Cocoa extract tobacco flavor and application thereof

Abstract

The invention relates to a cocoa extract tobacco flavor and application thereof. The cocoa extract tobacco flavor comprises a first cocoa extract and a second cocoa extract, the method comprises the following steps: mixing a cocoa powder raw material with an alcohol solvent, carrying out alcohol extraction treatment, carrying out solid-liquid separation on an alcohol extraction product, taking clear liquid, standing the clear liquid at low temperature, and degreasing to obtain a first cocoa extract; mixing the cocoa powder raw material with water, carrying out water extraction treatment, carrying out solid-liquid separation on a water extraction product, taking clear liquid, standing the clear liquid at low temperature, degreasing, loading a degreased product to a macroporous resin chromatographic column, eluting and purifying, and collecting eluant, so as to obtain a second cocoa extract. The cocoa extracts prepared by two specific preparation processes are creatively combined to serve as the tobacco flavor, the cocoa extracts and the tobacco flavor have a synergistic effect, and the flavor is added into tobacco products, so that the fragrance and richness of the tobacco products can be remarkably improved, the sensory comfort characteristic of smoke can be remarkably improved, and the tobacco flavor has a good taste. And the sensory quality of the tobacco product is comprehensively improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of tobacco flavors and fragrances, and relates to a cocoa extract tobacco flavor and application thereof, and in particular to a cocoa extract tobacco flavor with improved comprehensive sensory quality and application thereof. Background Art

[0002] Cocoa extract is one of the natural flavors used in the tobacco industry. Adding it to cigarettes can give the smoke a cocoa aroma, increase the roasted aroma, sweet aroma, and bean aroma, and play a role in enhancing the aroma of the smoke, suppressing irritation and removing impurities. Therefore, some manufacturers use cocoa products in tobacco products, thereby giving tobacco products characteristic cocoa aromas such as roasted aroma, nutty aroma and sweet aroma.

[0003] For example, CN118077949A discloses a method for preparing tobacco particles with cocoa aroma characteristics, as well as its products and applications. The preparation method comprises: subjecting cocoa powder to supercritical extraction to obtain a cocoa extract, and collecting the waste residue after extraction; mixing an adhesive, a moisture-proof agent, and a preservative in deionized water to obtain a mixed solution; adding the cocoa extract, the waste residue, and dry ice particles to the mixed solution, and mixing to obtain a mixed material; granulating the mixed material, and drying it to obtain the tobacco particles with cocoa aroma characteristics. This method can maximize the extraction of flavor components in the cocoa powder and enhance the cocoa aroma characteristics of the smoke.

[0004] For example, CN109439438A discloses a cocoa flavor essence for tobacco dropping pills, its preparation method, and its application. The cocoa flavor essence is composed of 94.0-97.5% cocoa extract, 0.5-1.0% cocoa aldehyde, and 2.0-5.0% ethyl laurate. The cocoa extract is prepared by adding 8-10 times the weight of caprylic decanoate glyceride to cocoa powder, refluxing the extract in an oil bath at 120-150°C for 2-2.5 hours, ultrasonically treating the extract for 30-60 minutes, centrifuging the extract, and filtering the supernatant with a 0.2-0.8 micron filter membrane. This cocoa flavor essence has good process adaptability, improves the production efficiency and yield of cocoa-flavored tobacco dropping pills, and reduces their production cost. It is also easy to use in cigarettes, enriching the aroma and imparting a distinctive flavor to cigarettes.

[0005] However, the preparation processes for cocoa flavorings for tobacco disclosed in the prior art are still very limited, and most of the resulting flavorings only have a flavoring effect and cannot effectively improve the sensory comfort of smoke, such as irritation, dryness, astringency, and odor. Therefore, it is very meaningful to develop a cocoa flavoring for tobacco that can comprehensively improve the sensory quality. Summary of the Invention

[0006] In view of the deficiencies in the prior art, the object of the present invention is to provide a cocoa extract tobacco flavoring and applications thereof, and in particular to provide a cocoa extract tobacco flavoring and applications thereof with improved comprehensive sensory quality.

