Preparation method of aroma-carrying particles with coffee aroma characteristic, product and application of aroma-carrying particles

Abstract

The invention provides a preparation method of fragrance-carrying particles with coffee fragrance characteristics and a product and application of the fragrance-carrying particles. The product obtained by the method disclosed by the invention can play roles in coordinating smoke, improving fragrance richness and improving the sensory quality of the product. In addition, the raw material used in the preparation method is bio-based waste coffee grounds, so that the production cost can be reduced, the development requirements of enterprises on cost reduction and efficiency improvement are met, and high-value application of low-cost bio-based waste can be realized.

Description

Technical Field

[0001] The present invention belongs to the technical field of tobacco processing, and particularly relates to a preparation method, product and application of flavor-loaded particles with coffee aroma characteristics. Background Art

[0002] In recent years, cigarette products with coffee flavor or characteristics similar to Maillard reaction products have been increasingly favored by consumers at home and abroad. With the widespread popularity of coffee among young people in China, using coffee flavorings to enrich the flavor characteristics of cigarettes obviously has a large consumer market. Moreover, many tobacco flavor extracts and the like already use many coffee flavorings or extracts.

[0003] CN119034252A discloses a method for extracting tobacco coffee flavor adjuvants from coffee bean powder, the method comprising: mixing coffee bean powder with water and adding a saponin-type surfactant to obtain a mixed solution; subjecting the mixed solution to subcritical extraction and performing solid-liquid separation to obtain a coffee extract. This method does not require the use of functional organic solvents, is environmentally friendly and safe; improves the extraction rate of fat-soluble components in coffee bean powder, and the characteristic aroma of the coffee extract is more coordinated with the tobacco flavor, which can improve the taste and grade of cigarette products.

[0004] CN118834727A discloses a coffee essence and its preparation method and application. In this method, coffee powder is roasted and then extracted with ethanol to obtain an extract and coffee residue; the extract is concentrated 1, and the obtained extract is dissolved with ethanol, and then successively subjected to freezing, filtration and concentration 2 to obtain extract 1; the coffee residue is extracted with water, and the obtained extract is successively subjected to extraction, evaporation to dryness and dilution to obtain extract 2; extract 1 and extract 2 are mixed to obtain a coffee essence integrating special aromas such as caramel sweetness, baking aroma and nut aroma. Adding it to the tobacco sheet of a heated cigarette imparts a strong coffee aroma to the heated cigarette, and the aroma is rich and can be naturally integrated with the tobacco base aroma, and the application effect is good.

[0005] At present, the methods for directly extracting flavor substances from coffee are relatively single, and the extraction methods are time-consuming, energy-consuming and inefficient, which is not conducive to the retention of coffee flavor substances and active ingredients. Therefore, there is an urgent need to provide an extraction method for coffee flavor that has broad application prospects both in terms of cost and effect to meet the application requirements. Summary of the Invention

[0006] The object of the present invention is to provide a preparation method, product and application of flavor-loaded particles with coffee aroma characteristics. The particle product obtained by the method can coordinate the smoke, enhance the richness of the aroma, improve the sensory quality of cigarette products and highlight the cigarette style characteristics, thereby laying a theoretical foundation for innovative applications in the tobacco industry.

[0007] To achieve the object of the present invention, the following technical solutions are adopted in the present invention:

[0008] In a first aspect, the present invention provides a method for preparing a flavor-carrying particle with coffee aroma characteristics, and the preparation method includes:

[0009] (1) Defat and dry coffee grounds, then mix them with pure water and perform water extraction to obtain an extract, and collect the supernatant after centrifugation;

[0010] (2) Concentrate the supernatant to obtain a concentrated solution, add ethanol to the concentrated extract for extraction, and then centrifuge the extract to collect the precipitate;

[0011] (3) Mix the precipitate with water, collect the retentate after dialysis and perform freeze-drying, and grind the dried powder to obtain a coffee ground extract;

[0012] (4) Mix the coffee ground extract, polysaccharide and chloromalonic acid in an aqueous sodium hydroxide solution, and then perform low-temperature plasma treatment on the mixture to obtain the flavor-carrying particle with coffee aroma characteristics.

