A method of preparing a tobacco extract

By employing a continuous process of crushing, extraction, filtration, and reflux, the problem of low extraction rate of tobacco leaf fragments was solved, enabling efficient and continuous extraction of effective components from tobacco leaves and improving extraction efficiency and material exchange efficiency.

CN117099996BActive Publication Date: 2025-11-04CHINA TOBACCO YUNAN NEW MATERIAL +1
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Patent Information

Application Number
CN202311134961.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-05
Publication Date
2025-11-04
Estimated Expiration
2043-09-05

AI Technical Summary

Technical Problem

Existing technologies have low extraction rates for tobacco leaf fragments and the extraction process is discontinuous, resulting in the failure to fully utilize the effective components.

Method used

A continuous rubbing-extraction-filtration-reflux operation is adopted. The rubbing-reflux extraction device is used to repeatedly rub and extract tobacco leaf fragments. Combined with the design of rubbing plate and filter hole, the effective components in tobacco leaves are extracted efficiently.

Benefits of technology

It improves the extraction rate and efficiency of effective components in tobacco leaf fragments, realizes integrated and continuous operation from extraction to filtration, and enhances the efficiency of material exchange and crushing.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a preparation method of tobacco leaf extract. The effective components in the tobacco leaf are extracted to a high degree through repeated or continuous rolling and extraction of tobacco leaf fragments, and the tobacco leaf extract is prepared with high efficiency. The application also uses an optimal device to improve the overall efficiency of the device and method, including a cylindrical rotary rolling part, a rolling plate capable of adjusting rolling conditions, a large-area rolling surface and filter holes integrated with the bin wall, and a temperature control part capable of providing temperature control function for most of the device.
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Description

Technical Field

[0001] This invention relates to the field of tobacco extract preparation technology, and in particular to a method for preparing tobacco leaf extract. Background Technology

[0002] The typical method for extracting tobacco leaf fragments involves soaking tobacco leaves or stems in an extraction solvent, then extracting and concentrating the solution to obtain a tobacco leaf extract. This process is then repeated with a new batch of tobacco leaves for another round of extraction. Current improvements to tobacco leaf extract preparation methods usually focus on optimizing the separation and purification of specific substances after extraction, with few solutions aimed at increasing the extraction rate of active ingredients from tobacco leaf fragments.

[0003] For example, the method for preparing the extract in Chinese patent CN201611266573.4 involves mixing tobacco powder and an extractant and then refluxing and heating. However, similar methods have low extraction rates under normal operating conditions, and the overall extraction effect on tobacco fragments is poor, failing to fully utilize the effective components in the tobacco fragments.

[0004] Chinese patent CN202122380494.9 discloses an extraction device for plant trace elements, which achieves the kneading operation during extraction by setting an elastic kneading component in conjunction with an extraction tank. First, in its kneading direction, the elastic kneading component applies pressure using an elastic element, which can only provide a constant elastic force. This may cause the extract to be gradually squeezed out between the elastic kneading component and the extraction tank during kneading, making kneading impossible. Second, in the disclosed specific solution, the rotation of the elastic kneading component during kneading continuously pushes the plant fragments to be extracted towards the periphery of the extraction tank, affecting kneading efficiency. Third, the extraction and kneading operation using this device is a one-time, non-continuous process, unable to achieve continuous and repeated extraction of a batch of plant fragments, potentially leading to low and insufficient extraction efficiency.

[0005] Therefore, designing a method for preparing tobacco leaf extract to achieve full and efficient extraction of components from tobacco leaf fragments, while realizing integrated and continuous operation from extraction to filtration, is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0006] In view of the problems existing in the prior art, the present invention provides a method for preparing tobacco leaf extract. Through a continuous rubbing-extraction-filtration-reflux operation, the method of this application can fully extract the effective components from tobacco leaf fragments. The rubbing operation described in this application can be understood in a general and unrestricted manner; rubbing means that two rough surfaces simultaneously squeeze and rub an object placed between them.

[0007] The solution provided in this application to address the above-mentioned problems is a method for preparing tobacco leaf extract, used to extract the effective components from tobacco leaves, comprising the following steps:

[0008] S1. Soak tobacco leaf fragments in solvent;

[0009] S2. The tobacco leaf fragments are crushed in the solvent, and after filtering a portion of the mixture of the tobacco leaf fragments and the solvent, the filtrate and the filter residue are mixed with the remaining mixture.