[0007] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0008] In a first aspect, the present invention provides a cocoa extract tobacco flavoring, wherein the cocoa extract tobacco flavoring comprises a first cocoa extract and a second cocoa extract;

[0009] The first cocoa extract is prepared by a preparation method comprising the following steps:

[0010] The cocoa powder raw material is mixed with an alcohol solvent for alcohol extraction, the alcohol extraction product is separated into solid and liquid, and the supernatant is taken and the supernatant is allowed to stand at a low temperature and then defatted to obtain a first cocoa extract;

[0011] The second cocoa extract is prepared by a preparation method comprising the following steps:

[0012] The cocoa powder raw material is mixed with water for water extraction treatment, the water extraction product is separated into solid and liquid, the supernatant is taken, the supernatant is allowed to stand at low temperature and then defatted, the defatted product is loaded onto a macroporous resin chromatography column, eluted and purified, and the eluate is collected to obtain a second cocoa extract.

[0013] The present invention creatively combines cocoa extracts obtained by two specific preparation processes as tobacco flavorings. Flavoring substances such as aldehydes, ketones, esters, pyrazines, furanones, pyrones, pyrroles, and alkaloids in the first cocoa extract cooperate with flavor components such as polyphenols (epicatechin, catechin and its polymers, etc.), organic acids, theobromine, and heterocyclic compounds in the second cocoa extract, and the two synergize to enhance the effect. When added to tobacco products, the flavoring can not only significantly enhance the aroma and richness of the tobacco products, and enhance the characteristic aromas such as cocoa aroma, baking aroma, sweet aroma, and flue-cured tobacco aroma, but can also significantly improve the sensory comfort characteristics of the smoke, such as the delicate, soft, rounded, irritation, dryness, astringency, and miscellaneous smell, thereby comprehensively improving the sensory quality of the tobacco products. Compared with the first cocoa extract alone or the second cocoa extract alone, the flavoring is significantly superior in the above-mentioned effects.

[0014] Preferably, the cocoa powder raw materials are each independently selected from natural cocoa powder and / or alkalized cocoa powder.

[0015] Preferably, the alkalized cocoa powder comprises heavily alkalized cocoa powder and / or lightly alkalized cocoa powder.

[0016] Preferably, the cocoa powder raw materials are each independently selected from any one of high-fat cocoa powder, medium-fat cocoa powder or low-fat cocoa powder, or a combination of at least two thereof.

[0017] Preferably, the alcohol solvent is selected from any one of ethanol, propylene glycol or glycerol, or a combination of at least two thereof.

[0018] More preferably, the alcohol solvent is a combination of propylene glycol and ethanol.

[0019] The present invention also creatively discovered that using a mixed solvent of propylene glycol and ethanol as the extraction solvent for the first cocoa extract, the final product enhances the aroma and richness of tobacco products, enhances characteristic aromas such as cocoa aroma, baking aroma, sweet aroma, and flue-cured tobacco aroma, and improves the sensory comfort characteristics of the smoke, such as the delicate, soft, rounded, irritation, dryness, astringency, and miscellaneous smell.

[0020] Preferably, the mass ratio of propylene glycol to ethanol is 1:4-2:1, for example, 1:4, 2:7, 1:3, 2:5, 1:2, 2:3, 1:1, 3:2, 2:1, etc. Other specific point values not listed within this numerical range are within the scope of protection of the present invention and will not be repeated here.

[0021] Based on the potential synergistic relationship between propylene glycol and ethanol in extracting spice and flavor substances, the effect is better when they meet the above-mentioned specific mass ratio relationship.

[0022] Preferably, the mass ratio of the cocoa powder raw material to the alcohol solvent is 1:(3-10), for example 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, etc. Other specific values within this numerical range are within the scope of protection of the present invention and are not further described here.

[0023] Preferably, the alcohol extraction treatment is carried out at 20-80°C, for example, 20°C, 25°C, 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 70°C, 80°C, etc. Other specific point values not listed within this numerical range are within the scope of protection of the present invention and are not described here one by one.

[0024] Preferably, the number of extractions in the alcohol extraction treatment is 1-3 times, for example, 1 time, 2 times or 3 times; each time is 40-120 minutes, for example, 40 minutes, 50 minutes, 60 minutes, 70 minutes, 80 minutes, 90 minutes, 100 minutes, 110 minutes, 120 minutes, etc. Other specific point values not listed within this numerical range are within the scope of protection of the present invention and are not described here one by one.

[0025] Preferably, ultrasonic-assisted extraction is also performed during the alcohol extraction process.

[0026] Preferably, stirring is performed during the alcohol extraction process.

