and a water content of 18%, and the conditions for membrane concentration were an 80 nm ceramic membrane with a 30,000 molecule cut-off capacity.

[0145] 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.

[0146] Comparative Example 1

[0147] The preparation method of the aromatic plant endogenous fragrance 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.

[0148] Comparative Example 2

[0149] The preparation method of the aromatic plant endogenous fragrance of Comparative Example 2 is the same as that of Example 1 except that the step of "subjecting the third extract to a Maillard reaction and concentrating the extract with a membrane to obtain the fourth extract" is omitted.

[0150] Comparative Example 3

[0151] The preparation method of the aromatic plant endogenous fragrance of Comparative Example 3 is the same as that of Example 1 except that “subjecting the aromatic plant dry powder to supercritical CO2 extraction to obtain Extract 1; and subjecting the Extract 1 to freeze-drying, thermal cracking, and molecular distillation to obtain the distillate to obtain Extract 2” is omitted.

[0152] Comparative Example 4

[0153] The preparation method of the aromatic plant endogenous fragrance of Comparative Example 4 is the same as that of 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.

[0154] Comparative Example 5

[0155] The preparation method of the aromatic plant endogenous fragrance of Comparative Example 5 is the same as that of Example 1 except that “the extract 1 is freeze-dried, thermally cracked, and molecularly distilled to obtain the distillate to obtain the extract 2; and the extract 3 is subjected to the Maillard reaction and membrane concentration to obtain the extract 4” is not included.

[0156] Performance Testing

[0157] 1. Analysis of aroma components of endogenous spices from aromatic plants

[0158] 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, transfer 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.

[0159] The types and contents of the aromatic plant endogenous spices prepared in Examples 1 to 5 and Comparative Examples 1 to 5 are shown in Table 1:

[0160] Table 1 Types of aromatic plant endogenous spices prepared in Examples 1 to 5 and Comparative Examples 1 to 5

[0161] Esters Aldehydes Ketones Acids Alcohols Phenols Heterocyclics Example 1 24121215211537 Example 2 191377161229 Example 3 181067141222 Example 4 221499191424 Example 5 231676191432 Comparative Example 1 59339422 Comparative Example 2 75347821 Comparative Example 3 116524816 Comparative Example 4 127500718 Comparative Example 5 53451028

[0162] From Table 1 we can see that:

[0163] 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.

[0164] 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.

[0165] 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.

[0166] 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.

[0167] Compared to Example 1, Comparative Example 5, which used only supercritical carbon dioxide extraction and enzymatic hydrolysis to produce Extracts 1 and 3, respectively, showed a significant reduction in the variety of aroma components, particularly phenolic and heterocyclic compounds. This demonstrates that the synergistic effect of thermal cracking and the Maillard reaction can significantly increase the variety and content of aroma compounds.

[0168] The above are merely examples of the present application and are not intended to limit the scope of the present invention. Various modifications and variations are possible for those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present application shall be included within the scope of the present invention.

Claims

1. A method for preparing endogenous fragrances from aromatic plants, wherein: The method comprises the following steps: Provide aromatic plant dry 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 the distillate is taken to obtain the extract 2; The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration, and concentration to obtain extract three; Extract 3 was subjected to a Maillard reaction and membrane concentration to obtain extract 4; The extract one, the extract two, the extract three and the extract four are mixed to obtain the aromatic plant endogenous fragrance.

2. The method for preparing the aromatic plant endogenous spices according to claim 1, wherein 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 to 6 hours; 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 the aromatic plant endogenous spices according to claim 1, wherein The extract 1 is freeze-dried, thermally cracked, and molecularly distilled, and the distillate is taken to obtain the extract 2: The freeze-drying temperature is -50~-5°C; and / or, The vacuum degree of freeze drying is 10-20 Pa; and / or, The freeze-drying time is 0.5 to 2.5 hours; and / or, The temperature of thermal cracking is 180-300°C; and / or, The heating rate of thermal cracking is 3-10°C / min; and / or, The thermal cracking time is 0.2 to 1.5 hours; 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 was 50~150 mL / h.

4. The method for preparing the aromatic plant endogenous spices according to claim 1, wherein The aromatic plant dry powder is subjected to enzymatic hydrolysis, filtration, and concentration to obtain the following extracts: The enzymatic enzyme comprises at least one of α-amylase and β-amylase; and / or, 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 mass ratio of enzyme to substrate in enzymatic hydrolysis is (1-3): (5-10); 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 the aromatic plant endogenous spices according to claim 1, wherein The extract three is subjected to a Maillard reaction and membrane concentration to obtain an extract four: Extract three is subjected to a Maillard reaction with L-alanine; and / or, 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 membrane is 50-200 nm; and / or, The molecular cutoff of the membrane concentration is greater than 25,000.

6. The method for preparing the aromatic plant endogenous spices according to claim 1, wherein: The extract 1, the extract 2, the extract 3 and the extract 4 are mixed to obtain the aromatic plant endogenous fragrance: The mass ratios of extract 1, extract 2, extract 3 and extract 4 are (0.5~1):(0.8~1):(1~2):(0.5~1.5).

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

8. An endogenous fragrance of an aromatic plant, wherein: The aromatic plant endogenous fragrance is prepared by the preparation method of the aromatic plant endogenous fragrance according to any one of claims 1 to 7.

9. An atomized flavor, wherein: The atomized flavor comprises the aromatic plant endogenous flavor according to claim 8.