A plant seed dry distillation refined product, and a preparation method and application thereof

Abstract

The application discloses a plant seed dry distillation refined product and a preparation method and application thereof. The dry distillation refined product is obtained by the following steps: carrying out dry distillation reaction on plant seeds to obtain a dry distillation seed raw material; uniformly mixing the dry distillation seed raw material with a solvent and then carrying out homogenization treatment, and then carrying out solid-liquid separation, collecting supernatant, and obtaining a dry distillation seed raw material extract; and carrying out molecular distillation on the dry distillation seed raw material extract and collecting a light component fraction. The dry distillation refined product takes cocoa beans or coffee beans as raw materials, greatly improves the content and types of aroma substances based on the synergistic effect between steps, especially the flavor characteristics of cocoa or coffee itself, and is applied to a heat-not-burn cigarette as a tobacco flavor, so that the heat-not-burn cigarette can release a flavor with obvious cocoa aroma or coffee aroma characteristics, and also has rich and mellow burnt aroma, and the richness and thickness of the aroma are greatly improved.

Description

Technical Field

[0001] This invention relates to a plant seed dry distillation refined product, specifically to a plant seed dry distillation refined product, its preparation method and application, belonging to the field of fragrance and flavor technology. Background Technology

[0002] Roasted and caramel-flavored heated cigarettes primarily utilize low-temperature heating technology. Specifically designed for coffee and cocoa sheets, this technology precisely heats the sheets using temperature control, releasing the aromatic substances and nicotine present in the coffee and cocoa to create smoke. This process heats the tobacco leaves to a level sufficient to release their flavor without igniting them. Its taste is closest to traditional cigarettes and is expected to be the first to be accepted by smokers. Comparative analysis of heated cigarettes and traditional cigarettes reveals that the fundamental sensory difference lies in their different heating temperatures. Traditional cigarettes involve combustion, with aroma compounds derived from the transfer of aroma compounds already present in coffee and cocoa, as well as from complex thermal decomposition reactions during combustion. Whether it's the transfer of aroma compounds or the production of aroma through thermal decomposition, the aroma compounds primarily originate from the pyrolysis / distillation zone of the cigarette during combustion, at temperatures ranging from approximately 250 to 600°C. Heated cigarettes, on the other hand, involve heating, not combustion, with heating temperatures generally not exceeding 300°C. The internal temperature of the cigarette is even lower. Therefore, compared to traditional cigarettes, heated cigarettes, due to their lower temperature, do not reach the aroma-producing temperature of traditional cigarettes, resulting in significantly less aroma richness. Consequently, external extracts are needed to enhance the smoke quality.

[0003] Currently, the main method for preparing coffee flavorings is by blending coffee extracts with different flavor bases. A large portion of these flavorings are used in beverages and food. For example, patent CN 106260372 A discloses a coffee flavoring composed of 15 compounds, including coffee extract, benzyl alcohol, furfuryl mercaptan, acetoin, terpinene-4-ol, and butyric acid. Patent CN 105062673 B discloses a coffee flavoring containing lysine, methionine, phenylalanine, tyrosine, fructose, glucose, and solvents. This coffee flavoring is used in cigars to create cigarettes with a coffee aroma. Currently, the application of coffee flavorings in beverages, food, and cigars mainly involves blending coffee extracts with different monomers; research on the preparation process from raw coffee beans to coffee extracts is still relatively limited.

[0004] Currently, the main method for preparing cocoa flavoring is by blending cocoa extract with different flavor bases. A large portion of these flavorings are used in beverages and food. Patent CN101445766A discloses a method using cocoa powder as a raw material, involving mixing, separation, enzymatic hydrolysis, and concentration to obtain a cocoa flavoring. Patent CN103960770B discloses a cocoa flavoring formula including cocoa extract, ketone flavorings, natural plant extracts, lipid flavorings, and diluents, and uses the resulting cocoa flavoring in cigars to create cigars with a cocoa aroma. Currently, the application of cocoa flavorings in beverages, food, and cigars mainly involves blending cocoa extract with different monomers; research on the preparation process from the source cocoa bean to cocoa extract is still relatively limited.