[0027] Preferably, in the preparation of the first cocoa extract, the defatting operation after the clear liquid is allowed to stand at low temperature is performed by standing at -20 to 10°C (for example, -20°C, -15°C, -10°C, -5°C, 0°C, 5°C, 10°C, etc.) for more than 2 hours (for example, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, etc.), filtering while cold, and taking the filtrate; other specific points within the above numerical range that are not listed are within the scope of protection of the present invention and are not further described here.

[0028] Preferably, the mass ratio of the cocoa powder raw material to water is 1:(4-15), for example 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, etc. Other specific values within this numerical range are within the scope of protection of the present invention and are not repeated here.

[0029] Preferably, the water extraction treatment is carried out at 40-99°C, for example, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, 90°C, 95°C, 99°C, etc. Other specific values within this numerical range are within the scope of protection of the present invention and are not described in detail here.

[0030] Preferably, the number of extractions in the water extraction treatment is 1-3 times, for example, 1 time, 2 times or 3 times; each time is 40-120 minutes, for example, 40 minutes, 50 minutes, 60 minutes, 70 minutes, 80 minutes, 90 minutes, 100 minutes, 110 minutes, 120 minutes, etc. Other specific point values within this numerical range are within the scope of protection of the present invention and are not repeated here.

[0031] Preferably, stirring is performed during the water extraction process.

[0032] Preferably, in the preparation of the second cocoa extract, the defatting operation after the supernatant is allowed to stand at low temperature is to stand at 1-25°C (e.g., 1°C, 4°C, 8°C, 10°C, 15°C, 20°C, 25°C, etc.) for more than 2 hours (e.g., 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, etc.), and then filter while cold to obtain the filtrate; other specific values within the above numerical range not listed are within the scope of protection of the present invention and are not further described here.

[0033] Preferably, the macroporous resin includes any one of AB-8, X-5, HJ-04, D101 or HPD100, or a combination of at least two thereof, more preferably AB-8 resin.

[0034] Compared with other types of macroporous resins, AB-8 resin is selected as the purification resin for the second cocoa extract. The final product enhances the aroma and richness of tobacco products, enhances the characteristic aromas such as cocoa aroma, baking aroma, sweet aroma, and flue-cured tobacco aroma, and improves the sensory comfort characteristics such as the delicate, soft and roundness, irritation, dryness, astringency, and miscellaneous smell of the smoke.

[0035] Preferably, the elution purification method is: first eluting with water, then eluting with 50% or more ethanol aqueous solution, and collecting the alcohol washing liquid.

[0036] Preferably, the concentration of the ethanol aqueous solution is 85-95%, for example, 85%, 87%, 88%, 90%, 92%, 95%, etc. Other specific point values within this numerical range that are not listed are within the scope of protection of the present invention and will not be repeated here.

[0037] Compared with ethanol aqueous solutions of other concentrations, the alcohol wash solution with 85-95% ethanol aqueous solution is selected to prepare the second cocoa extract, and the fragrance has a better effect in improving the comprehensive sensory quality of tobacco products.

[0038] Preferably, the amount of water is 1-3BV (bed volume), for example, 1BV, 1.5BV, 2BV, 2.5BV or 3BV; the amount of the ethanol aqueous solution is 2-5BV, for example, 2BV, 2.5BV, 3BV, 3.5BV, 4BV, 4.5BV, 5BV, etc.; other specific point values not listed in the above numerical range are within the scope of protection of the present invention and are not repeated here.

[0039] Preferably, the flow rate of the water or ethanol aqueous solution is 1-4BV / h, for example, 1BV / h, 1.5BV / h, 2BV / h, 2.5BV / h, 3BV / h, 3.5BV / h, 4BV / h, etc. Other specific point values not listed within this numerical range are within the scope of protection of the present invention and are not described here one by one.

[0040] Preferably, the mass ratio of the first cocoa extract to the second cocoa extract on a dry matter basis is 1:1-8:1, for example, 1:1, 1.5:1, 2:1, 2.5:1, 3:1, 3.5:1, 4:1, 4.5:1, 5:1, 5.5:1, 6:1, 7:1, 8:1, etc. Other specific values within this numerical range are within the scope of protection of the present invention and are not further described here. 3:1-5:1 is more preferred.

[0041] Based on the potential synergistic relationship between the first cocoa extract and the second cocoa extract in improving the sensory quality of tobacco flavoring, the effect is better when they meet a mass ratio of 1:1-8:1, especially 3:1-5:1.