[0013] In the method of the present invention, through defatting, water extraction and alcohol extraction of coffee grounds, macromolecular substances such as polysaccharides and proteins in coffee grounds can be better extracted and separated. Compared with the method of directly extracting flavor substances from coffee, it not only has low cost and low energy consumption, but also uses the macromolecules with cavity structure formed after coffee grounds extraction as carriers, which is beneficial to the preservation of the original coffee flavor. When it is compounded with other flavors and adsorption substances, multi-flavor flavor-carrying particles can be constructed, and it also has additional antioxidant activity and moisturizing properties. When it is applied to cigarettes, it can coordinate the smoke, enhance the richness of the aroma and improve the sensory quality of the product.

[0014] At the same time, the present invention uses coffee extract in combination with polysaccharide and chloromalonic acid. Since there are a large number of -OH groups in the molecular cavity of polysaccharide, and chloromalonic acid can increase the number of hydroxyl groups, hydrogen bonds can be formed with organic molecules with cavity structure, improving the adsorption effect of the material on phenol, carbon monoxide and tar in the smoke. Finally, low-temperature plasma is used to perform surface treatment on the material, and through etching, the pores on the fiber surface are increased, further enhancing the interception efficiency of the smoke.

[0015] In addition, the raw material used in the preparation method of the present invention is coffee grounds, a bio-based waste, which can not only reduce the production cost, but also realize the high-value application of low-cost bio-based waste, making a positive response to the country's goal of accelerating waste recycling.

[0016] Preferably, the solvent used for defatting in step (1) is n-hexanol and / or ethyl acetate.

[0017] Preferably, the solvent used for degreasing is n-hexanol and ethyl acetate.

[0018] In the present invention, using n-hexanol and ethyl acetate as the degreasing solvent can not only remove the odor of oxidized oil in coffee grounds to the greatest extent, but also well retain macromolecular substances such as polysaccharides and proteins in the coffee grounds.

[0019] Preferably, the mass ratio of n-hexanol to ethyl acetate is 1:(1 - 2), and for example, it can be 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8 or 1:1.9, etc.

[0020] Preferably, the temperature for degreasing is 70 - 90 °C, and for example, it can be 72 °C, 75 °C, 78 °C, 80 °C, 82 °C, 85 °C or 88 °C, etc.

[0021] Preferably, the mass ratio of the coffee grounds to pure water in step (1) is 1:(20 - 30), and for example, it can be 1:21, 1:23, 1:25, 1:27 or 1:29, etc.

[0022] Preferably, the temperature for water extraction in step (1) is 90 - 100 °C (for example, it can be 91 °C, 93 °C, 95 °C, 97 °C or 99 °C, etc.), and the time is 1 - 5 h (for example, it can be 1.5 h, 2 h, 2.5 h, 3 h, 3.5 h, 4 h or 4.5 h, etc.).

[0023] Preferably, the rotation speed for centrifugation in step (1) is 3000 - 5000 g (for example, it can be 3200 g, 3500 g, 3700 g, 4000 g, 4200 g, 4500 g or 4800 g, etc.), the time is 10 - 20 min (for example, it can be 11 min, 13 min, 15 min, 17 min or 19 min, etc.), and the temperature is 1 - 5 °C (for example, it can be 1 °C, 2 °C, 3 °C, 4 °C or 5 °C, etc.).

[0024] Preferably, in step (2), it is concentrated to 20 - 30% of the original volume of the extract, and for example, it can be 21%, 23%, 25%, 27% or 29%, etc.

[0025] Preferably, the temperature for concentration is 40 - 50 °C, and for example, it can be 41 °C, 43 °C, 45 °C, 47 °C or 49 °C, etc.

[0026] Preferably, the dosage of ethanol in step (2) is 1 - 5 times the volume of the concentrated solution, and for example, it can be 1 time, 2 times, 3 times, 4 times or 5 times, etc.

[0027] Preferably, the ethanol includes absolute ethanol or an aqueous ethanol solution with a concentration of 80-99% (such as 81%, 83%, 85%, 87%, 90%, 92%, 95% or 97%, etc.).

[0028] Preferably, the temperature of the alcohol extraction is 1-5°C (such as 1°C, 2°C, 3°C, 4°C or 5°C, etc.), and the time is 10-20 min (such as 11 min, 13 min, 15 min, 17 min or 19 min, etc.).