[0005] In summary, the aromas of coffee and cocoa extracts obtained through existing technologies are relatively weak, especially lacking the base aromas of coffee and cocoa, which cannot meet the requirements for flavorings needed for heated cigarettes. Summary of the Invention

[0006] To address the problems existing in the prior art, the first objective of this invention is to provide a plant seed dry distillation refined product. This dry distillation refined product uses cocoa beans or coffee beans as raw materials. Based on the synergistic effect between each step, it significantly increases the content and variety of aroma substances, especially the flavor characteristics of cocoa or coffee itself. Under low temperature conditions, while ensuring the release of flavors with obvious cocoa or coffee aroma characteristics, it also imparts a rich caramel aroma, greatly improving the richness and fullness of the aroma.

[0007] The second objective of this invention is to provide a method for preparing a refined product from the dry distillation of plant seeds. This method first induces caramelization and Maillard reactions in carbohydrates, proteins, lipids, and organic acids in cocoa or coffee beans through a dry distillation reaction, thereby producing caramel and roasted aromas on top of the cocoa or coffee aroma. Then, the product undergoes homogenization and molecular distillation to further extract phenolic and ester compounds from the tobacco raw material. Specifically, as the dry distillation temperature increases, the content of aroma compounds such as pyrazines, pyridines, alkaloids, ketones, alcohols, and esters in the refined product increases significantly, which can significantly improve the richness and sensory evaluation of the refined product, effectively solving the problem of weak base flavors and thin aromas in existing technologies.

[0008] The third objective of this invention is to provide an application of a plant seed dry distillation refined product as a flavoring agent for heated tobacco products. Based on the superior technical effects of the refined product, its application as a flavoring agent in heated tobacco products can effectively improve the sensory quality of heated tobacco products. GC-MS testing revealed that the refined product contains more than 20 aroma compounds. Sensory analysis showed that heated tobacco products using the refined product of this invention produce a rich and complex aroma, with a distinct cocoa or coffee flavor in the initial stage, followed by a rich and layered aroma of caramel sweetness and roasted notes in the middle and later stages. The overall smoke is more delicate and harmonious, with a significantly improved aftertaste, and a substantial increase in the consistency of aroma and smoke throughout.

[0009] To achieve the above-mentioned technical objectives, the present invention provides a method for preparing a plant seed dry distillation refined product, the process of which is as follows: the plant seeds are subjected to a dry distillation reaction to obtain dry distilled seed raw material; the dry distilled seed raw material is mixed evenly with a solvent and homogenized, and then the supernatant is collected after solid-liquid separation to obtain a dry distilled seed raw material extract; the dry distilled seed raw material extract is subjected to molecular distillation, and the light component fraction is collected to obtain the product.

[0010] The plant seeds are seeds of plants from the Rubiaceae and / or Sterculiaceae families that contain nicotine and caffeine.

[0011] As a preferred embodiment, the plant seeds are coffee beans and / or cocoa beans, and their form is flakes and / or powder.

[0012] As a preferred embodiment, when the plant seeds are in powder form, their particle size is 30-60 mesh. More preferably, when the plant seeds are in powder form, their particle size is 40-50 mesh.

[0013] As a preferred embodiment, the pyrolysis reaction process is as follows: tobacco raw materials are placed in a high-temperature pyrolysis reactor and heated in a sealed manner at 80–250°C for 0.5–2 hours, followed by natural cooling to room temperature. More preferably, the pyrolysis reaction process is as follows: tobacco raw materials are placed in a high-temperature pyrolysis reactor and heated in a sealed manner at 80–150°C for 0.5–1 hour, followed by natural cooling to room temperature.

[0014] Coffee beans themselves contain a wealth of chemical components, including carbohydrates, proteins, lipids, and organic acids. After roasting, they undergo caramelization and Maillard reactions, producing a sweet caramel and roasted aroma in addition to the characteristic coffee aroma. Cocoa beans are brownish-red with a distinctive cocoa aroma, have a moisture content of less than 5%, and are rich in chemical components. Besides fats, proteins, and carbohydrates, cocoa beans also contain theobromine, vitamin A, vitamin B1, vitamin B2, nicotinic acid, phosphorus, iron, and calcium. Theobromine has a mild stimulating and excitatory effect on the human body. As described above, both coffee and cocoa beans undergo caramelization and Maillard reactions during thermal distillation, producing the rich aroma components unique to cocoa. The coffee and cocoa beans, after dry distillation, undergo stepwise extraction to maximize the extraction of their characteristic flavor components. Therefore, the temperature and time of dry distillation are crucial operating parameters in the preparation method of this invention. As the dry distillation temperature increases, the content of aroma compounds in the coffee and cocoa beans, such as pyrazines, pyridines, alkaloids, ketones, alcohols, and esters, increases significantly, resulting in a richer and more flavorful refined product and a substantial improvement in the sensory quality of heated cigarettes. However, excessively high or low dry distillation temperatures fail to release the inherent flavor of the coffee or cocoa beans and hinder the formation of a harmonious complex aroma, thus lowering their sensory evaluation and failing to meet subsequent usage requirements.