[0042] Preferably, the cocoa extract tobacco flavoring is prepared by mixing a first cocoa extract and a second cocoa extract in proportion.

[0043] Preferably, the first cocoa extract and the second cocoa extract are mixed in proportion and then concentrated and / or dried.

[0044] In a second aspect, the present invention provides use of the cocoa extract tobacco flavoring according to the first aspect in the production of tobacco products.

[0045] Preferably, the tobacco products include traditional cigarettes, heated cigarettes, electronic cigarettes, and cigars.

[0046] Compared with the prior art, the present invention has the following beneficial effects:

[0047] The present invention creatively combines cocoa extracts obtained by two specific preparation processes as tobacco flavorings. Flavoring substances such as aldehydes, ketones, esters, pyrazines, furanones, pyrones, pyrroles, and alkaloids in the first cocoa extract cooperate with flavor components such as polyphenols (epicatechin, catechin and its polymers, etc.), organic acids, theobromine, and heterocyclic compounds in the second cocoa extract, and the two synergize to enhance the effect. When added to tobacco products, the flavoring can not only significantly enhance the aroma and richness of the tobacco products, and enhance the characteristic aromas such as cocoa aroma, baking aroma, sweet aroma, and flue-cured tobacco aroma, but can also significantly improve the sensory comfort characteristics of the smoke, such as the delicate, soft, rounded, irritation, dryness, astringency, and miscellaneous smell, thereby comprehensively improving the sensory quality of the tobacco products. Compared with the first cocoa extract alone or the second cocoa extract alone, the flavoring is significantly superior in the above-mentioned effects. DETAILED DESCRIPTION

[0048] In order to further illustrate the technical means and effects adopted by the present invention, the technical solutions of the present invention are further described below in conjunction with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.

[0049] The dry matter content of the first cocoa extract involved below is the content of the corresponding solvent measured using YC / T 242-2020 "Gas Chromatography Method for Determination of Ethanol, 1,2-Propanediol and Glycerol Contents of Tobacco Flavorings", and the mass fraction after deducting the solvent is used as the dry matter content of the product; the dry matter content of the second cocoa extract involved below is obtained by obtaining a freeze-dried product through vacuum freeze-drying.

[0050] Example 1

[0051] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1;

[0052] The first cocoa extract is prepared by the following method:

[0053] Heavy alkalized high-fat cocoa powder (Cargill, native to Africa) was extracted with a mixed solvent of 1,2-propylene glycol and ethanol (3:1 by mass) at a solid-liquid ratio of 1:3. The extractions were repeated twice, with the first extraction lasting 2 hours and the second 1 hour at 65°C. The solid solution was filtered through a 300-mesh filter, and the two filtrates were combined. The mixture was allowed to stand at -20°C for 2 hours, then filtered through a 400-mesh filter cloth while still cool to defat the product. The dry matter content of the product was then determined and calculated.

[0054] The second cocoa extract is prepared by the following method:

[0055] Take heavily alkalized high-fat cocoa powder (Cargill, native to Africa), add 5 times the weight of distilled water, extract at 80℃ with mechanical stirring for 2 hours, centrifuge the liquid while hot to remove the residue to obtain a clear liquid; the clear liquid is allowed to stand at 25℃ for 4 hours, and filtered through a 400-mesh filter cloth to defatted to obtain a defatted product;

[0056] Take AB-8 macroporous adsorption resin and perform soaking, column loading, and pretreatment according to standard procedures. At 25°C, apply the defatted product to a sample volume of 6 BV at a flow rate of 2 BV / h. After loading, let it sit for half an hour before eluting with distilled water (2 BV). Then, elute with 95% ethanol at a flow rate of 4 BV / h and an elution volume of 3 BV. Collect the ethanol eluate to obtain the product. Determine and calculate the dry matter content of the product.

[0057] Example 2

[0058] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1;

[0059] The first cocoa extract is prepared by the following method:

[0060] Heavy alkalized low-fat cocoa powder (Nederland, native to West Africa) was extracted with a mixed solvent of 1,2-propylene glycol and ethanol (1:1 by mass) at 25°C using an ultrasonic cycle extractor with a solid-liquid ratio of 1:10, an ultrasonic frequency of 40 kHz, a power of 750 W, a total extraction time of 90 minutes, an ultrasonic time and interval of 2 seconds / 1 second, and a stirring speed of 1500 rpm. The solid solution was filtered through a 300-mesh filter. The filtrate was allowed to stand at -20°C for 2 hours and then filtered through a 400-mesh filter cloth while still cool to defat the product. The dry matter content of the product was also determined.