[0029] Preferably, in step (2), the centrifugation speed is 3000-5000 g (such as 3200 g, 3500 g, 3700 g, 4000 g, 4200 g, 4500 g or 4800 g, etc.), the time is 10-20 min (such as 11 min, 13 min, 15 min, 17 min or 19 min, etc.), and the temperature is 1-5°C (such as 1°C, 2°C, 3°C, 4°C or 5°C, etc.).

[0030] Preferably, in step (3), the mass ratio of the precipitate to water is 1:(10-20), such as 1:11, 1:13, 1:15, 1:17 or 1:19, etc.

[0031] Preferably, the dialysis is carried out in a dialysis bag.

[0032] Preferably, the molecular weight cut-off of the dialysis bag is 3000-4000 Da, such as 3100 Da, 3300 Da, 3500 Da, 3700 Da or 3900 Da.

[0033] Preferably, the temperature of the dialysis is 20-30°C (such as 21°C, 23°C, 25°C, 27°C or 29°C, etc.), and the time is 2-4 days (such as 2.2 days, 2.5 days, 2.8 days, 3 days, 3.2 days, 3.5 days or 3.8 days, etc.).

[0034] Preferably, the polysaccharide in step (4) includes any one or a combination of at least two of sodium alginate, chitosan or cyclodextrin.

[0035] Preferably, the polysaccharide is cyclodextrin.

[0036] Preferably, the mass ratio of the coffee grounds extract, the polysaccharide to chloromalonic acid is (5-10):(1-2):(2-3).

[0037] Preferably, the concentration of the sodium hydroxide aqueous solution is 10-20%, such as 11%, 13%, 15%, 17% or 19%, etc.

[0038] Preferably, the material-liquid ratio of the coffee residue extract to the sodium hydroxide aqueous solution is 0.05-0.2 g / mL.

[0039] For example, it can be 0.06 g / mL, 0.08 g / mL, 0.1 g / mL, 0.12 g / mL, 0.15 g / mL, 0.17 g / mL or 0.19 g / mL, etc.

[0040] Preferably, the temperature of the mixing in step (4) is 85-95 °C (for example, it can be 86 °C, 88 °C, 90 °C, 92 °C or 94 °C, etc.), and the time is 1.5-3 h (for example, it can be 1.6 h, 1.8 h, 2 h, 2.2 h, 2.5 h, 2.7 h or 2.9 h, etc.).

[0041] The specific steps of the low-temperature plasma treatment in step (4) are as follows:

[0042] Add the mixture into the phosphate buffer solution, and then carry out low-temperature plasma treatment under half of the magnetic force.

[0043] Preferably, the phosphate solution is PBS solution, with a concentration of 0.05-0.2 mol / L (for example, it can be 0.06 mol / L, 0.08 mol / L, 0.1 mol / L, 0.12 mol / L, 0.15 mol / L, 0.18 mol / L, etc.), and the pH is 7-8 (for example, it can be 7.1, 7.3, 7.5, 7.7, or 7.9, etc.).

[0044] Preferably, the material-liquid ratio of the mixture to the phosphate is 0.01-0.05 g / mL, for example, it can be 0.02 g / mL, 0.03 g / mL or 0.04 g / mL, etc.

[0045] Preferably, during the low-temperature plasma treatment, the voltage is 50-90 V (for example, it can be 55 V, 60 V, 65 V, 70 V, 75 V, 80 V or 85 V, etc.), the current is 0.5-2 A (for example, it can be 0.6 A, 0.8 A, 1 A, 1.2 A, 1.5 A or 1.8 A, etc.), the distance between the two electrodes is 5-7 mm (for example, it can be 5.1 mm, 5.3 mm, 5.5 mm, 5.8 mm, 6 mm, 6.2 mm, 6.5 mm or 6.8 mm, etc.), and the discharge time is 80-100 s (for example, it can be 82 s, 85 s, 88 s, 90 s, 92 s, 95 s or 98 s, etc.). Other specific point values within the above numerical ranges can be selected, and will not be elaborated one by one here.

[0046] In the second aspect, the present invention provides a fragrance-carrying particle with coffee aroma characteristics, and the fragrance-carrying particle with coffee aroma characteristics is prepared by using the preparation method as described in the first aspect.

[0047] Thirdly, the present invention provides an application of the aroma-carrying particles with coffee aroma characteristics as described in the second aspect in a cigarette filter material.