[0010] S3. Repeat step S2 until the effective components in the tobacco leaf fragments are fully extracted, and then filter the mixture to obtain the tobacco leaf extract.

[0011] Furthermore, the temperature of the rubbing and rolling operation is 25℃~80℃.

[0012] Further, in step S1, the mass ratio of the solvent to the tobacco leaf fragments is (5-20):1.

[0013] Furthermore, in step S2, the filtering, mixing, and rubbing are performed simultaneously.

[0014] Furthermore, the effective components in the tobacco leaf fragments are fully extracted, which is equivalent to the simultaneous filtration, mixing, and rubbing processes lasting at least 1 hour.

[0015] Further, the active ingredients include: ethyl acetate, 2-butenal, isovaleral, n-butanol, hydroxyacetone, trioxymethylene, 2,3-pentanedione, pentanal, isoamyl alcohol, pyridine, 2-methylpropionic acid, pyrrole, n-pentanol, 3-methyl-2-buten-1-ol, 3-methyl-2-butenal, hexanal, 2-methyltetrahydrofuran-3-one, furfural, isovaleric acid, 2-methylbutyric acid, furfuryl alcohol, γ-butyrolactone, benzaldehyde, methylheptenone, 2-n-pentylfuran, 6-methyl-5-heptenyl-2-ol, 3-pyridinecarboxaldehyde, benzyl alcohol, phenylacetaldehyde, 2-acetylpyrrole, linalool, nonanal, 3-acetylpyridine, phenethyl alcohol, isophorone, 2,6 At least one of the following: 6-trimethyl-2-cyclohexene-1,4-dione, atroaldehyde, menthol, anethole, indole, p-vinylguaiacol, nicotine, eugenol, solanone, damascene, β-caryophyllene, mesmin, geranylacetone, 4-phenylpyridine, 2,6-di-tert-butyl-p-cresol, dihydroactinol, 2,3-bipyridine, stigmasterone A, stigmasterone B, stigmasterone C, stigmasterone D, pentadecaldehyde, myristic acid, diene, neophytadiene, phytone, farnesylacetone A, methyl palmitate, isophytol, palmitic acid, ceftazidimetrienol A, ceftazidimetrienol B, farnesylacetone B, erucamide, and trans-squalene.

[0016] Furthermore, the solvent includes at least one of water and organic solvents.

[0017] Furthermore, the method for preparing tobacco extract uses a tobacco fragment rubbing and reflux extraction device, which includes a rubbing section, a first filter hole, and a reflux section. The rubbing section includes a first chamber, a rubbing surface disposed inside the first chamber, and a rubbing plate that can rub the tobacco fragments on the rubbing surface. The reflux section includes a second chamber connected to the first chamber through the first filter hole, and a reflux section. The solid-liquid mixture in the second chamber can be refluxed back to the first chamber through the reflux section.

[0018] Preferably, the rubbing section further includes a rotating shaft and a motor for driving the rotating shaft to rotate; the first chamber is configured as a cylinder coaxial with the rotating shaft, the rubbing surface is configured as the inner sidewall of the first chamber, and the rubbing plate is pivotally connected to the rotating shaft.

[0019] Preferably, the grinding plate is connected to the rotating shaft via an adjustable-length connecting rod.

[0020] Preferably, the first filter hole is disposed on the rubbing surface.

[0021] Preferably, the device further includes a collection section, the collection section comprising: a collection port communicating with the second chamber through a second filter hole; the aperture of the second filter hole is smaller than that of the first filter hole.

[0022] Preferably, the collection part further includes a collection chamber, which is sleeved on the outside of the second chamber, the second filter hole is disposed on the chamber wall of the second chamber, and the collection port is disposed at the bottom of the collection chamber.

[0023] Preferably, the second compartment is fitted outside the first compartment, and the reflux section includes: a reflux pipe connecting the second compartment and the first compartment, and a reflux pump installed in the reflux pipe.

[0024] Preferably, it also includes a temperature control unit that can control the temperature of the first compartment and / or the second compartment.

[0025] Preferably, it also includes cover plates, the cover plates including a first compartment cover plate that can close a first compartment and a second compartment cover plate that can close a second compartment.

[0026] Preferably, the first compartment and / or the second compartment are provided with slag outlets.

