Preparation method and application of natural tobacco dried fruit extract

Abstract

The application discloses a preparation method and application of a natural tobacco dry fruit extract, and comprises the following steps: firstly, crushing dry fruit raw materials; solvent extraction is performed on the first batch of dry fruit raw materials to obtain a dry fruit conventional extract; the dry fruit conventional extract is subjected to standing, filtration and vacuum concentration to obtain a dry fruit conventional concentrated solution; the second batch of dry fruit raw materials is subjected to ultrahigh pressure extraction to obtain an ultrahigh pressure extract; the dry fruit conventional extract and the ultrahigh pressure extract are mixed, and pH is adjusted; when a design temperature is reached, an enzyme preparation is added, and pressure enzymolysis reaction is performed to obtain a dry fruit enzymolysis solution; and the dry fruit enzymolysis solution is subjected to vacuum freeze-drying treatment to obtain the natural tobacco dry fruit extract. The extract has obvious dry fruit characteristic fragrance, and has the outstanding effects of strengthening aroma characteristics, improving eating taste and taste in application, and has excellent application value and market potential.

Description

Technical Field

[0001] This invention belongs to the field of natural tobacco flavoring preparation, specifically relating to a method for preparing and applying a natural tobacco dried fruit extract. Background Technology

[0002] Flavoring and flavoring technology is one of the core technologies affecting the style and sensory quality of cigarettes. Among natural tobacco flavoring raw materials, many natural dried fruit raw materials are processed into tobacco flavoring raw materials through technological processes, including red dates, dried plums, raisins, tamarind, figs, apricots, goji berries, etc. These natural dried fruit raw materials are generally extracted and concentrated using low-concentration ethanol solutions to prepare tinctures, extracts, and other extracts. These natural tobacco dried fruit extracts have simple processes, easy-to-control procedures, and low costs and prices. They are usually used in the base material of cigarettes, playing a role in harmonizing the tobacco aroma and solving taste and mouthfeel problems.

[0003] Traditional natural dried fruit flavoring ingredients have clear advantages: simple processing and low price. However, their disadvantages are also significant. For example, in cigarette applications, they have limited functionality and insufficient aroma, failing to effectively influence the aroma characteristics of cigarettes. The reasons for this are threefold: First, traditional natural dried fruit ingredients are rich in sugars but have limited volatile components. Traditional extraction processes are relatively simple and cannot effectively enrich these volatile components. Second, traditional extraction and concentration processes are often crude, leading to heat-sensitive reactions of the limited volatile components due to excessively high extraction or concentration temperatures, or browning reactions of the abundant sugars and acids in the raw materials. Third, the process design and application goals of these extracts are often not high, mostly focusing only on improving the taste and mouthfeel of cigarettes. Therefore, traditional natural dried fruit flavorings for cigarettes lack or are insufficient in characteristic aromas, failing to highlight the inherent aroma characteristics of the natural dried fruit ingredients and thus failing to contribute to enhancing the aroma characteristics and sensory quality of cigarettes.

[0004] Ultra-high pressure extraction technology is a green, environmentally friendly, easy-to-control, highly efficient, and easily industrialized process. Compared with conventional solvent extraction and hot reflux extraction methods, it can be carried out at room temperature or below, which is beneficial to protect heat-sensitive components. It also has the advantages of short extraction time, high extraction rate, and low energy consumption, making it very suitable for the preparation of natural tobacco fragrance raw materials.

[0005] Therefore, for natural raw materials such as dried fruits, ultra-high pressure extraction technology can be utilized to better enhance the contribution of dried fruit flavorings to aroma characteristics and sensory quality in cigarette applications, thereby improving the technical level, application scope and market value of this type of natural tobacco flavoring. Summary of the Invention

[0006] One object of the present invention is to provide a new technical solution for the preparation method of natural tobacco dried fruit extract.

[0007] According to a first aspect of the present invention, a method for preparing a natural tobacco dried fruit extract is provided.