[0048] Compared with the prior art, the present invention has the following beneficial effects:

[0049] (1) In the method of the present invention, through degreasing, water extraction, and alcohol extraction of coffee grounds, macromolecular substances such as polysaccharides and proteins in the coffee grounds can be better extracted and separated. At the same time, using the macromolecular structure of polysaccharide-protein as a carrier, it is compounded with other flavors and adsorbing substances to form multi-aroma type aroma-carrying particles. After applying them to cigarettes, it can coordinate the smoke, enhance the richness of the aroma, and improve the sensory quality of the product.

[0050] (2) The raw material used in the preparation method of the present invention is the bio-based waste coffee grounds, which can not only reduce the production cost, meet the development requirements of enterprises for cost reduction and efficiency improvement, but also realize the high-value application of low-cost bio-based waste. Specific Embodiments

[0051] The technical solutions of the present invention will be further described below through specific embodiments. Those skilled in the art should understand that the embodiments are only for helping to understand the present invention and should not be regarded as specific limitations to the present invention.

[0052] The raw materials involved in the following examples and comparative examples can be used as long as they are purchased from regular distributors.

[0053] Example 1

[0054] This example provides an aroma-carrying particle with coffee aroma characteristics. The preparation method of the aroma-carrying particle with coffee aroma characteristics is as follows:

[0055] (1) Place the wet coffee grounds obtained from a coffee shop in an oven and dry them at 105 °C until constant weight. After drying, the coffee grounds sample is refluxed for 3 h for degreasing with a mixture of n-hexanol and ethyl acetate with a mass ratio of 2:3 (the amount used is 1 time the mass of the coffee grounds) at 80 °C using a Soxhlet extractor, then dried again. Then, it is mixed with pure water at a mass ratio of 1:25 and subjected to water extraction at 95 °C for 3 h to obtain an extract. After centrifugation at 4000 g and 3 °C for 15 min, the supernatant is collected;

[0056] (2) Concentrate the supernatant at 45 °C to 25% of the original volume to obtain a concentrated solution. Add the concentrated solution to anhydrous ethanol (3 times the volume of the concentrated solution) and perform alcohol extraction at 3 °C for 15 min. Then, centrifuge the extract at 4000 g and 3 °C for 15 min to collect the precipitate;

[0057] (3) Mix the precipitate with water at a mass ratio of 1:15, use a 3500 Da dialysis bag at 25 °C, dialyze for 3 days and change the water every 12 h. Collect the retentate in the dialysis bag and perform freeze-drying. Grind the dried powder to obtain the coffee residue extract;

[0058] (4) Add the coffee residue extract and cyclodextrin to an aqueous sodium hydroxide solution (the material-liquid ratio with the coffee residue extract is 0.1 g / mL), mix at 90 °C, then add chloro-malonic acid with stirring and continue to mix and stir for 2 h to obtain a mixture. The mass ratio of the coffee residue extract, cyclodextrin to chloro-malonic acid is 8:1.5:2.5;

[0059] (5) Add the mixture to a PBS solution (0.1 mol / L, pH value 7.4). The material-liquid ratio of the mixture to the PBS solution is 0.02 g / mL. Stir magnetically at 25 °C and 500 r / min for 4 h, cool down to 4 °C and hydrate for 18 h, then perform low-temperature plasma treatment at a voltage of 70 V, a current of 1 ± 0.1 A, a discharge time of 90 s, and a distance between the two electrodes of 7 mm. After freeze-drying, the aroma-carrying particles with coffee aroma characteristics are obtained.

[0060] Example 2

[0061] This example provides an aroma-carrying particle with coffee aroma characteristics. The preparation method of the aroma-carrying particle with coffee aroma characteristics is as follows:

[0062] (1) Place the wet coffee residue obtained from the coffee shop in an oven and dry it at 105 °C to constant weight. After drying, the coffee residue sample is defatted by refluxing with a 1:1 mixture of n-hexanol and ethyl acetate (the amount used is 1 time the mass of the coffee residue) in a Soxhlet extractor at 70 °C for 4 h, then dried again. Then mix it with pure water at a mass ratio of 1:30 and perform water extraction at 90 °C for 5 h to obtain an extract. Centrifuge at 3000 g and 5 °C for 20 min and collect the supernatant;