[0027] Preferably, the preparation method for preparing tobacco extract using this device includes the following steps:

[0028] S1: Adjust the length of the connecting rod according to the diameter of the tobacco leaf fragments to determine the position of the grinding plate, open the first chamber cover, put the tobacco leaf fragments to be extracted into the first chamber, inject an appropriate solvent into the first chamber, and extract the tobacco leaf fragments;

[0029] S2: The temperature control medium in the temperature control chamber is heated to a certain temperature, so that the solid-liquid mixture composed of tobacco leaf fragments and solvent is heated to an appropriate temperature, thereby accelerating the separation of components from the tobacco leaf fragments;

[0030] S3: Turn on the motor to drive the shaft to rotate, so that the rubbing plate continuously squeezes and rubs the tobacco leaf fragments to help extract the effective components from the tobacco leaf fragments. Part of the extract and part of the tobacco leaf fragments flow into the second chamber through the first filter hole.

[0031] S4: Turn on the reflux pump. The solid-liquid mixture of some tobacco leaf fragments and solvent in the second chamber is introduced into the first chamber through the reflux pipe for further rubbing. The solid-liquid mixture of some tobacco leaf fragments and solvent flows into the collection chamber after being filtered through the second filter hole.

[0032] S5: After a certain period of rubbing, extraction, filtration, and reflux, the effective components in the tobacco leaf fragments are fully extracted, and the filtrate is released from the collection port. The filter residue is released from the reflux first chamber outlet and the second chamber outlet.

[0033] Preferably, the diameter of the tobacco leaf fragments used is 1mm-20mm.

[0034] Preferably, the position of the rubbing plate should be adjusted so that the distance between it and the rubbing surface is slightly less than the average diameter of the tobacco leaf fragments, more preferably 30%-80% of the average diameter of the tobacco leaf fragments.

[0035] The beneficial effects of this invention are as follows:

[0036] 1. This invention is a method for preparing tobacco leaf extract. By repeatedly and even continuously rubbing and extracting tobacco leaf fragments, the effective components in the tobacco leaves are extracted to a high degree, and the preparation of tobacco leaf extract is highly efficient.

[0037] 2. The present invention also provides a preferred embodiment of a method for preparing tobacco extract. By using a preferred device, the overall efficiency of the device and method is improved by increasing the material exchange efficiency and rubbing efficiency. The device includes: a cylindrical rotary rubbing section; a rubbing plate with adjustable rubbing conditions; a large-area rubbing surface and filter holes integrated with the bin wall; and a temperature control section that can provide temperature control for most parts of the device.

[0038] 3. The preferred apparatus of the preparation method provided by the present invention is simple and reasonable. The rubbing section, reflux section and optional collection section and temperature control section are arranged in a step-by-step manner from the inside to the outside, with a high degree of integration, and the structure is compact and efficient.

[0039] 4. The preferred apparatus for the preparation method provided by the present invention fully considers operational requirements and is equipped with a collection port and a slag outlet, making it convenient for operators to use the apparatus. Attached Figure Description

[0040] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention. In these drawings, similar reference numerals are used to denote similar elements. The drawings described below are some embodiments of the invention, but not all embodiments. Other drawings will be readily available to those skilled in the art based on these drawings without any inventive effort.

[0041] Figure 1 This is a schematic diagram of the apparatus used in Embodiment 1 of the present invention;

[0042] Figure 2 for Figure 1 Enlarged schematic diagram of a portion of the inner wall of the first warehouse 1;

[0043] Figure 3 The total TIC particle flow map of the extract obtained in Example 1 of the present invention;

[0044] Figure 4 This is a TIC total particle flow map of the extract obtained in Comparative Example 1 of the present invention.

[0045] In the picture:

[0046] 1. First compartment; 1-1. Slag outlet of the first compartment; 2. Crushing surface; 3. First filter hole; 4. Crushing plate; 4-1. Connecting rod; 4-2. Rotating shaft; 4-3. Motor; 5. Second compartment; 5-1. Slag outlet of the second compartment; 6-1. Return pipe; 6-2. Return pump; 7. Second filter hole; 8. Collection port; 9. Collection compartment; 10. Temperature control compartment; 10-1. Temperature control medium outlet; 10-2. Temperature control medium inlet; 11-1. Cover plate of the first compartment; 11-2. Cover plate of the second compartment; 11-3. Limiting hole. Detailed Implementation

[0047] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0048] The method for preparing tobacco extract in this application can use a tobacco leaf fragment crushing and reflux extraction device to improve preparation efficiency.

[0049] The device first includes a grinding section, a first filter hole 3, and a reflux section.