[0008] The preparation method of this natural tobacco dried fruit extract includes the following steps: Step (1): Grind the natural dried fruit raw materials; Step (2): The first batch of dried fruit raw material is heated and extracted with a solvent to obtain a conventional extract of dried fruit. The solvent is ethanol with a volume percentage of 0-50%, the temperature is 100-120℃, the extraction time is 1-4h, and the mass ratio of the solvent to the mass of the dried fruit raw material is (5-10):1. Step (3): The conventional extract of dried fruit is subjected to static standing, filtration, and vacuum concentration to obtain a conventional concentrated extract of dried fruit. Step (4): The second batch of dried fruit raw material is subjected to ultra-high pressure extraction to obtain ultra-high pressure extract. The pressure of the ultra-high pressure extraction process is 100-300MPa, the pressure holding time is 5-10min, the pressure release time is 20-40s, and the mass ratio of the second batch of dried fruit raw material to the first batch of dried fruit raw material is 3:2. Step (5): After mixing the conventional concentrated liquid of dried fruit and the ultra-high pressure extract, a mixed liquid of dried fruit to be processed is obtained. The pH is adjusted to 3-6. When the material reaches a stable design temperature by heating, an enzyme preparation is added and the reaction is carried out under pressure to obtain the enzymatic hydrolysate of dried fruit. The temperature of the heating and pressurizing reaction is 20-70℃, and the temperature tolerance is strictly controlled within ±1℃ of the design temperature. The pressure is 1-3MPa and the reaction time is 10-15h. Step (6): The enzymatic hydrolysate of dried fruit is subjected to vacuum freeze-drying to obtain natural tobacco dried fruit extract.

[0009] Optionally, the dried fruit raw materials in step (1) include, but are not limited to, one or more of the following dried fruit raw materials: red dates, dried plums, raisins, tamarind, figs, apricots, and goji berries.

[0010] Optionally, the average size of the dried fruit raw material after pulverization in step (1) is 1-10 mm.

[0011] Optionally, the temperature of the vacuum concentration in step (3) is 50°C, the pressure is 0.08 MPa, and the concentration point is when the mass ratio of the concentrate to the dried fruit raw material is (1-4):1.

[0012] Optionally, the second portion of dried fruit raw material in step (4) can be the same as or different from the raw material in step (2).

[0013] Optionally, in step (4), before the second portion of dried fruit raw material is subjected to ultra-high pressure treatment, the second portion of dried fruit raw material is first soaked. The mass ratio of the second portion of dried fruit raw material to water in the soaking treatment is 1:(2-6), the time is 0.5-1.5h, and the temperature is 20-40℃.

[0014] Optionally, the enzyme preparation in step (5) is at least one of pectinase, cellulase, hemicellulase, protease and amylase, and the ratio of the enzyme preparation to the dried fruit mixture to be treated is (0.2-0.5):100, where the unit of material in the material-liquid ratio is g and the unit of liquid is mL.

[0015] Optionally, the ratio of enzyme preparation to dried fruit in the treatment solution is (0.3-0.4):100.

[0016] Optionally, the parameters for the vacuum freeze-drying process in step (6) are as follows: The freezing temperature is -80 to 20°C, and the vacuum pressure is 20 to 60 Pa.

[0017] According to a second aspect of the present invention, an application of the natural tobacco dried fruit extract described herein is provided, wherein the amount of the extract added is 0.1%-0.5%.

[0018] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention uses natural dried fruit raw materials as the research object. It first uses conventional extraction and ultra-high pressure extraction processes to process them in groups. After recovering the ethanol from the conventional extract, it is combined with the ultra-high pressure water extract, and then subjected to biological enzymatic hydrolysis and vacuum freeze-drying. The combination of parallel extraction and combined enzymatic hydrolysis not only retains the effect of traditional dried fruit extracts in improving the taste and mouthfeel of cigarettes, but also effectively controls the thermal reaction and browning reaction. This allows the final natural tobacco dried fruit extract to retain the characteristic aroma of the dried fruit raw materials to a certain extent. In cigarette applications, it effectively improves the aroma enhancement, sweetness enhancement and moisturizing effect, and enhances the cleanliness and comfort of the taste and aftertaste. Compared with traditional dried fruit extracts, the overall effect is significantly enhanced.

[0019] 2. In this invention, the dual-parallel extraction process, when targeting a single dried fruit raw material, retains the traditional preparation process of tobacco-grade dried fruit extracts while rationally incorporating ultra-high pressure extraction. This not only preserves the flavor and taste benefits of traditional dried fruit extracts but also leverages the high efficiency, environmental friendliness, and low energy consumption of ultra-high pressure extraction. More importantly, it protects the heat-sensitive volatile aroma components in the dried fruit extract, resulting in a final product with a balanced and harmonious aroma. Secondly, combining enzymatic hydrolysis and vacuum freeze-drying processes reduces the negative impact of thermal and browning reactions on the aroma characteristics of the dried fruit extract, significantly enhancing the preservation of characteristic volatile aroma components. Furthermore, the grouped extraction process design allows for flexible selection of different dried fruit raw materials for compound extraction within a single process system. It enables the targeted combination of different dried fruit raw materials based on their aroma and flavor advantages, resulting in a distinctive dried fruit extract with a prominent aroma characteristic.