[0063] (2) Concentrate the supernatant at 40 °C to 28% of the original volume to obtain a concentrated solution. Add the concentrated solution to a 95% ethanol aqueous solution (4 times the volume of the concentrated solution), perform ethanol extraction at 2 °C for 20 min, then centrifuge the extract at 5000 g and 2 °C for 10 min to collect the precipitate;

[0064] (3) Mix the precipitate with water at a mass ratio of 1:10, use a 4000 Da dialysis bag at 20 °C, dialyze for 4 days and change the water every 12 h. Collect the retentate in the dialysis bag and perform freeze-drying. Grind the dried powder to obtain the coffee residue extract;

[0065] (4) Add the coffee residue extract and cyclodextrin into an aqueous sodium hydroxide solution (the material-liquid ratio with the coffee residue extract is 0.15 g / mL), mix at 95 °C, then add chloro-malonic acid with stirring and continue to mix and stir for 1.5 h to obtain a mixture. The mass ratio of the coffee residue extract, cyclodextrin to chloro-malonic acid is 5:1:2;

[0066] (5) Add the mixture into a PBS solution (0.1 mol / L, pH value 7.4). The material-liquid ratio of the mixture to the PBS solution is 0.01 g / mL. Stir magnetically at 25 °C and 500 r / min for 4 h, cool down to 4 °C and hydrate for 18 h, then carry out low-temperature plasma treatment at a voltage of 60 V, a current of 1.5 ± 0.1 A, a discharge time of 80 s, and a distance between the two electrodes of 6 mm. After freeze-drying, the fragrant-loaded particles with coffee aroma characteristics are obtained.

[0067] Example 3

[0068] This example provides a kind of fragrant-loaded particles with coffee aroma characteristics. The preparation method of the fragrant-loaded particles with coffee aroma characteristics is as follows:

[0069] (1) Place the wet coffee residues obtained from the coffee shop in an oven and dry at 105 °C until constant weight. After drying, the coffee residue sample is defatted by refluxing with a mixture of n-hexanol and ethyl acetate with a mass ratio of 1:2 (the amount used is 1 time the mass of the coffee residues) in a Soxhlet extractor at 90 °C for 2 h, then dried again, and then mixed with pure water at a mass ratio of 1:20 and subjected to water extraction at 98 °C for 2 h to obtain an extract. Centrifuge at 5000 g and 2 °C for 12 min and collect the supernatant;

[0070] (2) Concentrate the supernatant at 50 °C to 23% of the original volume to obtain a concentrated solution. Add the concentrated solution into a 90% ethanol aqueous solution (2 times the volume of the concentrated solution), carry out ethanol extraction at 5 °C for 10 min, then centrifuge the extract at 3000 g and 5 °C for 20 min, and collect the precipitate;

[0071] (3) Mix the precipitate with water at a mass ratio of 1:20, use a 3000 Da dialysis bag at 30 °C, dialyze for 2 days and change the water every 12 h. Collect the retentate in the dialysis bag and carry out freeze-drying. Grind the dried powder to obtain the coffee residue extract;

[0072] (4) Add the coffee residue extract and cyclodextrin into an aqueous sodium hydroxide solution (the material-liquid ratio with the coffee residue extract is 0.2 g / mL), mix at 85 °C, then add chloro-malonic acid with stirring and continue to mix and stir for 3 h to obtain a mixture. The mass ratio of the coffee residue extract, cyclodextrin to chloro-malonic acid is 10:2:3;

[0073] (5) Add the mixture to PBS solution (0.1 mol / L, pH 7.4). The ratio of the mixture to the PBS solution is 0.03 g / mL. Stir magnetically at 25 °C and 500 r / min for 4 h, cool down to 4 °C and hydrate for 18 h. Then, perform low-temperature plasma treatment at a voltage of 50 V, a current of 0.8 ± 0.1 A, a discharge time of 90 s, and a distance between the two electrodes of 5 mm. After freeze-drying, the aroma-loaded particles with coffee aroma characteristics are obtained.

[0074] Example 4

[0075] This example provides an aroma-loaded particle with coffee aroma characteristics. The difference in its preparation method from Example 1 is only that the solvent used for defatting in step (1) is only n-hexanol, and the amount of defatting solvent is kept unchanged. The remaining steps and process parameters are the same as those in Example 1.