[0050] The rubbing section first includes a first chamber 1, which is used to contain a solid-liquid mixture of a solvent and tobacco leaf fragments, such as water or an organic solvent. The rubbing section also includes a rough rubbing surface 2 and a rubbing plate 4 that can press the tobacco leaf fragments onto the rubbing surface 2. In the rubbing section, the effective components in the tobacco leaf fragments are extracted by soaking and pressing them.

[0051] After being filtered through the first filter hole 3, part of the solid-liquid mixture in the grinding section enters the reflux section.

[0052] The reflux section includes a second chamber 5 and a reflux segment. The second chamber 5 is used to hold at least the solid-liquid mixture filtered through the first filter hole 3. The solid-liquid mixture in the second chamber 5 can be refluxed back to the first chamber 1 via the reflux segment for further extraction. Through continuous rubbing extraction-filtration-reflux operation, the tobacco leaf fragment rubbing reflux extraction device of this application can achieve full extraction of the effective components in tobacco leaf fragments.

[0053] The arrangement of the rubbing section is unrestricted. Specifically, the first chamber 1 can hold a solid-liquid mixture, and the rubbing surface 2 and rubbing plate 4 can cooperate to rub the tobacco leaf fragments in the solid-liquid mixture. To simplify the device and increase the effective rubbing area and efficiency, in some embodiments, the device further includes a rotating shaft 4-2 and a motor 4-3 that drives the rotating shaft 4-2. The first chamber 1 is configured as a cylinder coaxial with the rotating shaft 4-2, the rubbing surface 2 is configured as the inner wall of the first chamber 1, and the rubbing plate 4 is pivotally connected to the rotating shaft 4-2. Directly configuring the rubbing surface 2 as the inner wall of the first chamber 1 avoids the need for a separate component containing the rubbing surface 2. By configuring the rubbing chamber as the inner wall of the cylinder and rotating the rubbing plate 4, the effective rubbing area is the side surface that the rubbing plate 4 rotates over, resulting in greater continuity and reliability of the rubbing action. Preferably, the rubbing plate 4 is connected to the rotating shaft 4-2 via an adjustable-length connecting rod 4-1, so as to adjust the distance between the rubbing plate 4 and the rubbing surface 2 according to the tobacco leaf fragments of different diameters, thereby adjusting the rubbing force and effect. In other embodiments, the first chamber 1 can be set to any shape; the rubbing surface 2 can be set in other ways, such as setting a plate or cylinder with a rough surface separately; the rubbing plate 4 can realize the rubbing motion in other ways, such as not setting the rotating shaft 4-2 but using a reciprocating motion mechanism for reciprocating motion.

[0054] The arrangement of the rubbing plate 4 is not limited; it can be used in conjunction with the rubbing surface 2 to rub the tobacco leaf fragments placed between the rubbing plate 4 and the rubbing surface 2. In some embodiments, the rubbing plate 4 can be configured in different shapes to reduce the resistance of the movement of the rubbing plate 4, enhance the stirring effect, and facilitate the guidance of the tobacco leaf fragments to move between the rubbing plate 4 and the rubbing surface 2.

[0055] The arrangement of the first filter hole 3 is not limited; it can be used to filter the solid-liquid mixture flowing from the first chamber 1 into the second chamber 5. For example, it can be installed using a filter screen or filter element located between the rubbing section and the return section. In some embodiments, the first filter hole 3 is located on the rubbing surface 2, which allows for further cutting of the tobacco leaf fragments during rubbing and also enables timely transfer of the effective components squeezed out from the rubbing tobacco leaf fragments to the return section, preventing excessively high local concentrations that could cause the squeezed effective components to dissolve into the tobacco leaf fragment residue. Typically, the diameter of the first filter hole 3 is 0.5-3.0 mm.

[0056] The arrangement of the reflux section is unrestricted. Specifically, the second chamber 5 can be configured to hold a solid-liquid mixture. The connection between the second chamber 5 and the first chamber 1 is unrestricted; the solid-liquid mixture in the first chamber 1 can be filtered through the first filter hole 3 and then flow into the second chamber 5. In some embodiments, the second chamber 5 is fitted outside the first chamber 1, and the first filter hole 3 is located on the wall of the first chamber 1. The solid-liquid mixture in the first chamber 1 flows into the second chamber 5 spontaneously or with the assistance of agitation from the grinding plate 4, after being filtered through the first filter hole 3. The arrangement of the reflux section is also unrestricted; the solid-liquid mixture in the second chamber 5 can be returned to the first chamber 1. In some embodiments, the reflux section is configured as a reflux pipe 6-1 connecting the first chamber 1 and the second chamber 5, and a reflux pump 6-2 located on the reflux pipe 6-1. In other embodiments, the reflux section can also be designed with other connection relationships between the first chamber 1 and the second chamber 5, so that the solid-liquid mixture in the second chamber 5 is driven back into the first chamber 1 by gravity or other forces. Typically, the diameter of the reflux pipe 6-1 is 4-8 cm.