[0061] The second cocoa extract is prepared by the following method:

[0062] Take lightly alkaline low-fat cocoa powder (purchased from Zhengzhou Zhongyi Biotechnology Co., Ltd., originating from Indonesia), add 15 times the mass of distilled water, and extract with an ultrasonic circulation extractor at 25°C, with an ultrasonic frequency of 40kHz, a power of 750W, a total extraction time of 50min, an ultrasonic time and interval time of 2s / 1s, a stirring speed of 1300rpm, and filter the feed liquid through a 300-mesh filter; the filtrate is allowed to stand at 4°C for 2h and filtered through a 400-mesh filter cloth for defatting to obtain a defatted product.

[0063] Take AB-8 macroporous adsorption resin and perform soaking, column loading, and pretreatment according to standard procedures. At 25°C, apply the defatted product to a sample volume of 15 BV at a flow rate of 4 BV / h. After loading, let it sit for half an hour before eluting with distilled water (1 BV). Then, elute with 85% ethanol at a flow rate of 2 BV / h and an elution volume of 4 BV. Collect the ethanol eluate to obtain the product. Determine the dry matter content of the product.

[0064] Example 3

[0065] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 3:1; wherein the preparation methods of the first cocoa extract and the second cocoa extract are the same as those of Example 1.

[0066] Example 4

[0067] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 1:1; wherein the preparation methods of the first cocoa extract and the second cocoa extract are the same as those of Example 1.

[0068] Example 5

[0069] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 8:1; wherein the preparation methods of the first cocoa extract and the second cocoa extract are the same as those of Example 1.

[0070] Example 6

[0071] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this embodiment and Example 1 is only that the preparation method of the first cocoa extract is different, and 1,2-propylene glycol is used instead of a mixed solvent of 1,2-propylene glycol / ethanol (mass ratio 3:1) as the extraction solvent. Other conditions are consistent with Example 1.

[0072] Example 7

[0073] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this embodiment and Example 1 is only that the preparation method of the first cocoa extract is different, and ethanol is used instead of a mixed solvent of 1,2-propylene glycol / ethanol (mass ratio 3:1) as the extraction solvent. Other conditions are consistent with Example 1.

[0074] Example 8

[0075] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this embodiment and Example 1 is only that the second cocoa extract is prepared by a different method, and HJ-04 resin is used instead of AB-8 resin. Other conditions are the same as those in Example 1.

[0076] Example 9

[0077] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this embodiment and Example 1 is only that the second cocoa extract is prepared by a different method, and X-5 resin is used instead of AB-8 resin. Other conditions are the same as those in Example 1.

[0078] Example 10

[0079] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this embodiment and Example 1 is only that the second cocoa extract is prepared by a different method, and D101 resin is used instead of AB-8 resin. Other conditions are the same as those in Example 1.

[0080] Example 11

[0081] This embodiment provides a cocoa extract tobacco flavoring, comprising a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference from Example 1 lies only in the preparation method of the second cocoa extract, in which HPD100 resin is used instead of AB-8 resin. Other conditions are the same as those in Example 1.

[0082] Example 12

[0083] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this embodiment and Example 1 is only that the second cocoa extract is prepared by a different method, using 75% ethanol instead of 95% ethanol. Other conditions are the same as those in Example 1.

[0084] Example 13

[0085] This embodiment provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this embodiment and Example 1 is only that the second cocoa extract is prepared by a different method, using 50% ethanol instead of 95% ethanol. Other conditions are the same as those in Example 1.

[0086] Comparative Example 1

[0087] This comparative example provides a cocoa extract tobacco flavoring, which is simply the first cocoa extract in Example 1.

[0088] Comparative Example 2

[0089] This comparative example provides a cocoa extract tobacco flavoring, which is simply the second cocoa extract in Example 1.

[0090] Comparative Example 3

[0091] This comparative example provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this comparative example and Example 1 is only the preparation method of the second cocoa extract, which is as follows:

[0092] Take heavily alkalized high-fat cocoa powder (Cargill, native to Africa), add 5 times the weight of distilled water, extract at 80°C with mechanical stirring for 2 hours, centrifuge the hot liquid to remove the residue to obtain a clear liquid; the clear liquid is allowed to stand at 25°C for 4 hours, and filtered through a 400-mesh filter cloth to defat, thereby obtaining a second cocoa extract.