[0076] Example 5

[0077] This example provides an aroma-loaded particle with coffee aroma characteristics. The difference in its preparation method from Example 1 is only that the solvent used for defatting in step (1) is only ethyl acetate, and the amount of defatting solvent is kept unchanged. The remaining steps and process parameters are the same as those in Example 1.

[0078] Example 6

[0079] This example provides an aroma-loaded particle with coffee aroma characteristics. The difference in its preparation method from Example 1 is only that a dialysis bag with a molecular weight cut-off of 2500 Da is used in step (3). The remaining steps and process parameters are the same as those in Example 1.

[0080] Example 7

[0081] This example provides an aroma-loaded particle with coffee aroma characteristics. The difference in its preparation method from Example 1 is only that a dialysis bag with a molecular weight cut-off of 5000 Da is used in step (3). The remaining steps and process parameters are the same as those in Example 1.

[0082] Example 8

[0083] This example provides an aroma-loaded particle with coffee aroma characteristics. The difference in its preparation method from Example 1 is only that the voltage during low-temperature plasma treatment in step (5) is 30 V, and parameters such as current, discharge time, and distance between the two electrodes are kept unchanged. The remaining steps and process parameters are the same as those in Example 1.

[0084] Example 9

[0085] This embodiment provides a flavor-carrying particle with the characteristic of coffee aroma. The difference in its preparation method from that of Embodiment 1 is only that the voltage during the low-temperature plasma treatment in step (5) is 100V, and the parameters such as current, discharge time, and distance between the two electrodes remain unchanged, and the remaining steps and process parameters are the same as those in Embodiment 1.

[0086] Comparative Example 1

[0087] This comparative example provides a flavor-carrying particle with the characteristic of coffee aroma. The difference in its preparation method from that of Embodiment 1 is only that degreasing treatment is not carried out in step (1), and after drying the wet coffee residue, it is mixed with pure water for water extraction, and the water extraction process parameters remain unchanged, and the remaining steps and process parameters are the same as those in Embodiment 1.

[0088] Comparative Example 2

[0089] This comparative example provides a flavor-carrying particle with the characteristic of coffee aroma. The difference in its preparation method from that of Embodiment 1 is only that step (3) is not included, and after drying the precipitate in step (2), step (4) is carried out, and the remaining steps and process parameters are the same as those in Embodiment 1.

[0090] Comparative Example 3

[0091] This comparative example provides a flavor-carrying particle with the characteristic of coffee aroma. The difference in its preparation method from that of Embodiment 1 is only that step (4) is as follows:

[0092] The coffee residue extract and cyclodextrin are added to an aqueous sodium hydroxide solution (the material-liquid ratio with the coffee residue extract is 0.1 g / mL) and mixed at 90°C for 2 h to obtain a mixture, and the mass ratio of the coffee residue extract to cyclodextrin is 8:1.5;

[0093] The remaining steps and process parameters are the same as those in Embodiment 1.

[0094] Comparative Example 4

[0095] This comparative example provides a flavor-carrying particle with the characteristic of coffee aroma. The difference in its preparation method from that of Embodiment 1 is only that step (4) is as follows: The coffee residue extract is added to an aqueous sodium hydroxide solution (the material-liquid ratio with the coffee residue extract is 0.1 g / mL) and mixed at 90°C, and then chloromalonic acid is added with stirring and mixed and stirred for another 2 h to obtain a mixture, and the mass ratio of the coffee residue extract to chloromalonic acid is 8:2.5;

[0096] The remaining steps and process parameters are the same as those in Embodiment 1.

[0097] Comparative Example 5

[0098] This comparative example provides a flavor-carrying particle with coffee aroma characteristics. The difference in its preparation method from that of Example 1 is only that it does not include step (5). After freeze-drying the mixture obtained in step (4), the flavor-carrying particle with coffee aroma characteristics is obtained;

[0099] The remaining steps and process parameters are the same as those in Example 1.

[0100] Test Example 1 Sensory Quality

[0101] The flavor-carrying particles with coffee aroma characteristics obtained in Examples 1-9 and Comparative Examples 1-5 were respectively added to the filter rod at 70 mg / rod, and then test cigarettes were made with the tobacco cut on the machine. Cigarettes without adding any flavoring agents were prepared by the same process as control cigarettes. The test cigarettes and control cigarettes were subjected to sensory quality tests according to national standards.