[0057] To facilitate collection operations, in some embodiments, the device further includes a collection section, which includes a collection port 8 communicating with the second chamber 5 through a second filter hole 7; the aperture of the second filter hole 7 is smaller than that of the first filter hole 3. Specifically, the collection port 8 can be connected to the external environment of the device and can allow the solid-liquid mixture to pass through. Considering the ease of setting the second filter hole 7 and the collection port 8, as well as other specific needs in collection operations, in some embodiments, the collection section further includes a collection chamber 9. Specifically, the setting method and connection relationship of the collection chamber 9 are not limited, as long as it can accommodate the solid-liquid mixture. The second filter hole 7 can filter the solid-liquid mixture flowing from the second chamber 5 into the collection chamber 9, for example, through a filter screen or filter element located between the second chamber 5 and the collection chamber 9. Considering the integration of the device, in some embodiments, the collection chamber 9 is sleeved on the outside of the second chamber 5, the bottom of the collection chamber 9 is provided with a collection port 8, and the second filter hole 7 is provided in the chamber wall of the second chamber 5. Typically, the diameter of the second filter hole 7 is 0.05-0.12 mm.

[0058] To enable the device itself to control the extraction temperature of tobacco leaf fragments, in some embodiments, the device further includes a temperature control unit that can control the temperature of the first chamber 1 and / or the second chamber 5. The arrangement of the temperature control unit is not limited; for example, it can be configured as a temperature control rod inserted into the first chamber 1 and / or the second chamber 5, a temperature control sleeve fitted over the first chamber 1 and / or the second chamber 5, or a temperature control chamber 10 that can contain the temperature control medium.

[0059] To enable the device to be sealed, in some embodiments, the device further includes a cover plate, which includes a first compartment cover plate 11-1 for sealing the first compartment 1 and a second compartment cover plate 11-0 for sealing the second compartment 5. In embodiments where a rotating shaft 4-2 is provided, the cover plate may also include a limiting hole 11-3 to limit the rotating shaft 4-2 and prevent the rotating shaft 4-2 from shaking.

[0060] To facilitate the discharge of liquid or slag from the device, in some embodiments, the first chamber 1 and / or the second chamber 5 are provided with slag outlets that can discharge solids, liquids, and solid-liquid mixtures.

[0061] The following is the apparatus used in Example 1 of the preparation method of tobacco leaf extract. Please refer to [the example]. Figure 1 , 2 .

[0062] The tobacco leaf fragment rubbing and reflux extraction device used in Example 1 firstly includes a rubbing section, a first filter hole 3, a reflux section, a collection section, a temperature control section, and a cover plate.

[0063] The grinding section includes a first chamber 1, which is cylindrical. The inner wall of the first chamber 1 is a rough grinding surface 2, and the chamber wall is also provided with a first filter hole 3 with a diameter of 2mm. The bottom of the first chamber 1 is provided with a first chamber slag outlet 1-1. The grinding section also includes a rotating shaft 4-2 coaxial with the first chamber 1, and a motor 4-3 that drives the rotating shaft 4-2 to rotate. The grinding plate 4 is connected to an adjustable length connecting rod 4-1, and the connecting rod 4-1 is pivotally connected to the rotating shaft 4-2. The connecting rod 4-1 is provided with multiple screw holes, and the grinding plate 4 can be installed and its length adjusted by screws at different installation positions on the connecting rod 4-1.

[0064] The reflux section includes a second chamber 5 and a reflux segment. The second chamber 5, which is cylindrical, is fitted outside the first chamber 1 and its bottom is connected to a reflux pipe 6-1. A reflux pump 6-2 is installed on the reflux pipe 6-1 to pump the liquid in the second chamber 5 back to the first chamber 1. The bottom of the second chamber 5 is provided with a second chamber slag outlet 5-1.

[0065] The second chamber wall has a second filter hole 7 with a diameter of 0.1 mm in the bottom third section. Correspondingly, the second chamber wall has a collection chamber 9 with a collection part on the outer sleeve in the bottom third section. The collection chamber 9 has a collection port 8 at the bottom.

