Cardbean dry distillation spice as well as preparation method and application thereof

Abstract

The invention relates to carob dry distillation spice as well as a preparation method and application thereof, and belongs to the technical field of tobacco spices. The preparation method comprises the following steps: mixing carob beans fermented by pichia pastoris with a dry distillation auxiliary agent, and sequentially carrying out dry distillation and condensation; the dry distillation temperature is 200 to 400 DEG C; the dry distillation time is 20 to 50 minutes. The invention provides the preparation method of the dry distillation spice suitable for the carob beans by taking the carob beans as a raw material and optimizing the steps of dry distillation temperature, time, heating rate and the like. Compared with the prior art, the preparation method of the carob dry distillation spice is simple, easy to operate, relatively low in cost, easy for industrial production and very high in practicability. In addition, the method has a certain promotion effect on meeting social requirements, reducing the production cost of spices, researching the effect of dry distillation spices on tobacco products and the like, and also lays a foundation for further development and application of the carob beans.

Description

TECHNICAL FIELD

[0001] The present application relates to a carob dry distillation flavor and a preparation method and application thereof, and belongs to the technical field of tobacco flavor. BACKGROUND

[0002] The tobacco industry will take a new step in reducing tar and harm in the future, and the tar control and reduction level will continue to improve. The tar content and harm index of domestic cigarettes are steadily decreasing, and the tar content is synchronized with developed countries in Europe and the United States. The formation of main harmful components has a comparative advantage with internationally renowned brands. However, low-tar cigarettes increase the dry feeling and lack of aroma, which affects the quality of cigarettes and the sensory experience of consumers to some extent. Developing new tobacco flavor is an effective method to solve this problem.

[0003] Tobacco flavor technology is one of the core technologies in cigarette manufacturing. It can modify the defects in tobacco leaf or leaf formula, improve the toughness and combustibility of tobacco, reduce the irritation of smoke, and improve the ability of tobacco to resist corrosion. Through flavoring, the aroma characteristics of the product can be improved to cover the odor and highlight the aroma, enrich and correct the aroma of cigarettes, and keep the aroma of cigarettes stable. In addition, the use of flavor substances can also have a shielding effect on certain odors, which can mask, dilute and neutralize the odor in cigarettes. On the other hand, it can give cigarettes different aroma styles to meet the needs of different consumers on the basis of added flavor and tobacco aroma.

[0004] Traditional tobacco flavor is generally extracted from natural plants by alcohol extraction, water extraction or molecular distillation. Dry distillation is a reaction process in which flavor raw materials are heated and decomposed in the absence of air, which can produce characteristic flavors of incense and baking aroma. At present, there are few reports on the development of dry distillation tobacco flavor raw materials in the tobacco industry, and the development of characteristic tobacco flavor using dry distillation reaction has broad prospects.

[0005] Carob is usually derived from the Mediterranean carob tree (Ceratonia siliqua), which is a plant of the Fabaceae family and originated in the Mediterranean region. Its pod shape is similar to that of a broad bean, containing sweet flesh and hard seeds. The pods of this tree (carob pods) can be used to extract carob gum, make carob powder and carob extract. As a natural plant, its unique aroma components have potential application value. Carob extract can be used as a food flavor, a natural food thickening agent and a stabilizer, and its use in tobacco products can improve and enhance the quality of cigarettes. However, there is no related research report on the preparation of characteristic baking aroma and incense aroma flavor using carob. SUMMARY

[0006] The first object of the present application is to provide a preparation method of a dry distillation flavor of carob beans, and to provide a preparation method of a dry distillation flavor of carob beans with a characteristic baking aroma and incense aroma style.

[0007] The second object of the present application is to provide a dry distillation flavor of carob beans to solve the problem that no characteristic baking aroma and incense aroma style flavor is prepared from carob beans in the prior art.

[0008] The third object of the present application is to provide the application of the dry distillation flavor of carob beans in tobacco product flavoring and perfuming, and to provide the application of the dry distillation flavor of carob beans in improving the quality of tobacco products.

[0009] In order to achieve the above objects, the technical scheme adopted by the preparation method of a dry distillation flavor of carob beans in the present application is as follows:

[0010] The preparation method of a dry distillation flavor of carob beans comprises mixing carob beans after fermentation by Pichia pastoris with a dry distillation aid, and sequentially performing dry distillation and condensation; the temperature of the dry distillation is 200-400℃; and the time of the dry distillation is 20-50min.