[0102] Thirteen professional smokers were organized to conduct sensory scoring on each index of the cigarettes obtained above according to GB5606.4-2005 "Cigarettes - Part 4: Sensory Technical Requirements". The specific definitions of the sensory quality evaluation indexes are shown in Table 1, the scoring criteria are shown in Table 2, and the scoring results are shown in Table 3 (the average value of each group is taken and reserved to one decimal place).

[0103] Table 1

[0104]

[0105] Table 2

[0106]

[0107]

[0108] Table 3

[0109]

[0110] It can be seen from Table 3 that compared with the control cigarettes, the flavor-carrying particles with coffee aroma characteristics obtained in Examples 1-3 of the present invention can endow the cigarettes with excellent coffee aroma characteristics after being added to the cigarettes, and the harmony and taste of the cigarettes are better, and the indexes such as foreign smell and irritation are lower.

[0111] It can be seen from Examples 4-5 that when the solvents used for degreasing are not n-hexanol and ethyl acetate defined in the present invention, it will affect the effect of the flavor-carrying particles in improving the taste of cigarettes;

[0112] It can be seen from Examples 6-7 that when the molecular weight cut-off of the dialysis bag used for dialysis is not within the defined range of the present invention, it will also affect the taste and coffee aroma of the cigarettes; it can be seen from Comparative Example 1 that when the coffee grounds are not degreased, the foreign smell and irritation indexes of the final cigarettes are higher, and the harmony is worse;

[0113] As can be seen from Comparative Example 2, when dialysis treatment is not carried out after alcohol extraction, there are more impurities in the obtained particles, and thus the various indexes of the obtained cigarettes also decrease;

[0114] As can be seen from Comparative Examples 3 and 4, when the coffee extract is not used in combination with any one of chloromalonic acid and cyclodextrin, the flavor-enhancing effect of the particles is also poor, and the sensory quality of the cigarettes is poor;

[0115] As can be seen from Comparative Example 5, when the coffee extract is not subjected to subsequent low-temperature plasma treatment, the sensory quality of the cigarettes is also significantly poor.

[0116] Comparison of the release amounts of harmful chemical components in the mainstream smoke of Test Example 2

[0117] The aroma-carrying particles with coffee aroma characteristics obtained in Examples 1-9 and Comparative Examples 1-5 were respectively added to the filter rod at 70 mg / cigarette, and then the test cigarettes were made on a cigarette making machine with cut tobacco. Cigarettes without adding any other flavoring agents were prepared by the same process as the blank control cigarettes, and the release amounts of harmful chemical components in the mainstream smoke captured from the test cigarettes and the blank control cigarettes were tested.

[0118] Test method:

[0119] The tar content was determined by measuring the total particulate matter and tar with a smoking machine for conventional analysis of cigarettes according to GB / T 19609-2004;

[0120] The CO content was determined by the non-dispersive infrared method for the determination of carbon monoxide in the gas phase of cigarette mainstream smoke according to GB / T 23356-2009;

[0121] The phenol content was determined by the high performance liquid chromatography method for the determination of main phenolic compounds in cigarette mainstream smoke according to YC / T 255-2008;

[0122] The results are shown in Table 4 below.

[0123] Table 4

[0124]

[0125]

[0126] As can be seen from the data in Table 4, the aroma-carrying particles with coffee aroma characteristics prepared in Examples 1-3 of the present invention can effectively reduce the harmful chemical components in the mainstream smoke when used in cigarettes.

[0127] As can be seen from Examples 8-9, when the voltage of the low-temperature plasma treatment is too low, the surface etching effect on the material is poor, and thus there are fewer surface pores in the material, reducing the adsorption effect of the final product on the mainstream smoke; while when the voltage is too high, the substances exposed on the surface will be degraded and etched away, which will also affect the total amount of surface pores of the material;

[0128] As can be seen from Comparative Example 5, when low-temperature plasma treatment is not carried out, the adsorption effect of the particles on the flue gas is significantly worse.