[0020] 4. The raw materials of this invention are all natural plant materials. Only a small amount of low-concentration ethanol is used in the conventional extraction process. No organic solvents are used in other processes. The overall process is green and environmentally friendly. It is also simple and easy to operate and control, making it easy to achieve large-scale and industrialized production. This provides an innovative, technologically advanced and market-potential technical solution for the development of natural tobacco flavorings. Detailed Implementation

[0021] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit the present invention or its application or use. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0022] The method for preparing the natural tobacco dried fruit extract disclosed herein includes the following steps: Step (1): Grind the dried fruit raw materials.

[0023] To achieve better processing results, the average size of the dried fruit raw materials after pulverization in step (1) is 1-10 mm.

[0024] Step (2): The first batch of dried fruit raw material is extracted with a solvent to obtain a conventional extract of dried fruit. The solvent volume percentage is 0-50% ethanol, the temperature is 100-120℃, the extraction time is 1-4h, and the mass ratio of the solvent to the mass of the dried fruit raw material is (5-10):1.

[0025] Step (3): The conventional extract of dried fruit is subjected to static, filtration and vacuum concentration treatment to obtain conventional concentrated extract of dried fruit.

[0026] The temperature of the vacuum concentration process in step (3) is 50°C and the pressure is 0.08 MPa.

[0027] To ensure optimal processing results in subsequent steps, the mass ratio of the concentrated dried fruit solution to the raw dried fruit is (1-4):1.

[0028] Step (4): The second batch of dried fruit raw material is subjected to ultra-high pressure extraction to obtain ultra-high pressure extract. The pressure of ultra-high pressure extraction is 100-300MPa, the pressure holding time is 5-10min, the pressure release time is 20-40s, and the mass ratio of the second batch of dried fruit raw material to the first batch of dried fruit raw material is 3:2.

[0029] In order to achieve better ultra-high pressure extraction, in step (4), the second batch of dried fruit raw material is soaked before ultra-high pressure extraction.

[0030] In practice, the mass ratio of the second portion of dried fruit raw material to water in the soaking treatment can be 1:(2-6), the time can be 0.5-1.5h, and the temperature can be 20-40℃.

[0031] Step (5): After mixing the conventional concentrated liquid of dried fruit and the ultra-high pressure extract, a mixed liquid of dried fruit to be processed is obtained. The pH is adjusted to 3-6. When the material reaches a stable design temperature by heating, an enzyme preparation is added and the reaction is carried out under pressure to obtain a hydrolysate of dried fruit. The reaction temperature is 20-70℃, and the temperature tolerance is strictly controlled within ±1℃ of the design temperature. The pressure is 1-3MPa and the reaction time is 10-15h. In practice, malic acid aqueous solution or citric acid aqueous solution can be used to adjust the pH.

[0032] To ensure the effectiveness of the enzymatic hydrolysis reaction, the enzyme preparation in step (5) is at least one of pectinase, cellulase, hemicellulase, protease and amylase. The ratio of the enzyme preparation to the dried fruit mixture to be treated is (0.2-0.5):100, where the unit of material in the material-liquid ratio is g and the unit of liquid is mL.

[0033] To further improve the efficiency and effectiveness of the enzymatic hydrolysis reaction, the ratio of enzyme preparation to dried fruit mixture in the treatment solution is (0.3-0.4):100.

[0034] Step (6): The enzymatic hydrolysate of dried fruit is subjected to vacuum freeze-drying to obtain natural tobacco dried fruit extract.

[0035] The parameters for the vacuum freeze-drying process in step (6) can be as follows: freezing temperature is -80 to 20℃, and vacuum pressure is 20 to 60 Pa.

[0036] This disclosure also provides an application of a natural tobacco dried fruit extract, wherein the amount of dried fruit extract added is 0.1%-0.5%.

[0037] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, and the materials and reagents used are commercially available. Unless otherwise specified, the equipment used in the experiments is well known to those skilled in the art. Example

[0038] Weigh 200g of crushed jujube granules (average size 3-4mm) and add them to a 5L round-bottom flask. Add 1200g of 25% ethanol. Extraction conditions: temperature 110℃, time 2h, solvent to jujube raw material mass ratio 6:1. After extraction, allow to stand at room temperature, filter, collect the filtrate, and concentrate under reduced pressure to obtain 1000g of jujube concentrate. The mass ratio of jujube concentrate to jujube raw material is 2:1.

[0039] Weigh 300g of crushed jujube granules (average size 3-4mm), add 1500g of water and soak at 35℃ for 2h. The mass ratio of jujube raw material to water is 1:5. Then perform ultra-high pressure extraction to obtain ultra-high pressure extract. The pressure of ultra-high pressure extraction is 200MPa, the pressure holding time is 7min, and the pressure release time is 30s.