[0011] The above scheme has the beneficial effect that the preparation method of a dry distillation flavor of carob beans in the present application is an opening invention. The present application uses carob beans as raw materials, and provides a preparation method of a dry distillation flavor suitable for carob beans by optimizing the temperature, time and heating rate of dry distillation. Compared with the prior art, the preparation method of a dry distillation flavor of carob beans selected by the present application is simple, easy to operate, low in cost, easy to industrialize, and has strong practicability.

[0012] Preferably, the Pichia pastoris is preserved in the China Industrial Microbial Culture Collection Center (CICC) with a preservation number of CICC 1958.

[0013] Further, the fermentation broth of Pichia pastoris contains various enzymes, including amylase, lipase and protease, which can decompose the cell wall of carob beans and degrade starch, fat and protein therein. The fermentation treatment of carob beans by Pichia pastoris can promote cell rupture, help the release of flavor components, and significantly improve the quality of the dry distillation flavor of carob beans.

[0014] As a further improvement, the addition amount of the dry distillation aid is 0.5-4.5% of the mass of the carob beans; and the dry distillation aid is an ethanol-water solution with a volume fraction of 40-50%.

[0015] The above scheme has the beneficial effect that the present application uses an ethanol-water solution as a dry distillation aid in the dry distillation process, which facilitates the distillation of flavor components in the carob beans during the dry distillation heating process, and improves the yield of the dry distillation flavor.

[0016] As a further improvement, the temperature of the dry distillation is 300-350 DEG C; the time of the dry distillation is 30-35 min; and the temperature increasing rate of the dry distillation is 30-45 DEG C / min.

[0017] As a further improvement, the temperature of the dry distillation is 300-350 DEG C; the time of the dry distillation is 30-35 min; and the temperature increasing rate of the dry distillation is 30-45 DEG C / min.

[0018] As a further improvement, the carob beans after fermentation of the Pichia pastoris are prepared by the following method: the fermentation supernatant of the Pichia pastoris is sprayed on the surface of the carob beans, and the fermentation is carried out at 25-40 DEG C for 1-4 days.

[0019] As a further improvement, the Pichia pastoris is inoculated in a wort liquid medium, and the fermentation is carried out at 25-30 DEG C for 2-5 days, and the fermentation supernatant is obtained by centrifugation; and the fermentation supernatant is 5-10% of the mass of the carob beans.

[0020] As a further improvement, the condensed product is mixed with 10-12 times of weight of anhydrous ethanol to obtain the carob bean dry distillation flavor.

[0021] In order to achieve the above-mentioned purpose, the technical scheme adopted by the carob bean dry distillation flavor in the present application is:

[0022] The carob bean dry distillation flavor prepared by the preparation method of the carob bean dry distillation flavor.

[0023] The beneficial effects of the above-mentioned scheme are that the carob bean dry distillation flavor prepared by the present application has rich aroma and large amount of aroma, and has typical incense and baking aroma in addition to the original aroma characteristics of carob beans, which enriches the aroma characteristics of carob bean flavor, and promotes the further use of carob bean flavor.

[0024] Further, the present application has certain promoting effect on meeting social needs, reducing the production cost of flavor, researching the effect of dry distillation flavor on tobacco products, and laying a foundation for the further development and application of carob beans.

[0025] In order to achieve the above-mentioned purpose, the technical scheme adopted by the carob bean dry distillation flavor in the present application is:

[0026] The carob bean dry distillation flavor in the present application is used in the flavoring and perfuming of tobacco products

[0027] The beneficial effects of the above-mentioned scheme are that the carob bean dry distillation flavor prepared by the present application can be applied in cigarettes, heated cigarettes, low-grade flue-cured tobacco leaves and cigar tobacco leaves, the applicable range of raw materials is wide, and it is suitable for large-scale production. The carob bean dry distillation flavor can be applied in the quality improvement of tobacco products, and lays a foundation for the next industrialized development.