[0015] As a preferred embodiment, the solvent is at least one of ethanol and propylene glycol.

[0016] As a preferred embodiment, the mass ratio of the dry distillation fume to the solvent is 1:6 to 10.

[0017] As a preferred embodiment, the homogenization method is high-pressure homogenization, the conditions of which are: after the dry distillation fume and solvent are mixed evenly, homogenization is carried out at a pressure of 100-150 bar for 40-60 min.

[0018] As a preferred embodiment, the solid-liquid separation method is centrifugal separation, with the following conditions: centrifugation at 3000-500 rpm for 5-10 minutes at room temperature.

[0019] As a preferred embodiment, the molecular distillation conditions are: vacuum degree of 1.0 to 3.0 mbar, temperature of 60 to 100°C, feeding rate of 2 to 6 mL / min, and film scraping rate of 200 to 300 r / min.

[0020] The present invention also provides a plant seed dry distillation refined product, which is prepared by the method described in any one of the above methods.

[0021] As a preferred embodiment, the main aroma compounds in the dry distillation product include: pyridine, alcohols, caffeine, esters, and pyrazines.

[0022] Chromatographic analysis revealed that the main components of the refined product obtained from coffee beans as a substrate were pyridine, methylbutanol, methylpyrimidine, acetic acid, hydroxybutyric acid, furanol, methylbutyric acid, hydroxycyclopenten-1-one, maltol, ethoxypyrrole, pyrrolidone, 2-hydroxyγ-butyrolactone, 2-methylpyridinol, 2-hydroxypropionamide, methylpyridinone, pyridinol, hexadecanoic acid, caffeine, and palmitic acid. Compared with traditional coffee flavorings, the content of pyridine, furanol, pyrrolidone, and pyridinol was significantly increased, thus achieving a rich coffee flavor and a harmonious and complex caramel-sweet aroma in the refined product.

[0023] The main components of the refined product obtained from cocoa beans are hexene glycol, caffeine, benzaldehyde, phenethyl alcohol, pyrazine, ethyl palmitate, ethyl oleate, ethyl benzoate, ethyl phenylacetate, ethyl myristate, ethyl laurate, and ethyl linoleate. Compared to traditional cocoa flavorings, the content of hexene glycol, caffeine, benzaldehyde, phenethyl alcohol, and pyrazine is significantly increased, thus achieving a rich cocoa flavor and a harmonious and complex caramel and roasted aroma.

[0024] The present invention also provides an application of plant seed dry distillation refined products as flavorings for heated non-combustible cigarettes.

[0025] Compared with the prior art, the beneficial technical solution of the present invention is as follows:

[0026] 1) The plant seed dry distillation product provided by the present invention uses cocoa beans or coffee beans as raw materials. Based on the synergistic effect between each step, it greatly increases the content and types of aroma substances, especially the flavor characteristics of cocoa or coffee itself. Under low temperature conditions, while ensuring the release of flavors with obvious cocoa or coffee aroma characteristics, it also imparts a rich caramel aroma, greatly improving the richness and fullness of the aroma.

[0027] 2) The preparation method provided by this invention first induces the caramelization and Maillard reactions of carbohydrates, proteins, lipids and organic acids in cocoa beans or coffee beans through a dry distillation reaction, thereby producing caramel and roasted aromas on the basis of cocoa or coffee aromas. Then, it undergoes homogenization and molecular distillation treatments to further extract phenolic and ester compounds from tobacco raw materials. Among them, as the dry distillation temperature increases, the content of aroma substances such as pyrazines, pyridines, alkaloids, ketones, alcohols and esters in the dry distillation refined product increases significantly, which can significantly improve the richness and sensory evaluation of the refined product, and effectively solve the problem of weak base flavor and thin aroma of coffee or cocoa flavoring in the prior art.