[0129] The applicant declares that the present invention illustrates a preparation method, product and application of a flavor-carrying particle with coffee aroma characteristics through the above-mentioned embodiments. However, the present invention is not limited to the above detailed methods, that is, it does not mean that the present invention must rely on the above detailed methods to be implemented. Those skilled in the art should understand that any improvement to the present invention, the equivalent substitution of each raw material of the product of the present invention, the addition of auxiliary components, the selection of specific methods, etc. all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A preparation method of flavor-carrying particles with coffee aroma characteristics, characterized in that, The preparation method includes: (1) Degrease the coffee grounds and then dry them, then mix them with pure water and perform water extraction to obtain an extract, and collect the supernatant after centrifugation; (2) Concentrate the supernatant to obtain a concentrated solution, add ethanol to the concentrated solution for extraction, then centrifuge the extract, and collect the precipitate; (3) Mix the precipitate with water, dialyze and collect the retentate and perform freeze-drying, and grind the dried powder to obtain the coffee grounds extract; (4) Mix the coffee grounds extract, polysaccharide and chloromalonic acid in an aqueous sodium hydroxide solution, then perform low-temperature plasma treatment on the mixture, and obtain the aroma-loaded particles with coffee aroma characteristics after freeze-drying.

2. The preparation method according to claim 1, characterized in that, The solvent used for degreasing in step (1) is n-hexanol and / or ethyl acetate; Preferably, the solvent used for degreasing is n-hexanol and ethyl acetate; Preferably, the mass ratio of n-hexanol to ethyl acetate is 1:(1-2); Preferably, the temperature of degreasing is 70-90°C; Preferably, the mass ratio of the coffee grounds to pure water in step (1) is 1:(20-30); Preferably, the temperature of water extraction in step (1) is 90-100°C, and the time is 1-5 h; Preferably, the rotation speed of centrifugation in step (1) is 3000-5000 g, the time is 10-20 min, and the temperature is 1-5°C.

3. The preparation method according to claim 1 or 2, characterized in that, In step (2), the concentration is to 20-30% of the original volume of the extract; Preferably, the temperature of concentration is 40-50°C.

4. The preparation method according to any one of claims 1-3, characterized in that, The amount of ethanol used in step (2) is 1-5 times the volume of the concentrated solution; Preferably, the ethanol includes anhydrous ethanol or an aqueous ethanol solution with a concentration of 80-99%; Preferably, the temperature of ethanol extraction is 1-5°C, and the time is 10-20 min.

5. The preparation method according to any one of claims 1 to 4, characterized in that, The rotation speed of centrifugation in step (2) is 3000-5000 g, the time is 10-20 min, and the temperature is 1-5°C.

6. The preparation method according to any one of claims 1-5, characterized in that, The mass ratio of the precipitate to water in step (3) is 1:(10-20); Preferably, the dialysis is carried out in a dialysis bag; Preferably, the molecular weight cut-off of the dialysis bag is 3000-4000 Da; Preferably, the temperature of dialysis is 20-30°C, and the time is 2-4 days.

7. The preparation method according to any one of claims 1-6, characterized in that, The polysaccharide in step (4) includes any one or a combination of at least two of sodium alginate, chitosan or cyclodextrin; Preferably, the polysaccharide is cyclodextrin; Preferably, the mass ratio of the coffee grounds extract, polysaccharide and chloromalonic acid is (5-10):(1-2):(2-3); Preferably, the concentration of the aqueous sodium hydroxide solution is 10-20%; Preferably, the material-liquid ratio of the coffee grounds extract to the aqueous sodium hydroxide solution is 0.05-0.2 g / mL; Preferably, the temperature of mixing in step (4) is 85-95°C, and the time is 1.5-3 h.

8. The preparation method according to any one of claims 1-7, characterized in that, The specific steps of the low-temperature plasma treatment in step (4) are: Add the mixture to a phosphate buffer solution, and then perform low-temperature plasma treatment under half magnetic force; Preferably, the phosphate solution is a PBS solution, with a concentration of 0.05-0.2 mol / L and a pH of 7-8; Preferably, the material liquid ratio of the mixture to phosphate is 0.01 - 0.05 g / mL; Preferably, during the low-temperature plasma treatment, the voltage is 50 - 90 V, the current is 0.5 - 2 A, the distance between the two electrodes is 5 - 7 mm, and the discharge time is 80 - 100 s.

9. A flavor-carrying particle with the characteristic of coffee aroma, characterized in that, The fragrance-carrying particles with coffee aroma characteristics are prepared by the preparation method according to any one of claims 1 - 8.

10. Use of the fragrance-carrying particles with coffee aroma characteristics according to claim 9 in a cigarette filter.

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