[0066] The second compartment 5 has a temperature control section in the upper two-thirds section. The temperature control section includes a temperature control chamber 10 that can contain a temperature control medium. The temperature control chamber 10 has a temperature control medium outlet 10-1 and a temperature control medium inlet 10-2. The temperature control medium is, for example, water or oil.

[0067] The cover plate 11 of the device includes a first compartment cover plate 11-1 that can close the first compartment 1, a second compartment cover plate 11-2 that can close the second compartment 5, and a limiting hole 11-3 for limiting the rotation shaft 4-2.

[0068] The operation steps of Example 1 are as follows:

[0069] S1: Adjust the length of the connecting rod 4-1 according to the diameter of the tobacco leaf fragments to determine the position of the rubbing plate 4. Open the first chamber cover 11-1, put 5kg of tobacco leaf fragments to be extracted into the first chamber 1, and inject 50kg of water into the first chamber 1 to extract the tobacco leaf fragments. The tobacco leaf fragments are obtained by coarsely crushing the finished tobacco leaves to an average equivalent diameter of 10mm using a pulverizer. The distance of the rubbing plate 4 is adjusted to 8mm from the rubbing surface.

[0070] S2: Heat the temperature control medium in the temperature control chamber 10 to heat the solid-liquid mixture of tobacco leaf fragments and water to 60°C, thereby accelerating the separation of components from the tobacco leaf fragments;

[0071] S3: Turn on motor 4-3 to drive shaft 4-2 to rotate, so that the rubbing plate 4 continuously squeezes and rubs the tobacco leaf fragments to help extract the effective components from the tobacco leaf fragments. Part of the extract and part of the tobacco leaf fragments flow into the second chamber 5 through the first filter hole 3.

[0072] S4: Turn on the reflux pump 6-2. The solid-liquid mixture of some tobacco leaf fragments and water in the second chamber 5 is introduced into the first chamber 1 through the reflux pipe 6-1 for further crushing. The solid-liquid mixture of some tobacco leaf fragments and water flows into the collection chamber 9 after being filtered through the second filter hole 7.

[0073] S5: After two hours of rubbing, extraction, filtration, and reflux, the effective components in the tobacco leaf fragments are fully extracted, and the filtrate is released from collection port 8. The filter residue is released from the first reflux chamber outlet 1-1 and the second reflux chamber outlet 5-1. The filtrate is the tobacco leaf extract obtained in Example 1.

[0074] The preparation method of the tobacco extract in Example 2 is basically the same as that in Example 1, except that the distance of the rubbing plate 4 in step S1 is adjusted to 3 mm from the rubbing surface.

[0075] The preparation method of the tobacco extract in Example 3 is basically the same as that in Example 1, except that: the first chamber 1 and the second chamber 5 of the extraction device are set separately and connected by a connecting pipe equipped with a delivery pump; the first filter hole 3 is not set on the wall of the first chamber, but is set as an independent filter screen in the connecting pipe.

[0076] The preparation method of the tobacco extract in Example 4 is basically the same as that in Example 1, except that the extraction device used only includes a grinding section. The mixture is stirred and ground at the same speed as in Example 1. After every 30 minutes of extraction, it is filtered through a filter with the same pore size as the first filter hole 3 in Example 1. The filtrate and residue are then remixed and added back to the grinding section. This process is repeated until the fourth time. Instead of remixing, a filter with the same pore size as the second filter hole 7 is used for filtration. The filtrate is the tobacco extract obtained in Example 4.

[0077] The preparation method of the tobacco extract in Example 5 is basically the same as that in Example 1, except that the solid-liquid mixture is heated to 25°C in step S2 and the mass of tobacco fragments in step S1 is 10 kg.

[0078] The preparation method of the tobacco extract in Example 6 is basically the same as that in Example 1, except that: the solid-liquid mixture is heated to 80°C in step S2; and the mass of tobacco fragments in step S1 is 2.5 kg.

[0079] The preparation method of the tobacco extract in Example 7 is basically the same as that in Example 1, except that the extraction time in step S5 is one hour.

[0080] The preparation method of the tobacco extract in Comparative Example 1 is a conventional extraction method. Specifically, 50 kg of water and 5 kg of tobacco fragments are injected into an extraction tank and stirred at the same speed as in Example 1. The extraction temperature is set to 60°C and the tobacco fragments are soaked and extracted for 2 hours. After extraction, the mixture is filtered step by step using a filter screen with the same pore size as the first filter pore 3 and the second filter pore 7. The filtrate is the tobacco extract obtained in Comparative Example 1.