[0028] 3) Based on the excellent technical effects of the above-mentioned refined material, the application of it as a flavoring agent in heated cigarettes can effectively improve the sensory quality of heated cigarettes. According to GC-MS testing, the total amount of aroma substances in the refined material is more than 20 kinds. According to sensory analysis, the heated cigarettes using the refined material of this invention have a rich and mellow aroma with high richness. The initial stage has obvious cocoa or coffee flavor, and the middle and later stages have rich caramel and roasted aromas with distinct layers. The overall smoke is more delicate and harmonious, the aftertaste is significantly improved, and the consistency of aroma and smoke is greatly improved. Attached Figure Description

[0029] Figure 1 To analyze the GC-MS diagram of aroma components in the coffee extract obtained in Example 1 of this invention using SPME / GC-MS;

[0030] Figure 1 In this list, 1 is pyridine; 2 is methylbutanol; 3 is maltol; 4 is acetic acid; 5 is hydroxybutyric acid; 6 is furanol; 7 is methylbutyric acid; 8 is hydroxycyclopenten-1-one; 9 is ethoxypyrrole; 10 is caffeine; 11 is pyrrolidone; 12 is 2-hydroxyγ-butyrolactone; 13 is 2-methylpyridinol; 14 is 2-hydroxypropionamide; 15 is methylpyridinone; 16 is pyridinol; 17 is hexadecanoic acid; 18 is methylpyrimidine; and 19 is palmitic acid.

[0031] Figure 2 GC-MS chromatogram of aroma components in the cocoa extract obtained in Example 2 of this invention was analyzed using SPME / GC-MS.

[0032] Figure 2 In the following, 1 is hexene glycol; 2 is phenylethanol; 3 is benzaldehyde; 4 is caffeine; 5 is pyrazine; 6 is ethyl palmitate; 7 is ethyl oleate; 8 is ethyl benzoate; 9 is ethyl tetradecanoate; 10 is ethyl laurate; and 11 is ethyl linoleate. Detailed Implementation

[0033] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making inventive steps are within the scope of protection of the present invention.

[0034] Example 1

[0035] 1 kg of coffee beans were ground to approximately 40-50 mesh and placed in a high-temperature dry distillation reactor. The reactor was heated at 100°C under sealed conditions for 1 hour. After cooling to room temperature, 0.7 kg of dry-distilled coffee was obtained. The dry-distilled coffee and propylene glycol were mixed uniformly at a mass ratio of 1:10 and homogenized under high pressure at 150 bar for 60 minutes. The homogenized mixture was then transferred to a centrifuge flask for solid-liquid separation at room temperature. After centrifugation, the supernatant was collected, yielding 4.2 kg of homogenized dry-distilled coffee or dry-distilled cocoa extract. Molecular distillation was then performed under conditions of vacuum 1.0-3.0 mbar, evaporation temperature 60-100°C, feeding rate 2 mL / min, and scraping speed 300 r / min, yielding 0.6 kg of purified dry-distilled coffee.

[0036] When the refined product obtained in this embodiment is applied to heated cigarettes, sensory evaluation tests show that the heated cigarettes have a distinct coffee flavor in the initial stage, and a rich aroma of caramel and roast in the middle and later stages, with the caramel aroma being more pronounced. The overall aroma richness of the smoke is significantly improved.

[0037] Example 2

[0038] 1 kg of cocoa beans were placed in a high-temperature dry distillation reactor and heated at 150°C in a sealed container for 0.5 h. After cooling to room temperature, 0.6 kg of dry distilled cocoa was obtained. The dry distilled cocoa and propylene glycol were mixed evenly at a mass ratio of 1:10 and homogenized under high pressure at 150 bar for 60 min. The homogenized mixture of dry distilled cocoa and propylene glycol was then placed in a centrifuge flask and subjected to solid-liquid separation at room temperature. After centrifugation, the supernatant was collected, yielding 3.5 kg of homogenized dry distilled cocoa extract. Molecular distillation was then carried out under conditions of vacuum of 1.0-3.0 mbar, evaporation temperature of 60-100°C, feeding rate of 2 mL / min, and scraping film speed of 300 r / min, yielding 0.5 kg of refined dry distilled cocoa product.

[0039] When the refined product obtained in this embodiment is applied to heated cigarettes, sensory evaluation tests show that the heated cigarettes have a distinct cocoa flavor in the initial stage, and a rich aroma of caramel sweetness and roasted aroma in the middle and later stages, with the roasted aroma being more pronounced.