[0028] As a further improvement, the tobacco product is a cigarette, a heated cigarette. BRIEF DESCRIPTION OF DRAWINGS

[0029] Figure 1 Figure is a colony morphology chart of Pichia pastoris in the present application;

[0030] Figure 2 Figure is a chart of the carob dry distillation flavor prepared in the present application;

[0031] Figure 3 Figure is a chart of the flavor note profile of the carob dry distillation flavor in Example 1 of the present application;

[0032] Figure 4 Figure is a chart of the flavor note profile of the carob dry distillation flavor in Example 2 of the present application;

[0033] Figure 5 Figure is a chart of the flavor note profile of the carob dry distillation flavor in Example 3 of the present application;

[0034] Figure 6 Figure is a chart of the flavor note profile of the carob dry distillation flavor in Example 4 of the present application;

[0035] Figure 7 Figure is a chart of the flavor note profile of the carob dry distillation flavor in Example 5 of the present application;

[0036] Figure 8 Figure is a chart of the flavor note profile of the carob dry distillation flavor in Example 7 of the present application. DETAILED DESCRIPTION

[0037] Reducing harm is the trend and demand of the development of tobacco industry, however, low-tar cigarettes bring about an increase in dryness and a lack of aroma, which affects the quality of cigarettes and the sensory experience of consumers, and cigarette flavoring can solve the problem of insufficient sensory experience of consumers caused by low-tar cigarettes to a certain extent. Carob is a kind of natural plant, and its unique aroma components have potential application value, and carob extract can improve and enhance the quality of tobacco products. However, there is no relevant research report on the preparation of characteristic baking and incense style flavor from carob.

[0038] Based on this, the present application provides a preparation method of carob dry distillation flavor, first, Pichia pastoris is used to ferment carob, and then the fermented carob is subjected to dry distillation in the presence of a dry distillation aid at 200-400℃ for 20-50min, and then condensed, to prepare carob dry distillation flavor with characteristic baking and incense style.

[0039] As a further improvement, the pyrolysis auxiliary agent is added in an amount of 0.5-4.5% of the mass of the carob beans; and the pyrolysis auxiliary agent is an ethanol-water solution with a volume fraction of 40-50%.

[0040] Preferably, the pyrolysis auxiliary agent is added in an amount of 4.5% of the mass of the carob beans; and the pyrolysis auxiliary agent is an ethanol-water solution with a volume fraction of 50%.

[0041] As a further improvement, the temperature of the pyrolysis is 300-350℃; the time of the pyrolysis is 30-35 min; and the heating rate of the pyrolysis is 30-45℃ / min.

[0042] As a further improvement, the temperature of the pyrolysis is 300-350℃; the time of the pyrolysis is 30-35 min; and the heating rate of the pyrolysis is 30-45℃ / min.

[0043] Preferably, the temperature of the pyrolysis is 300℃; the time of the pyrolysis is 30 min; and the heating rate of the pyrolysis is 30℃ / min.

[0044] As a further improvement, the carob beans after fermentation by the Pichia pastoris are prepared by the following method: the fermentation supernatant of the Pichia pastoris is sprayed on the surface of the carob beans, and the fermentation is carried out at 25-40℃ for 1-4 days.

[0045] Preferably, the fermentation is carried out at a temperature of 25℃ for 2 days.

[0046] As a further improvement, the fermentation supernatant is 5-10% of the mass of the carob beans.

[0047] The present application is further described in detail below with reference to specific examples. Unless otherwise specified, the equipment and reagents used in the examples, experimental examples and comparative examples are commercially available.

[0048] The Pichia pastoris used in the present application is commercially available, and the strain is preserved in the China Industrial Microbial Culture Collection Center (CICC) with a preservation number of CICC 1958, and the colony morphology thereof is shown in Figure 1

[0049] The preparation method of the fermentation supernatant of the Pichia pastoris in the following examples of the present application is as follows:

[0050] The Pichia pastoris is inoculated in the wort liquid medium at an inoculation amount of 5% (v / v), and is cultured at 25℃ with 200 rpm oscillation for 48 h, so that the final viable cell count reaches about 5×10 8 CFU / mL, and then the fermentation supernatant is harvested by centrifugation at 4℃ and 8000 rpm for 10 min.

[0051] ​Specific embodiments of the present invention regarding the dry distillation of carob spices and its preparation method:

[0052] This invention involves spraying the supernatant from Pichia pastoris fermentation onto the surface of carob powder at 5-10% of the powder's weight, fermenting at 25-40°C for 1-4 days, drying, then spraying a 40-50% ethanol-water solution at 0.5-5% of the carob powder's weight, followed by dry distillation at 200-400°C for 20-50 minutes. The distillation product is then collected, weighed, and dissolved in 10 times its weight of anhydrous ethanol to obtain the carob dry distillation flavoring. Figure 2 The specific implementation steps are as follows:

[0053] Example 1: Optimization of carob fermentation temperature

[0054] This embodiment optimizes the fermentation temperature of carob, and the specific implementation steps are as follows:

[0055] The supernatant from the fermentation of Pichia pastoris was sprayed onto the surface of carob powder at a mass ratio of 5.0%. Fermentation temperatures were set at 25℃, 30℃, 35℃, and 40℃, and fermentation was carried out for 3 days. After drying, a 50% ethanol-water solution (4.5% carob mass by volume) was sprayed on the carob powder. The carob powder fermented under different temperature conditions was placed in a high-temperature resistant glass tube and subjected to a dry distillation reaction in a low-temperature distillation apparatus. The dry distillation temperature was set at 300℃, the heating rate was 30℃ / min, and the reaction was carried out for 30 min. The mixture was then condensed in a water bath, and the dry distillation product was collected. Ethanol was added at a mass ratio of 1:10, and the mixture was filtered to obtain carob dry distillation flavoring.

[0056] Carob dry distillation flavoring was injected into Sichuan Tobacco's No. 0 blank cigarettes, 3 μL per cigarette. Sensory evaluation was conducted according to GB5606.4-2005 "Sensory Evaluation Method for Tobacco and Tobacco Products" and YC / T 497-2014 "Sensory Evaluation Method for Chinese-style Cigarette Style". The evaluation focused on aroma indicators such as fruity, woody, sour, roasted, smoky, and nutty notes, as well as sensory quality indicators such as aroma, harmony, and off-flavors. Sensory evaluation aroma radar charts were plotted (as shown in Tables 1 and 2). Figure 3 (As shown).

[0057] Table 1. Summary of Sensory Evaluation Scores for Carob Flavorings at Different Fermentation Temperatures (points)

[0058]

[0059] The results showed that a fermentation temperature of 35℃ yielded the best results, with a pronounced fruity aroma, a prominent sour aroma, hints of wood and smokiness, enhanced sweetness, rich smoke, significantly reduced acridity, and a pleasant aftertaste. While fermentation temperatures of 25℃ and 30℃ also exhibited noticeable sour and fruity aromas, the aroma intensity and sweetness were less pronounced than at 35℃, and there was a slight acridity. At fermentation temperatures above 35℃, although the aroma intensity remained sufficient, some off-flavors appeared, and the aftertaste became unpleasant. Therefore, the optimal fermentation temperature was 35℃.

[0060] Table 2. Summary of sensory quality scores of cigarettes with carob dry distillation flavoring added at different fermentation temperatures (points)

[0061]

[0062] Subsequent GC-MS analysis of aroma components showed that after fermentation, the contents of carob dry distillation flavorings such as 5-methylfuranaldehyde, furfuryl alcohol, methylcyclopentenolone, 2,3-dimethyl-2-cyclopentenone, and 4-hydroxy-2,5-dimethyl-3(2H)furanone increased, enhancing the sweet, caramel, nutty, and roasted aromas. After fermentation, the contents of carob dry distillation flavorings such as 2,4-dimethylphenol, 2,6-dimethoxyphenol, and guaiacol also increased, enhancing the woody and smoky aromas.

[0063] Example 2: Optimization of carob fermentation time

[0064] This embodiment optimizes the fermentation time of carob, and the specific implementation steps are as follows:

[0065] The supernatant from the fermentation of Pichia pastoris was sprayed onto the surface of carob powder at a mass ratio of 5.0%. The fermentation temperature was set at 35℃, and the fermentation time was set at 1 day, 2 days, 3 days, and 4 days. After drying, a 50% ethanol-water solution with a volume fraction of 4.5% carob mass was sprayed on the carob powder. Carob powder with different fermentation times was placed in a high-temperature resistant glass tube and subjected to a dry distillation reaction in a low-temperature distillation apparatus. The dry distillation temperature was set at 300℃, the heating rate was 30℃ / min, and the reaction was carried out for 30 min. The mixture was then condensed in a water bath, and the dry distillation product was collected. Ethanol was added at a mass ratio of 1:10, and the mixture was filtered to obtain carob dry distillation flavoring.

[0066] Carob dry distillation flavoring was injected into Sichuan Tobacco's No. 0 blank cigarettes, 3 μL per cigarette. Sensory evaluation was conducted according to "GB5606.4-2005 Sensory Evaluation Method for Tobacco and Tobacco Products" and "YC / T 497-2014 Sensory Evaluation Method for Chinese Style Cigarettes". The evaluation focused on aroma indicators such as fruity, woody, sour, roasted, smoky, and nutty aromas, as well as sensory quality indicators such as aroma, harmony, and off-flavors. Sensory evaluation aroma radar charts were plotted (as shown in Tables 3 and 4). Figure 4 (As shown).