[0040] The regular concentrated jujube extract and the ultra-high pressure extract were mixed to obtain a dried fruit mixed solution to be processed. The pH was adjusted to 4.5, and then the solution was transferred to a high-pressure reactor. The water bath heating switch and the stirring switch were turned on. When the temperature of the material in the reactor stabilized at 40±1℃, the enzyme preparation was added, and then the reactor was sealed. The pressure of the high-pressure reactor was adjusted to 1.5 MPa, and the reaction time was 12 hours. After that, the heating switch was turned off, and the solution was allowed to cool naturally to room temperature to obtain the dried fruit enzymatic hydrolysate.

[0041] The dried fruit enzymatic hydrolysate was freeze-dried at -60℃ and 30Pa to obtain jujube extract A.

[0042] Comparative Example 1 Weigh 200g of crushed jujube granules (average size 3-4mm) and add them to a 5L round-bottom flask. Add 1200g of 25% ethanol. Extraction conditions: temperature 110℃, time 2h, solvent to jujube raw material mass ratio 6:1. After extraction, allow to stand at room temperature, filter, collect the filtrate, and concentrate under reduced pressure to obtain 1000g of jujube concentrate. The mass ratio of jujube concentrate to jujube raw material is 2:1.

[0043] Weigh 300g of crushed jujube granules (average size 3-4mm), add 1500g of water and soak at 35℃ for 2 hours. The mass ratio of jujube raw material to water is 1:5. Then filter to obtain jujube water extract.

[0044] The regular concentrated jujube extract and the jujube aqueous extract were mixed to obtain a dried fruit mixed solution to be processed. The pH was adjusted to 4.5, and then transferred to a high-pressure reactor. The water bath heating switch and the stirring switch were turned on. When the temperature of the material in the reactor stabilized at 40±1℃, the enzyme preparation was added, and then the reactor was sealed. The pressure of the high-pressure reactor was adjusted to 1.5 MPa. After the reaction time was 12 hours, the heating switch was turned off, and the mixture was allowed to cool naturally to room temperature to obtain the dried fruit enzymatic hydrolysate.

[0045] The dried fruit enzymatic hydrolysate was freeze-dried at -60℃ and 30Pa to obtain jujube extract B.

[0046] Comparative Example 2 Weigh 200g of crushed jujube granules (average size 3-4mm) and add them to a 5L round-bottom flask. Add 1200g of 25% ethanol. Extraction conditions: temperature 110℃, time 2h, solvent to jujube raw material mass ratio 6:1. After extraction, allow to stand at room temperature, filter, collect the filtrate, and concentrate under reduced pressure to obtain 1000g of jujube concentrate. The mass ratio of jujube concentrate to jujube raw material is 2:1.

[0047] Weigh 300g of crushed jujube granules (average size 3-4mm), add 1500g of water and soak at 35℃ for 2h. The mass ratio of jujube raw material to water is 1:5. Then perform ultra-high pressure extraction to obtain ultra-high pressure extract. The pressure of ultra-high pressure extraction is 200MPa, the pressure holding time is 7min, and the pressure release time is 30s.

[0048] The jujube extract was obtained by mixing the regular concentrated jujube extract and the ultra-high pressure extract and then freeze-drying them at -60℃ and 30Pa.

[0049] Jujube extracts A, B, and C prepared in the examples were added to the blank tobacco leaf group at a ratio of 0.03% respectively, and equilibrated at 22°C and 60% humidity for more than 12 hours. Cigarette products were then manufactured using laboratory processes in the cigarette industry. Sensory evaluation was then conducted according to YC / T415-2011, "Sensory Evaluation Method for Tobacco Products". The results are shown in Table 1.

[0050] Table 1 Sensory evaluation results Group Evaluation Result Description blank The aroma is slightly inferior, with insufficient aroma volume, slight burnt bitterness and woody off-flavors, diffuse and stuffy smoke, moderate irritation, and dry aftertaste with slight residue. Example 1 The aroma is good, with a good amount of fragrance. It has a slight fruity and brewing aroma, similar to stewed red dates. The sweetness is obvious. The smoke has a certain roundness and fluffiness, and is full and penetrating. There are few impurities and little irritation. The aftertaste is sweet and refreshing, and the comfort level is good. Comparative Example 1 The aroma is slightly better, with a moderate amount of fragrance, a slight fruity aroma, and a noticeable sweetness. The smoke is smooth and gentle, with few impurities and a slight irritation. The aftertaste is sweet, clean, and comfortable. Comparative Example 2 The aroma is slightly better, with a slightly better quantity and characteristic fruity aroma reminiscent of jujube skin. It has a certain sweetness, the smoke is clear and relatively rich, with a slight woody aroma and a slight irritation. The aftertaste is relatively clean and slightly astringent. As can be seen from the sensory evaluation results in Table 1, the jujube extracts prepared in the three examples can all modify and improve the sensory defects of the blank leaf group when applied to cigarettes, including aroma, off-flavors, irritation, smoke state and aftertaste. Jujube extract A prepared in Example 1 has a more outstanding effect, which can give cigarettes a distinct dried fruit aroma, effectively improve the sensory quality of cigarettes, and has the outstanding effect of strengthening aroma characteristics and improving taste and mouthfeel. It has excellent application value and market potential.

