High-theobromine tea extract as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of natural perfume for cigarettes, and particularly relates to a high-theobromine tea extract as well as a preparation method and application thereof. The preparation method comprises the following steps: sequentially carrying out water elution and alcohol solution desorption on a tea leaf extract with theobromine content higher than that of caffeine by adopting a macroporous adsorption resin column, and collecting a desorption solution, so as to obtain the high-theobromine tea leaf extract. The preparation process of the high-theobromine tea extract is simple, convenient and easy to operate, and is suitable for industrial production and application; and fat-soluble flavor substances and tea polyphenols in the tea leaf extract are well reserved in the separation process. After being used in tobacco products, especially blended with other tea leaf extracts, the tea leaf extract can obviously improve the aroma, strength, sensory comfort and characteristic note of smoke.

Description

Technical Field

[0001] The invention belongs to the technical field of natural tobacco flavors, and particularly relates to a high-theobromine tea extract, a preparation method and an application thereof. Background Art

[0002] Tea extract is a natural flavoring widely used in the tobacco industry. Adding it to cigarettes enriches the aroma, reduces irritation, and improves the aftertaste. The purine alkaloids found in traditionally cultivated tea are primarily caffeine, accounting for 2%-4% of the tea's dry matter. Theobromine is a secondary component, making up approximately 0.05% of the dry matter. Theophylline is even lower, at approximately 0.002%. However, within the tea group (Camellia Sect. Thea), several species contain significantly higher levels of theobromine than caffeine, including C. ptilophylla, C. purpurea, C. irrawadiensis, C. crassicoluma, and C. gymnogyna. Theobromine, a representative example, can contain up to 6.8% of theobromine, while containing virtually no caffeine or theophylline. Theobromine is also the predominant alkaloid in cocoa beans, comprising approximately 1% of their dry weight, far lower than the theobromine content in cocoa tea. Theobromine is directly related to some of the sensory flavors of beverages and foods such as tea and chocolate, and is also closely related to the sensory quality of tobacco flavorings such as tea extracts and cocoa tea extracts. However, pure theobromine has no aroma, and adding it to cigarettes has no significant effect on the sensory quality of cigarettes. This research team has confirmed through experiments that within a certain ratio range, theobromine has a synergistic effect on related natural tobacco flavorings. Therefore, the study of the separation and preparation technology of theobromine enriched in cocoa tea extracts and the development of tea extract tobacco flavorings with high theobromine content will further enhance the effects of cocoa tea extracts while maintaining their original advantages, which will have guiding significance for the deep processing of tea extract tobacco flavorings.

[0003] In the field of separation and purification of functional components of tea leaves, macroporous adsorption resin technology has been widely used in the directional enrichment and removal of target components. For example, Chinese patent CN1374280A discloses a process for removing alkaloids from tea polyphenol extracts by selective adsorption with macroporous resins, which dissolves the extract in water or an organic solvent and achieves efficient separation of alkaloids and tea polyphenols after adsorption on a resin column. However, the core purpose of this technology is to remove alkaloids to purify tea polyphenols, and it does not involve how to achieve selective enrichment of specific alkaloids (such as theobromine) by optimizing resin properties, while effectively retaining other natural flavor substances in the tea extract and improving the effect of such natural spices. In addition, current research on theobromine in tobacco flavorings mostly focuses on its detection method, and less on its extraction and separation process research. Therefore, the present invention develops an industrialized preparation method for a high-theobromine tea extract suitable for the field of natural spices, adopts macroporous adsorption resin column chromatography technology to achieve appropriate enrichment of theobromine in the tea extract, and comprehensively applies the developed high-theobromine tea extract to various tobacco products. Summary of the Invention

[0004] The first object of the present invention is to provide a method for preparing a high-theobromine tea extract, which is simple and easy to operate and suitable for industrial production applications.

[0005] The second object of the present invention is to provide the above-mentioned high-theobromine tea extract, which, after being used in tobacco products, has different degrees of improvement in the aroma, strength, sensory comfort, characteristic fragrance and other aspects of the smoke compared to the unseparated tea extract.

[0006] A third object of the present invention is to provide a composition of high-theobromine tea extract, which can further enhance the aroma, concentration, sensory comfort, and characteristic fragrance of smoke compared to a single high-theobromine tea extract, with better effects.

[0007] The fourth object of the present invention is to provide the use of the above-mentioned high-theobromine tea extract or the above-mentioned high-theobromine tea extract composition in cigarettes.

[0008] In order to achieve the above object, the technical solution adopted by the present invention is:

[0009] The invention discloses a method for preparing a high-theobromine tea extract. The method comprises the following steps: using a macroporous adsorption resin column to sequentially perform water elution and alcohol solution desorption on a tea extract having a theobromine content higher than that of caffeine, and collecting the desorbed liquid to obtain the high-theobromine tea extract.