[0081] The volatile components of five tobacco extracts from Examples 1-4 and Comparative Example 1 were extracted using a simultaneous distillation-extraction method, and then analyzed by GC / MS. The GC / MS analysis conditions are as follows:

[0082] Instrumentation: Gas Chromatography-Mass Spectrometry (Shimadzu GCMS-QP2020); Gas Chromatography Conditions: DB-5MS column (30m*0.25mm*0.25μm). Temperature Program: Initial temperature 50℃, hold for 1 min, increase to 160℃ at a rate of 4℃ / min, hold for 2 min; increase to 260℃ at a rate of 8℃ / min, hold for 10 min; Injector temperature: 200℃; Column oven temperature: 60℃; Injection mode: Split; Column flow rate: 1 mL / min; Purge flow rate: 3 mL / min; Split ratio: 10:1; Carrier gas: High-purity helium; Injection volume: 1 μL; Solvent delay: 2 min; Mass Spectrometry Conditions: Ionization mode: EI; Electron energy: 70 eV; Interface temperature: 250℃; Ion source temperature: 200℃; Acquisition mode: Scan; Scan range: 40-500 amu.

[0083] Samples were analyzed under the above conditions. Similarity was searched using the standard NIST14 library, and the chemical components in the samples were determined by comparing with literature and combining with experience. Using the GCMS Solution 4.45SP1 data processing system, naphthalene was used as an internal standard for semi-quantitative analysis using the internal standard method to obtain the content of each chemical component. The results are summarized in the table below.

[0084]

[0085]

[0086] Note: " / " indicates that the ingredient was not detected.

[0087] Total ion chromatography of volatile components of tobacco extracts in Example 1 and Comparative Example 1 is shown in the figure. Figure 3 , 4 .

[0088] The total ion chromatograms of Examples 2-7 are similar to those of Example 1. The extraction effects of Examples 5-7 are similar to those of Examples 1-4.

[0089] It can be seen that the preparation method provided in this application has a high extraction efficiency. Compared with traditional methods, the types and degree of extraction of effective components from solutions and tobacco leaf fragments of the same mass ratio are significantly improved.

[0090] It can also be seen that the continuous rubbing-extraction-filtration-reflux operation improves the overall extraction effect compared to discrete stirring and rubbing. Furthermore, integrating the filter holes with the rubbing surface can further optimize the extraction effect. This is because the filter holes can further cut the tobacco leaf fragments and promptly transfer the effective components of the rubbed tobacco leaf fragments to the reflux section, avoiding excessively high local concentrations that would cause the rubbed effective components to dissolve into the tobacco leaf fragment residue.

[0091] The above-described contents can be implemented individually or in various combinations, and these variations are all within the protection scope of this invention.

[0092] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes the element.

[0093] The above description, in conjunction with specific preferred embodiments, provides a further detailed explanation of the present invention. It should not be construed that the specific embodiments of the present invention are limited to these descriptions. For those skilled in the art, various simple deductions or substitutions can be made without departing from the concept of the present invention, and all such deductions or substitutions should be considered within the scope of protection of the present invention.