[0093] Comparative Example 4

[0094] This comparative example provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this comparative example and Example 1 is only the preparation method of the first cocoa extract, which is as follows:

[0095] Heavy alkalized high-fat cocoa powder (Cargill, native to Africa) was extracted with a mixed solvent of 1,2-propylene glycol / ethanol (mass ratio 3:1) at a solid-liquid ratio of 1:3. The extraction was repeated twice, with the first extraction lasting 2 hours and the second extraction lasting 1 hour at 65°C. The solid solution was filtered through a 300-mesh filter, and the two filtrates were combined. The solution was allowed to stand at -20°C for 2 hours and then filtered through a 400-mesh filter cloth while still cool to defatting.

[0096] Prepare AB-8 macroporous adsorption resin and perform soaking, column loading, and pretreatment according to standard procedures. Load the degreased product at 2 BV / h at 25°C, using a sample volume of 6 BV. After loading, allow the sample to stand for half an hour before eluting with distilled water, using a 2 BV elution volume. Elute with 95% ethanol at a flow rate of 4 BV / h and an elution volume of 3 BV. Collect the ethanol eluate to obtain the product.

[0097] Comparative Example 5

[0098] This comparative example provides a cocoa extract tobacco flavoring, which is composed of a first cocoa extract and a second cocoa extract in a dry matter mass ratio of 5:1. The difference between this comparative example and Example 1 is only that the first cocoa extract and the second cocoa extract are prepared by different methods, and both lack defatting treatment. The details are as follows:

[0099] The first cocoa extract is prepared by the following method:

[0100] Take heavily alkalized high-fat cocoa powder (Cargill, native to Africa) and extract it with a mixed solvent of 1,2-propylene glycol / ethanol (mass ratio 3:1) with a solid-liquid ratio of 1:3. The extraction is carried out twice, the first extraction is 2 hours, the second extraction is 1 hour, and the extraction temperature is 65°C; the solid liquid is filtered through a 300-mesh filter, and the two filtrates are collected and combined to obtain the product.

[0101] The second cocoa extract is prepared by the following method:

[0102] Take heavily alkalized high-fat cocoa powder (Cargill, native to Africa), add 5 times the weight of distilled water, extract at 80℃ with mechanical stirring for 2h, and centrifuge the hot solution to remove the residue to obtain a clear liquid;

[0103] Prepare AB-8 macroporous adsorption resin and perform soaking, column loading, and pretreatment according to standard procedures. At 25°C, apply the above-mentioned clear solution at a flow rate of 2 BV / h, with a sample volume of 6 BV. After loading, allow the sample to stand for half an hour before eluting with distilled water, with an elution volume of 2 BV. Then, elute with 95% ethanol at a flow rate of 4 BV / h, with an elution volume of 3 BV. Collect the ethanol eluate to obtain the product.

[0104] Test Example 1

[0105] The cocoa extract tobacco flavorings prepared in Examples 1-13 and Comparative Examples 1-5 were added to unflavored, unadded, blank cigarettes at a dry matter dosage of 100 μg / g using a cigarette flavoring injection machine to form sample cigarettes. Another blank cigarette was also infused with an equal amount of solvent to form a reference cigarette. The cigarettes were sealed and stored at a temperature of (22±1)°C and a relative humidity of 60%±2% for at least 48 hours. Sensory evaluation of the sample and reference cigarettes was conducted according to the method described in "YC / T 497-2014 Sensory Evaluation Method for Chinese-Style Cigarettes." The results are shown in Tables 1-4.

[0106] Table 1

[0107]

[0108] Note: A higher score for the "bitterness" index indicates a bitterer taste, which is an indicator of side effects.