[0010] Furthermore, the tea extract with a higher theobromine content than caffeine is an extract of a tea variety with theobromine as the dominant alkaloid and / or a product treated by microbial fermentation, enzymatic hydrolysis, and Maillard reaction.

[0011] Furthermore, the tea variety with theobromine as the dominant alkaloid is selected from any one or more of cocoa tea, purple fruit tea, Yunnan-Myanmar tea, thick-axis tea, bald room tea, and red bud tea.

[0012] Furthermore, the macroporous adsorption resin in the macroporous adsorption resin column is any one of AB-8, X-5, HPD100, HJ-04, and HZ816.

[0013] Furthermore, in the sample loading operation, the sample loading amount is less than the theobromine adsorption saturation amount of the macroporous adsorption resin column, and the sample loading flow rate is 1 to 3 BV / h.

[0014] Furthermore, after the sample is loaded, it needs to be left to stand for 0.25-1h.

[0015] Furthermore, the amount of water used in the water elution is 1 to 3 BV; the alcohol solution is an ethanol aqueous solution with an ethanol volume fraction of 35% to 90%; the amount of alcohol solution used in the alcohol solution desorption is 2 to 5 BV, and the elution flow rate is 1 to 4 BV / h.

[0016] Furthermore, after collecting the desorption liquid, the process also includes removing part or all of the solvent; the method for removing the solvent is any one of reverse osmosis membrane filtration, vacuum distillation, freeze drying, and spray drying.

[0017] A high-theobromine tea extract is prepared by the above-mentioned preparation method of the high-theobromine tea extract.

[0018] A composition of a high-theobromine tea extract comprises the high-theobromine tea extract and any other tea extract, wherein the dry matter mass ratio of the high-theobromine tea extract to the other tea extract is 1:(0.5-10). The present invention does not specifically limit the other tea extract, as long as it is a conventional tea extract.

[0019] Furthermore, the theobromine content in the high-theobromine tea extract composition is between 6% and 9% on a dry basis.

[0020] Furthermore, the composition of high theobromine tea extract comprises the above-mentioned high theobromine tea extract and a tea extract with a theobromine content of 1%-4% on a dry basis; the mass ratio of the high theobromine tea extract to the tea extract with a theobromine content of 1%-4% on a dry basis is 1:(0.5-10), more preferably 1:(3.5-5).

[0021] Application of the high-theobromine tea extract or the combination of the high-theobromine tea extract in tobacco products.

[0022] Furthermore, the tobacco product is one of cigarettes, pipe tobacco, cigars, and hookahs.

[0023] Furthermore, the cigarettes include traditional combustion cigarettes and heat-not-burn cigarettes.

[0024] Furthermore, the high-theobromine tea extract or the high-theobromine tea extract composition is added to shredded tobacco in an amount of 0.0005-0.005% of the mass of the shredded tobacco based on dry matter.

[0025] Furthermore, the high theobromine tea extract or the high theobromine tea extract composition is applied to cigarette paper in an amount of 0.05-0.5 g / m2 based on dry matter. 2 .

[0026] A tobacco product containing the high-theobromine tea extract or a combination of the high-theobromine tea extracts.

[0027] The beneficial technical effects of the present invention are:

[0028] The preparation process of the high-theobromine tea extract of the present invention is simple and easy to operate, and is suitable for industrial production and application; and the separation process better retains the fat-soluble flavor substances and tea polyphenols in the tea extract. After using it in tobacco products, it has the effects of reducing cigarette irritation to the oral cavity, throat, and nasal cavity, reducing oral residue and astringency, reducing throat dryness, and increasing sweetness. At the same time, it can also increase the aroma, richness, strength and characteristic aroma intensity of the cigarette, which are improved to varying degrees compared with tea extracts that have not been enriched and separated. In addition, after the high-theobromine tea extract is formulated with other tea extracts, it is found that it has a synergistic effect on tea extract, a natural tobacco flavoring, and can further enhance the aroma quality, aroma quantity, sensory comfort, and characteristic aroma of the smoke, with better effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 The HPLC-DAD chromatogram of the cocoa tea water extract in Example 1 is shown. DETAILED DESCRIPTION

[0030] The following is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it is not intended that the specific implementation of the present invention is limited to these descriptions. For those skilled in the art of the present invention, without departing from the inventive concept, several simple deductions or replacements can also be made, all of which should be considered to belong to the scope of protection of the present invention. The specific conditions not indicated in the examples are carried out according to conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used, unless otherwise specified, are conventional products obtained through commercial channels.