[0067] Table 3. Summary of Sensory Evaluation Scores for Carob Distillation Spices at Different Fermentation Times (points)

[0068]

[0069] The results showed that a fermentation time of 3 days yielded the best results, with a prominent sour aroma, distinct fruity notes, woody and smoky notes, enhanced sweetness, rich smoke, significantly reduced astringency, and a pleasant aftertaste. While fermentation temperatures of 1 day and 2 days provided acceptable sour and fruity aromas, they also had a slightly astringent taste, and the sweetness was not as pronounced as at 3 days. At 4 days, although the overall aroma quality was acceptable, there were slight off-odors, and the aftertaste was slightly unpleasant. Therefore, a fermentation time of 3 days is the optimal fermentation time for carob powder.

[0070] Table 4. Summary of sensory quality scores for cigarettes with carob dry distillation flavoring added at different fermentation times (points)

[0071]

[0072] Example 3 Optimization of distillation temperature

[0073] This embodiment optimizes the temperature of the dry distillation, and the specific implementation is as follows:

[0074] The supernatant from the fermentation of Pichia pastoris was sprayed onto the surface of carob powder at a mass ratio of 5.0%. The fermentation temperature was set at 35℃, and the fermentation time was set at 3 days. After drying, a 50% ethanol-water solution (4.5% carob mass by volume) was sprayed on the carob powder. The carob powder was then placed in a high-temperature resistant glass tube and subjected to a low-temperature dry distillation apparatus. The dry distillation temperatures were set at 200℃, 250℃, 300℃, 350℃, and 400℃, with a heating rate of 30℃ / min for 30 min. The mixture was then condensed in a water bath, and the dry distillation product was collected. Ethanol was added at a mass ratio of 1:10, and the mixture was filtered to obtain carob dry distillation flavoring.

[0075] Carob dry distillation flavoring was injected into Sichuan Tobacco's No. 0 blank cigarettes, 3 μL per cigarette. Sensory evaluation was conducted according to "GB5606.4-2005 Sensory Evaluation Method for Tobacco and Tobacco Products" and "YC / T 497-2014 Sensory Evaluation Method for Chinese-style Cigarette Style". The evaluation focused on aroma indicators such as fruity, woody, sour, roasted, smoky, and nutty aromas, as well as sensory quality indicators such as aroma, harmony, and off-flavors. Sensory evaluation aroma radar charts were plotted (as shown in Tables 5 and 6). Figure 5 (As shown).

[0076] Table 5. Summary of Sensory Evaluation Scores for Carob Spices Distilled at Different Distillation Temperatures (points)

[0077]

[0078] The results showed that carob dry distillation yielded the best aroma richness at 300℃, with the highest scores for sweet and fruity aromas, and also noticeable fresh and floral aromas, significantly reduced irritation, and the best sensory evaluation. At 200℃ and 250℃, the aroma was insufficient, and the roasted and smoky aromas were not prominent. At 350℃ and 400℃, the dry distillation reaction was excessive, resulting in an overly strong smoky aroma with some woody off-flavors. Therefore, the preferred dry distillation temperature is 300℃.

[0079] Table 6. Summary of sensory quality scores (points) of cigarettes with carob distillation flavoring added at different distillation temperatures.

[0080]

[0081] Example 4 Optimization of distillation time

[0082] This embodiment optimizes the distillation time, and the specific implementation is as follows:

[0083] The supernatant from the fermentation of Pichia pastoris was sprayed onto the surface of carob powder at a mass ratio of 5.0%. The fermentation temperature was set at 35℃, and the fermentation time was set at 3 days. After drying, a 50% ethanol-water solution (4.5% carob mass by volume) was sprayed on the carob powder. The carob powder was then placed in a high-temperature resistant glass tube and subjected to a low-temperature dry distillation apparatus. The dry distillation temperature was set at 300℃, the heating rate at 30℃ / min, and the dry distillation reaction time was 20 min, 30 min, 40 min, and 50 min. The mixture was condensed in a water bath, and the dry distillation product was collected. Ethanol was added at a mass ratio of 1:10, and the mixture was filtered to obtain carob dry distilled flavoring.