[0040] Example 3

[0041] 1 kg of coffee beans were ground to approximately 40-50 mesh and placed in a high-temperature dry distillation reactor. The reactor was heated at 250°C under sealed conditions for 0.5 hours. After cooling to room temperature, 0.5 kg of dry-distilled coffee was obtained. The dry-distilled coffee and propylene glycol were mixed uniformly at a mass ratio of 1:10 and homogenized under high pressure at 150 bar for 60 minutes. The homogenized mixture was then transferred to a centrifuge flask for solid-liquid separation at room temperature. After centrifugation, the supernatant was collected, yielding 2.8 kg of homogenized dry-distilled coffee extract. Molecular distillation was then performed under conditions of a vacuum of 1.0-3.0 mbar, an evaporation temperature of 60-100°C, a feeding rate of 2 mL / min, and a scraping rate of 300 r / min, yielding 0.35 kg of purified coffee dry distillate.

[0042] When the refined product obtained in this embodiment is applied to heated cigarettes, sensory evaluation tests show that the heated cigarettes have a distinct coffee flavor in the initial stage, a rich burnt aroma in the middle and later stages, and a significant improvement in the overall aroma richness of the smoke.

[0043] As demonstrated in Examples 1 and 3, with increasing pyrolysis temperature, the resulting refined pyrolysis product, when applied to heated cigarettes, initially exhibits a distinct coffee flavor. However, in the later stages, the aroma shifts from sweet caramel to burnt caramel. This is due to the different rates of caramelization and Maillard reactions in the coffee beans during the pyrolysis stage. This also proves that, within the scope required by this invention, the aroma and flavor of the refined pyrolysis product can be directly controlled by adjusting the relevant pyrolysis parameters. Furthermore, it should be noted that the yield of the refined pyrolysis product decreases with increasing pyrolysis temperature. Therefore, strict temperature control is necessary during the pyrolysis process. Excessive temperature not only causes the caramelization and Maillard reactions to transform into carbonization reactions, producing a large amount of bitterness, but also leads to a significant decrease in product yield.

Claims

1. A method for preparing a purified product from the dry distillation of plant seeds, characterized in that: Plant seeds are subjected to dry distillation to obtain dry distilled seed raw material; the dry distilled seed raw material is mixed with a solvent and homogenized, then separated into solid and liquid components, and the supernatant is collected to obtain dry distilled seed raw material extract; the dry distilled seed raw material extract is subjected to molecular distillation, and the light component fraction is collected to obtain the final product. The plant seeds are seeds of plants from the Rubiaceae and / or Sterculiaceae families that contain nicotine and caffeine.

2. The method for preparing a plant seed dry distillation purified product according to claim 1, characterized in that: The plant seeds are coffee beans and / or cocoa beans, and their morphology is flakes and / or powder; when the plant seeds are in powder form, their particle size is 30-60 mesh.

3. The method for preparing a plant seed dry distillation purified product according to claim 1, characterized in that: The process of the dry distillation reaction is as follows: tobacco raw materials are placed in a high-temperature dry distillation reactor and heated in a sealed manner at 80-250°C for 0.5-2 hours, and then naturally cooled to room temperature.

4. The method for preparing a plant seed dry distillation purified product according to claim 1, characterized in that: The solvent is at least one of ethanol and propylene glycol; the mass ratio of the dry distillation fume to the solvent is 1:6 to 10.

5. The method for preparing a plant seed dry distillation purified product according to claim 1, characterized in that: The homogenization method is high-pressure homogenization, and the conditions are: after the dry distillation fume and solvent are mixed evenly, homogenize at a pressure of 100-150 bar for 40-60 min.

6. The method for preparing a plant seed dry distillation purified product according to claim 1, characterized in that: The solid-liquid separation method is centrifugal separation, and the conditions are: centrifugation at 3000-500 rpm for 5-10 minutes at room temperature.

7. The method for preparing a plant seed dry distillation purified product according to claim 1, characterized in that: The conditions for molecular distillation are: vacuum degree of 1.0 to 3.0 mbar, temperature of 60 to 100 °C, feeding rate of 2 to 6 mL / min, and scraping rate of 200 to 300 r / min.

8. A plant seed dry distillation refined product, characterized in that: Prepared by the method described in any one of claims 1 to 7.

9. A plant seed dry distillation refined product according to claim 8, characterized in that: The main aroma compounds in the dry distillation product include pyridine, alcohols, caffeine, esters, and pyrazines.

10. The application of the plant seed dry distillation refined product according to claim 8, characterized in that: As a flavoring agent for heated tobacco products.

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