[0109] As can be seen from the data in Table 1, compared with the comparative example products, the cocoa extract tobacco flavoring of the present invention combines two cocoa extracts prepared by specific preparation processes. When added to cigarettes, it can not only significantly enhance the aroma and richness of the cigarettes, enhancing the characteristic aromas such as cocoa aroma, roasted aroma, sweet aroma, and flue-cured tobacco aroma, but also significantly improve the sensory comfort characteristics of the smoke, such as the delicate, soft and roundedness, irritation, dryness, astringency, and miscellaneous smell, thereby comprehensively improving the sensory quality of the cigarettes. Compared with the same amount of the first cocoa extract (Comparative Example 1) or the same amount of the second cocoa extract (Comparative Example 2), the cocoa extract tobacco flavoring of the present invention is significantly superior in terms of sensory quality, indicating that the first cocoa extract and the second cocoa extract synergistically enhance the sensory quality of cigarettes.

[0110] Table 2

[0111]

[0112]

[0113] As shown in Table 2, a comparison of Example 1 with Examples 3-5 demonstrates that, based on the potential synergistic relationship between the first and second cocoa extracts in improving the sensory quality of tobacco products, the effects are even greater when the mass ratio of the first and second cocoa extracts is between 1:1 and 8:1, and particularly between 3:1 and 5:1. A comparison of Example 1 with Examples 6-7 demonstrates that using a mixed solvent of propylene glycol and ethanol as the extraction solvent for the first cocoa extract results in a more effective final product in improving the sensory quality of tobacco products than using either ethanol or propylene glycol alone as the extraction solvent.

[0114] Table 3

[0115]

[0116]

[0117] As can be seen from the data in Table 3, by comparing Example 1 with Examples 8-11, it can be seen that, compared with other types of macroporous resins, the selection of AB-8 resin as the purification resin for the second cocoa extract results in a final product that enhances the aroma and richness of tobacco products, including characteristic aromas such as cocoa, roasted, sweet, and flue-cured tobacco, and is superior in improving the sensory comfort characteristics of the smoke, such as its delicate, soft, rounded nature, irritation, dryness, astringency, and odor.

[0118] Table 4

[0119]

[0120]

[0121] As can be seen from the data in Table 4, by comparing Example 1 with Examples 12-13, it can be seen that when the alcohol wash solution with 85-95% ethanol aqueous solution is selected as the second cocoa extract, the flavoring is more effective in improving the overall sensory quality of tobacco products compared with ethanol aqueous solutions with other concentrations.

[0122] Test Example 2

[0123] The cocoa extract tobacco flavorings prepared in Example 2 and Comparative Examples 1-2 were diluted with 50% ethanol and evenly sprayed onto unflavored blank tobacco from heat-not-burn cigarettes at a dry matter ratio of 150 μg / g. Sample tobacco was used. Separate portions of the blank tobacco were sprayed with an equal amount of 50% ethanol to serve as reference tobacco. The sample and reference tobaccos were equilibrated at a constant temperature and humidity for at least 48 hours before being rolled into heat-not-burn cigarettes. Sensory evaluation of the heat-not-burn sample and reference cigarettes was conducted according to the method described in "YC / T 497-2014 Sensory Evaluation Method for Chinese-Style Cigarettes." The results are shown in Table 5.

[0124] Table 5

[0125]

[0126] Note: The scores of the “coolness”, “fruity aroma”, “bean aroma”, “green aroma”, “floral aroma”, “paste aroma”, “milky aroma” and “herbal aroma” indicators of each evaluated cigarette are all 0.

[0127] As can be seen from the data in Table 5, compared with the same amount of the first cocoa extract (Comparative Example 1) or the same amount of the second cocoa extract (Comparative Example 2), the cocoa extract tobacco flavoring of the present invention combines cocoa extracts produced by two specific preparation processes and is added to heat-not-burn cigarettes. It is more effective in enhancing the aroma and richness of tobacco products, enhancing characteristic aromas such as cocoa aroma, roasted aroma, sweet aroma, and flue-cured tobacco aroma, and improving the sensory comfort characteristics of smoke, such as the delicate, soft and roundedness, irritation, dryness, astringency, and miscellaneous smells. This improves the sensory quality of the tobacco products, further demonstrating that the first cocoa extract and the second cocoa extract produced by the specific preparation process selected by the present invention synergistically enhance the sensory quality of tobacco products.

[0128] The applicant declares that the present invention is illustrated by the above-described embodiments, but the present invention is not limited to the above-described embodiments. This does not mean that the present invention must rely on the above-described embodiments in order to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent replacements for raw materials in the present invention, additions of auxiliary ingredients, and selection of specific methods, etc., fall within the scope of protection and disclosure of the present invention.

[0129] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection of the present invention.