[0084] Carob dry distillation flavoring was injected into Sichuan Tobacco's No. 0 blank cigarettes, 3 μL per cigarette. Sensory evaluation was conducted according to "GB5606.4-2005 Sensory Evaluation Method for Tobacco and Tobacco Products" and "YC / T 497-2014 Sensory Evaluation Method for Chinese-style Cigarette Style". The evaluation focused on aroma indicators such as fruity, woody, sour, roasted, smoky, and nutty aromas, as well as sensory quality indicators such as aroma, harmony, and off-flavors. Sensory evaluation aroma radar charts were plotted (as shown in Tables 7 and 8). Figure 6 (As shown).

[0085] Table 7. Summary of Sensory Evaluation Scores for Carob Distillation Spices at Different Distillation Times (points)

[0086]

[0087] The results showed that the carob dry distillation produced the best aroma richness at a time of 30 min, with the highest scores for sweet and fruity aromas, and also noticeable fresh and floral aromas, while significantly reducing the irritation. Therefore, the optimal dry distillation time is 30 min.

[0088] Table 8. Summary of sensory quality scores (points) for cigarettes with carob distillation flavoring added at different distillation times.

[0089]

[0090] Example 5: Optimization of Heating Rate

[0091] This embodiment optimizes the heating rate, and the specific implementation steps are as follows:

[0092] The supernatant from the fermentation of Pichia pastoris was sprayed onto the surface of carob powder at a mass ratio of 5.0%. The fermentation temperature was set at 35℃, and the fermentation time was set at 3 days. After drying, a 50% ethanol-water solution (4.5% carob mass by volume) was sprayed on the carob powder. The carob powder was then placed in a high-temperature resistant glass tube and subjected to a low-temperature dry distillation apparatus. The dry distillation temperature was set at 300℃, and the heating rate was set at 20℃ / min, 25℃ / min, 30℃ / min, 35℃ / min, and 40℃ / min. The dry distillation time was 30 min. The mixture was condensed in a water bath, and the dry distillation product was collected. Ethanol was added at a mass ratio of 1:10, and the mixture was filtered to obtain carob dry distilled flavoring.

[0093] Carob dry distillation flavoring was injected into Sichuan Tobacco's No. 0 blank cigarettes, 3 μL per cigarette. Sensory evaluation was conducted according to "GB5606.4-2005 Sensory Evaluation Method for Tobacco and Tobacco Products" and "YC / T 497-2014 Sensory Evaluation Method for Chinese-style Cigarette Style". The evaluation focused on aroma indicators such as fruity, woody, sour, roasted, smoky, and nutty aromas, as well as sensory quality indicators such as aroma, harmony, and off-flavors. Sensory evaluation aroma radar charts were plotted (as shown in Tables 9 and 10). Figure 7 (As shown).

[0094] Table 9. Summary of Sensory Evaluation Scores for Carob Distillation Spices at Different Heating Rates (points)

[0095]

[0096] The results showed that the carob dry distillation process prepared at 30℃ / min produced the richest aroma, with the highest scores for sweet and fruity notes, a noticeable spicy note, and also prominent fresh and floral notes, resulting in good smoke comfort. Therefore, a dry distillation heating rate of 30℃ / min is preferred.

[0097] Table 10 Summary of Sensory Quality Scores of Cigarettes with Different Heating Rates for Carob Distillation Flavoring (points)

[0098]

[0099] Example 6: GC-MS Analysis of Carob Dry Distillation Flavoring

[0100] This embodiment analyzes the aroma components of the carob dry distillation flavoring prepared in Example 5 at a heating rate of 30℃ / min. The specific implementation steps are as follows:

[0101] 0.1 mL of carob pyrolysis flavoring was added to 0.8 mL of dichloromethane and 0.1 mL of phenethyl acetate internal standard solution (0.8411 mg / mL). The mixture was then filtered through an organic microporous membrane and analyzed by GC-MS.

[0102] GC conditions: Agilent 7890B-5977 (30m × 250μm id × 0.25μm df) column; injection port temperature 250℃; carrier gas He; column flow rate 1mL / min; temperature program: initial temperature 50℃, hold for 4min, increase to 250℃ at 2℃ / min, hold for 6min; injection volume 1μL; split ratio 5:1.

[0103] MS conditions: Electron impact source (EI) in ionization mode; transfer line temperature 280°C; ion source temperature 230°C; quadrupole temperature 150°C; ionization energy 70 eV; solvent delay 4 min; scan mode MRM.