Claims

1. A method for preparing a tobacco leaf extract, used to extract the effective components from tobacco leaves, characterized in that, The tobacco leaves are extracted using a tobacco leaf fragment rubbing and reflux extraction device, which includes a rubbing section, a first filter hole (3), and a reflux section. The rubbing section includes a first chamber (1), a rubbing surface (2) disposed inside the first chamber (1), and a rubbing plate (4) that can rub the tobacco leaf fragments on the rubbing surface (2). The reflux section includes a second chamber (5) that is connected to the first chamber (1) through the first filter hole (3), and a reflux section. The solid-liquid mixture in the second chamber (5) can be refluxed back to the first chamber (1) through the reflux section. The rubbing section also includes a rotating shaft (4-2) and a motor (4-3) for driving the rotating shaft (4-2) to rotate; the first chamber (1) is configured as a cylinder coaxial with the rotating shaft (4-2), the rubbing surface (2) is configured as the inner sidewall of the first chamber (1), and the rubbing plate (4) is pivotally connected to the rotating shaft (4-2); the second chamber (5) is sleeved outside the first chamber (1), and the return section includes: a return pipe (6-1) connecting the second chamber (5) and the first chamber (1), and a return pump (6-2) disposed in the return pipe (6-1); it also includes a collection section, the collection section including: a collection port (8) communicating with the second chamber (5) through a second filter hole (7); the aperture of the second filter hole (7) is smaller than that of the first filter hole (3); the rubbing plate (4) is connected to the rotating shaft (4-2) through an adjustable length connecting rod; It also includes a temperature control unit that can control the temperature of the first chamber (1) and / or the second chamber (5); it also includes a cover plate, the cover plate including a first chamber cover plate (11-1) that can close the first chamber (1) and a second chamber cover plate (11-2) that can close the second chamber (5); the first chamber (1) and / or the second chamber (5) are provided with slag outlets; The method for preparing tobacco extract using the extraction apparatus includes the following steps: S1: Adjust the length of the connecting rod according to the diameter of the tobacco leaf fragments to determine the position of the rubbing plate (4), open the first chamber cover (11-1), put the tobacco leaf fragments to be extracted into the first chamber (1), inject appropriate solvent into the first chamber (1), and extract the tobacco leaf fragments; S2: Heat the temperature control medium in the temperature control chamber (10) to a certain temperature, so that the solid-liquid mixture composed of tobacco leaf fragments and solvent is heated to an appropriate temperature, thereby accelerating the separation of components from the tobacco leaf fragments; S3: Turn on the motor (4-3) to drive the rotating shaft (4-2) to rotate, so that the rubbing plate (4) continuously squeezes and rubs the tobacco leaf fragments to help extract the effective components in the tobacco leaf fragments. Part of the extract and part of the tobacco leaf fragments flow into the second chamber (5) through the first filter hole (3). S4: Turn on the reflux pump. The solid-liquid mixture of some tobacco leaf fragments and solvent in the second chamber (5) is introduced into the first chamber (1) through the reflux pipe for further rubbing. The solid-liquid mixture of some tobacco leaf fragments and solvent flows into the collection chamber after being filtered through the second filter hole (7). S5: After a certain period of rubbing, extraction, filtration and reflux operation, the effective components in the tobacco leaf fragments are fully extracted and the filtrate can be released from the collection port (8). The filter residue is released from the slag outlet (1-1) of the first reflux chamber and the slag outlet (5-1) of the second reflux chamber.

2. The preparation method according to claim 1, characterized in that, The active ingredients include: ethyl acetate, 2-butenal, isovaleral, n-butanol, hydroxyacetone, trioxymethylene, 2,3-pentanedione, pentanal, isopentanol, pyridine, 2-methylpropionic acid, pyrrole, n-pentanol, 3-methyl-2-buten-1-ol, 3-methyl-2-butenal, hexanal, 2-methyltetrahydrofuran-3-one, furfural, isovaleric acid, 2-methylbutyric acid, furfuryl alcohol, γ-butyrolactone, benzaldehyde, methylheptenone, 2-n-pentylfuran, 6-methyl-5-heptenyl-2-ol, 3-pyridinecarboxaldehyde, benzyl alcohol, phenylacetaldehyde, 2-acetylpyrrole, linalool, nonanal, 3-acetylpyridine, phenethyl alcohol, isophorone, 2,6,6 At least one of the following: trimethyl-2-cyclohexene-1,4-dione, atroaldehyde, menthol, anethole, indole, p-vinylguaiacol, nicotine, eugenol, solanone, damascene, β-caryophyllene, mesmin, geranylacetone, 4-phenylpyridine, 2,6-di-tert-butyl-p-cresol, dihydroactinol, 2,3-bipyridine, mesostachine A, mesostachine B, mesostachine C, mesostachine D, pentadecaldehyde, myristic acid, diene, neophytadiene, phytone, farnesylacetone A, methyl palmitate, isophytol, palmitic acid, ceftazidimetrienol A, ceftazidimetrienol B, farnesylacetone B, erucamide, and trans-squalene.

3. The preparation method according to claim 2, characterized in that, The first filter hole (3) is disposed on the rubbing surface (2).

Citation Information

Patent Citations

  • Extraction method of chlorogenic acid in tobacco leaves

    CN106631797A

  • Efficient separation and purification multilayer filtering device for biopharmacy

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  • Device for extracting tea polyphenol from low-grade green tea

    CN214103046U

  • Extraction device for plant trace elements

    CN216092323U

  • A tobacco leaf fragment rubbing and grinding reflux extraction device

    CN220966400U