Claims

1. A method for preparing a natural tobacco dried fruit extract, characterized in that, Includes the following steps: Step (1): Grind the natural dried fruit raw materials; Step (2): The first batch of dried fruit raw material is extracted with a solvent to obtain a conventional extract of dried fruit. The solvent is ethanol with a volume percentage of 0-50%, the temperature is 100-120℃, the extraction time is 1-4h, and the mass ratio of the solvent to the mass of the dried fruit raw material is (5-10):

1. Step (3): The conventional extract of dried fruit is subjected to static standing, filtration, and vacuum concentration to obtain a conventional concentrated extract of dried fruit. Step (4): The second batch of dried fruit raw material is subjected to ultra-high pressure extraction to obtain ultra-high pressure extract. The pressure of the ultra-high pressure extraction process is 100-300MPa, the pressure holding time is 5-10min, the pressure release time is 20-40s, and the mass ratio of the second batch of dried fruit raw material to the first batch of dried fruit raw material is 3:

2. Step (5): After mixing the conventional concentrated liquid of dried fruit and the ultra-high pressure extract, a mixed liquid of dried fruit to be processed is obtained. The pH is adjusted to 3-6. When the material reaches a stable design temperature by heating, an enzyme preparation is added and the reaction is carried out under pressure to obtain a hydrolysate of dried fruit. The reaction temperature is 20-70℃, and the temperature tolerance is strictly controlled within ±1℃ of the design temperature. The pressure is 1-3MPa and the reaction time is 10-15h. Step (6): The enzymatic hydrolysate of dried fruit is subjected to vacuum freeze-drying to obtain natural tobacco dried fruit extract.

2. The method for preparing the natural tobacco dried fruit extract according to claim 1, characterized in that, The dried fruit ingredients in step (1) include, but are not limited to, one or more of the following: red dates, dried plums, raisins, tamarind, figs, apricots, and goji berries.

3. The method for preparing the natural tobacco dried fruit extract according to claim 1, characterized in that, The average size of the dried fruit raw material after pulverization in step (1) is 1-10 mm.

4. The method for preparing the natural tobacco dried fruit extract according to claim 1, characterized in that, The vacuum concentration in step (3) is carried out at a temperature of 50°C and a pressure of 0.08 MPa. The concentration point is when the mass ratio of the concentrate to the dried fruit raw material is (1-4):

1.

5. In the method for preparing natural tobacco dried fruit extract according to claim 1, the second portion of dried fruit raw material in step (4) may be the same as or different from the raw material in step (2).

6. The method for preparing the natural tobacco dried fruit extract according to claim 1, characterized in that, In step (4), before the second portion of dried fruit raw material is extracted under ultra-high pressure, the second portion of dried fruit raw material is soaked. The mass ratio of the second portion of dried fruit raw material to water during the soaking process is 1:(2-6), the time is 0.5-1.5h, and the temperature is 20-40℃.

7. The method for preparing the natural tobacco dried fruit extract according to claim 1, characterized in that, The enzyme preparation in step (5) is at least one of pectinase, cellulase, hemicellulase, protease and amylase. The ratio of the enzyme preparation to the liquid to be treated with the dried fruit is (0.2-0.5):100, where the unit of material in the material-liquid ratio is g and the unit of liquid is mL.

8. The method for preparing the natural tobacco dried fruit extract according to claim 7, characterized in that, The ratio of enzyme preparation to dried fruit in the treatment solution is (0.3-0.4):

100.

9. The method for preparing the natural tobacco dried fruit extract according to claim 1, characterized in that, The parameters for the vacuum freeze-drying process in step (6) are as follows: freezing temperature is -80 to 20°C, and vacuum pressure is 20 to 60 Pa.

10. A method for preparing a natural tobacco dried fruit extract according to any one of claims 1 to 9, characterized in that, The application rate of dried fruit extract is 0.1%-0.5%.