[0104] The results are shown in Table 11. The results indicate that the fermented carob dry distillation flavoring contained relatively high levels of 5-methylfuranaldehyde, 2-methylbutyric acid, methylcyclopentenolone, 2,3-dimethyl-2-cyclopentenolone, 2,4-dimethylphenol, guaiacol, β-guaiacolene, and camphor. Among these, the content of camphor and β-guaiacolene increased after fermentation, enhancing the aroma, floral, and herbal notes. The content of 2-methylbutyric acid and 1-acetoxy-2-butanone also increased after fermentation, enhancing the sour and fruity aromas, enriching the tobacco aroma, softening the smoke, and reducing the irritation of cigarettes. After fermentation, the content of carob dry distillation flavorings such as 5-methylfuranaldehyde, furfuryl alcohol, methylcyclopentenolone, 2,3-dimethyl-2-cyclopentenone, and 4-hydroxy-2,5-dimethyl-3(2H)furanone increases, enhancing the sweet, caramel, nutty, and roasted aromas. 2,4-Dimethylphenol, 2,6-dimethoxyphenol, and guaiacol can increase the woody and smoky aromas.

[0105] Table 11. Main GC-MS aroma components of carob dry distillation flavoring

[0106]

[0107] Note: The difference between the fermented sample and the carob spice prepared by heating at a rate of 30℃ / min in Example 5 is that the fermentation process of Pichia pastoris was not carried out before the dry distillation.

[0108] II. Specific embodiments of the application of the dry distillation carob flavoring of the present invention in flavoring and flavoring tobacco products:

[0109] Example 7: Application of carob dry distillation flavoring in cigarettes

[0110] The carob dry distillation flavoring prepared in Example 5 at a heating rate of 30℃ / min was injected into Sichuan Tobacco's No. 0 blank cigarettes, 3 μL per cigarette. Sensory evaluation was conducted according to GB5606.4-2005 "Sensory Evaluation Methods for Tobacco and Tobacco Products", and a sensory evaluation aroma radar chart was plotted based on the aroma (e.g., ...). Figure 8 (As shown).

[0111] The results showed that carob dry distillation flavoring significantly increased the amount and richness of aroma, significantly enhanced fruity and sweet aromas, and also noticeably improved the fresh and floral aromas, similar to the overall aroma of carob. Furthermore, it softened the smoke, increased sweetness, and reduced irritation.

[0112] Example 8: Application of carob dry distillation flavoring in heated cigarettes

[0113] The carob dry distillation flavoring prepared in Example 5 at a heating rate of 30℃ / min was injected into blank heated cigarettes, 3 μL per cigarette. Using the blank heated cigarettes as a control, sensory evaluation was conducted by evaluators according to GB5606.4-2005 "Sensory Evaluation Methods for Tobacco and Tobacco Products". The evaluation results are shown in Table 12. Compared with the blank sample, it improved the cigarette aroma, enhanced harmony, reduced irritation, masked off-flavors, and provided a more comfortable and clean aftertaste. Furthermore, the natural tobacco aroma and the unique, refreshing aroma of carob were more pronounced in the heated cigarette.

[0114] Table 12 Sensory quality ratings of heated cigarettes before and after flavoring

[0115]

[0116] Example 9: Application of carob dry distillation flavoring in enhancing the aroma of low-grade tobacco leaves in Liangshan.

[0117] The carob dry distillation flavoring prepared in Example 5 at a heating rate of 30℃ / min was diluted 10 times with 10% ethanol and sprayed onto unsuitable tobacco leaves from Liangshan (variety K326, grade C4F, 2021) at 1% of the tobacco leaf tissue weight. The tobacco leaves were then equilibrated in a sealed environment at 22℃ and 60% humidity for 8 hours. The unprocessed and flavored tobacco leaves were shredded and rolled into cigarettes for sensory evaluation. The unprocessed Liangshan unsuitable tobacco leaves had a decent aroma, but lacked sweetness, exhibited a noticeable earthy and local off-flavor, and had a woody and pungent taste. After flavoring, the sweet and caramel-sweet aroma was enhanced, the sweetness was significantly improved, a certain fruity aroma was highlighted, the pungent taste was significantly reduced, the off-flavor was lessened, and the usability was increased.