[0130] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any appropriate manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A cocoa extract tobacco flavoring, characterized in that: The cocoa extract tobacco flavoring comprises a first cocoa extract and a second cocoa extract; The first cocoa extract is prepared by a preparation method comprising the following steps: The cocoa powder raw material is mixed with an alcohol solvent for alcohol extraction, the alcohol extraction product is separated into solid and liquid, and the supernatant is taken and the supernatant is allowed to stand at a low temperature and then defatted to obtain a first cocoa extract; The second cocoa extract is prepared by a preparation method comprising the following steps: The cocoa powder raw material is mixed with water for water extraction treatment, the water extraction product is separated into solid and liquid, the supernatant is taken, the supernatant is allowed to stand at low temperature and then defatted, the defatted product is loaded onto a macroporous resin chromatography column, eluted and purified, and the eluate is collected to obtain a second cocoa extract.

2. The cocoa extract tobacco flavoring according to claim 1, characterized in that The cocoa powder raw materials are each independently selected from natural cocoa powder and / or alkalized cocoa powder; Preferably, the alkalized cocoa powder comprises heavily alkalized cocoa powder and / or lightly alkalized cocoa powder; Preferably, the cocoa powder raw materials are each independently selected from any one of high-fat cocoa powder, medium-fat cocoa powder or low-fat cocoa powder, or a combination of at least two thereof.

3. The cocoa extract tobacco flavoring according to claim 1 or 2, characterized in that The alcohol solvent is selected from any one of ethanol, propylene glycol or glycerol or a combination of at least two thereof; preferably a combination of propylene glycol and ethanol; Preferably, the mass ratio of propylene glycol to ethanol is 1:4-2:1; Preferably, the mass ratio of the cocoa powder raw material to the alcohol solvent is 1:(3-10).

4. The cocoa extract tobacco flavoring according to any one of claims 1 to 3, characterized in that: The alcohol extraction treatment is carried out at 20-80°C; Preferably, the alcohol extraction process is performed 1-3 times, each time for 40-120 minutes; Preferably, ultrasonic-assisted extraction is also performed during the alcohol extraction process; Preferably, stirring is performed during the alcohol extraction process.

5. The cocoa extract tobacco flavoring according to any one of claims 1 to 4, characterized in that: In the preparation of the first cocoa extract, the operation of defatting the clear liquid after standing at low temperature is to stand at -20 to 10° C. for more than 2 hours, filter while it is cold, and take the filtrate.

6. The cocoa extract tobacco flavoring according to any one of claims 1 to 5, characterized in that: The mass ratio of the cocoa powder raw material to water is 1:(4-15); Preferably, the water extraction treatment is carried out at 40-99°C; Preferably, the water extraction process is performed 1-3 times, each time for 40-120 minutes; Preferably, stirring is performed during the water extraction process.

7. The cocoa extract tobacco flavoring according to any one of claims 1 to 6, characterized in that: In the preparation of the second cocoa extract, the operation of defatting the clear liquid after standing at low temperature is to stand at 1-25° C. for more than 2 hours, filter while cold, and take the filtrate.

8. The cocoa extract tobacco flavoring according to any one of claims 1 to 7, characterized in that: The macroporous resin includes any one of AB-8, X-5, HJ-04, D101 or HPD100 or a combination of at least two thereof; AB-8 resin is more preferred; Preferably, the elution purification method is: first eluting with water, then eluting with 50% or more ethanol aqueous solution, and collecting the alcohol washing liquid; Preferably, the concentration of the ethanol aqueous solution is 85-95%; Preferably, the amount of water is 1-3BV, and the amount of ethanol aqueous solution is 2-5BV; Preferably, the flow rate of the water or ethanol aqueous solution is 1-4 BV / h.

9. The cocoa extract tobacco flavoring according to any one of claims 1 to 8, characterized in that: The mass ratio of the first cocoa extract to the second cocoa extract on a dry matter basis is 1:1-8:1, more preferably 3:1-5:1; Preferably, the cocoa extract tobacco flavoring is prepared by mixing a first cocoa extract and a second cocoa extract in a certain proportion; Preferably, the first cocoa extract and the second cocoa extract are mixed in proportion and then concentrated and / or dried.

10. Use of the cocoa extract tobacco flavoring according to any one of claims 1 to 9 in the production of tobacco products; Preferably, the tobacco products include traditional cigarettes, heated cigarettes, electronic cigarettes, and cigars.

Images