[0118] Unsuitable Liangshan tobacco leaves, both before and after flavoring, were shredded and extracted with 50% ethanol to obtain an ethanol extract. 10 mL of the ethanol extract was extracted twice with 8 mL of dichloromethane solution, the extracts were combined, and the solution was removed with anhydrous sodium sulfate before being concentrated to 1.0 mL. After adding an internal standard, qualitative and quantitative analysis was performed by GC-MS under the same conditions as in Example 6. The results are shown in Table 13. The table shows that after flavoring, the levels of sweet aroma compounds in Liangshan tobacco leaves, such as furfural, methyl maltol, 5-methylfurfural, 2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-one, and 4-hydroxy-2,5-dimethyl-3(2H)-furanone, significantly increased. These compounds impart a sweet aroma to the smoke, such as roasted, fresh, or caramelized, reducing smoke irritation and improving taste. Simultaneously, the levels of acidic components, such as acetic acid, 2-methylbutyric acid, and benzoic acid, also increased, enhancing fruity aroma, enriching the aroma, and reducing smoke irritation. Guaiacin can increase the richness and fullness of the aroma in cigarettes.

[0119] Table 13 Changes in the content of main aroma components in non-applicable tobacco leaves from Liangshan before and after flavoring.

[0120]

[0121]

[0122] Example 10: Application of carob dry distillation flavoring in cigar tobacco leaves

[0123] The carob dry distillation flavoring prepared in Example 5 at a heating rate of 30℃ / min was diluted 10 times with 10% ethanol and sprayed onto the surface of the filler tobacco leaves (Chuxue 14, upper middle, 2022) at 1% of the tobacco leaf tissue weight. The tobacco leaves were fermented in a sealed container at 32℃ and 70% humidity for 96 hours. After the fermented cigar tobacco leaves were balanced for moisture, they were rolled into cigars with a ring gauge of 44 (approximately 1.0 cm in diameter), and cigars of uniform weight (1.9 ± 0.1 g) were selected for sensory evaluation.

[0124] The results showed that the aroma of Chu Xue 14 domestic cigar tobacco was acceptable, but the strength and irritation were relatively high, with some woody off-flavors. After fermentation and flavoring treatment, the sweetness of the cigar was significantly improved, the roasted and caramelized aromas were enhanced, the floral and fruity aromas were significantly improved, the aroma richness was increased, the irritation was significantly reduced, the off-flavors were reduced, and the usability was increased.

[0125] In summary, this invention provides a carob dry distillation flavoring, its preparation method, and its application. It establishes a carob fermentation and dry distillation reaction flavoring preparation process, which can promote the satisfaction of social needs, reduce production costs, and increase the market value of carob. It also lays the foundation for the further development and application of carob.

[0126] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing a carob pyrolysis flavoring, characterized in that: The process includes the following steps: mixing carob fermented with Pichia pastoris with a dry distillation aid, and then performing dry distillation and condensation in sequence; the dry distillation temperature is 200~400℃; and the dry distillation time is 20~50min.

2. The method for preparing carob dry distillation flavoring according to claim 1, characterized in that: The amount of the pyrolysis aid added is 0.5-4.5% of the carob mass; the pyrolysis aid is an ethanol-water solution with a volume fraction of 40-50%.

3. The method for preparing carob dry distillation flavoring according to claim 1, characterized in that: The heating rate of the dry distillation is 20~40℃ / min.

4. The method for preparing carob dry distillation flavoring according to claim 3, characterized in that: The distillation temperature is 300~350℃; the distillation time is 30~35min; and the distillation heating rate is 30~45℃ / min.

5. The method for preparing carob dry distillation flavoring according to any one of claims 1 to 4, characterized in that: The carob fermented with Pichia pastoris was prepared by the following method: the fermentation supernatant of Pichia pastoris was sprayed onto the surface of the carob and fermented at 25-40°C for 1-4 days.

6. The method for preparing carob dry distillation flavoring according to claim 5, characterized in that: Pichia pastoris was inoculated into malt extract liquid culture medium and cultured at 25-30°C for 2-5 days. The fermentation supernatant was obtained by centrifugation. The fermentation supernatant was 5-10% of the carob weight.

7. The method for preparing carob dry distillation flavoring according to claim 6, characterized in that: The condensed product is mixed with 10 to 12 times its weight of anhydrous ethanol to obtain carob dry distillation flavoring.

8. A carob pyrolysis flavoring prepared by the method of any one of claims 1 to 7.

9. The application of the carob dry distillation flavoring as described in claim 8 in the flavoring and flavoring of tobacco products.

10. The application of the carob dry distillation flavoring according to claim 9 in flavoring and flavoring tobacco products, characterized in that: The tobacco products mentioned are cigarettes and heated cigarettes.

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