[0031] (1) Embodiment

[0032] Example 1

[0033] Example 1 provides a method for preparing a high-theobromine tea extract, comprising the following steps:

[0034] (1) Cocoa tea (purchased from Guangdong Degaoxin Planting Co., Ltd.) was taken, 8 times the mass of distilled water was added, and the mixture was mechanically stirred and extracted at 90°C for 2 h. The extract was cooled and filtered to remove the residue to obtain the cocoa tea extract. The theobromine content was measured using NY / T 3631-2020 "Determination of theobromine and theophylline content in tea by high performance liquid chromatography" and was 3.0451 mg / g. The liquid chromatogram is shown in Figure 1 After deducting the solvent content, the theobromine dry basis content was calculated to be 3.39%.

[0035] (2) Take AB-8 macroporous adsorption resin and soak, load, and pretreat according to conventional procedures. At room temperature, take the above cocoa tea extract at a sample flow rate of 2 BV / h and a sample volume of 4 BV. After the sample is loaded, let it stand for 1 hour; then rinse with distilled water with an elution volume of 1 BV, and then elute with an ethanol solution with a volume fraction of 95% ethanol for desorption at an eluent flow rate of 4 BV / h and an elution volume of 2 BV. Collect the desorbed liquid to obtain the high theobromine tea extract.

[0036] This embodiment also provides a high-theobromine tea extract obtained by the above preparation method. The theobromine dry basis content of the high-theobromine tea extract was measured to be 28.37%, which is 8.37 times the dry basis content of 3.39% before separation and enrichment, achieving a higher enrichment rate.

[0037] Example 2

[0038] Example 2 provides a method for preparing a high-theobromine tea extract, comprising the following steps:

[0039] (1) Cocoa tea (purchased from Guangdong Degaoxin Planting Co., Ltd.) was pulverized using a grinder and added to a 10% ethanol-water solution at a material-liquid mass ratio of 1:12. Extraction was performed using an ultrasonic circulation extractor for 50 min. After the extraction, the extract was filtered using a filter to obtain a cocoa tea extract; the theobromine content on a dry basis was determined to be 3.12%. One times the mass of purified water was added to the cocoa tea extract, and the mixture was thoroughly stirred and mixed using a high-shear mixer to obtain a cocoa tea extract dilution.

[0040] (2) Take HJ-04 macroporous adsorption resin (purchased from Tianjin Haoju Resin Technology Co., Ltd.) and soak, column pack and pretreat according to conventional operations; take the above cocoa tea extract dilution solution and load it at a flow rate of 4BV / h at room temperature, with a loading volume of 6BV. After loading, let it stand for 15 minutes, then rinse with distilled water, with an elution volume of 2BV, and then elute with 50% ethanol, with an eluent flow rate of 1BV / h and an elution volume of 4BV. Collect the ethanol eluate to obtain the high theobromine tea extract.

[0041] This embodiment also provides a high-theobromine tea extract obtained by the above preparation method. The theobromine dry basis content of the high-theobromine tea extract is measured to be 26.16%.

[0042] Example 3

[0043] Example 3 provides a composition of high-theobromine tea extract, which is prepared by mixing the high-theobromine tea extract prepared in Example 1 and the cocoa tea aqueous extract obtained in step (1) of Example 1 in a dry matter ratio of 1:3.5 (the theobromine dry matter content in the composition is 8.94%).

[0044] Example 4

[0045] Example 4 provides a composition of high-theobromine tea extract, which is prepared by mixing the high-theobromine tea extract prepared in Example 2 and the cocoa tea extract obtained in step (1) of Example 2 in a dry matter ratio of 1:5 (the theobromine dry basis content in the composition is 6.96%).

[0046] (2) Test examples

[0047] Test Example 1

[0048] The flavoring effect of the high-theobromine tea extract prepared by the present invention on cigarettes was tested, and the specific method is as follows:

[0049] The cocoa tea aqueous extract prepared in Example 1, the high-theobromine tea extract, and the high-theobromine tea extract composition prepared in Example 3 were diluted with water to form solutions with the same dry matter content. The solutions were added to blank experimental cigarettes produced by Shanghai Tobacco Group without flavoring or additives at a dosage of 20 μg / g of dry matter using a cigarette flavoring injection machine to prepare three sample cigarettes. Another blank cigarette was added with an equal amount of pure water as a reference cigarette. The cigarettes were sealed and stored at a temperature of (22±1)°C and a relative humidity of 60%±2% for more than 5 days. The sample cigarettes and the reference cigarettes were subjected to sensory evaluation with reference to YC / T 497-2014 "Sensory Evaluation Method for Chinese-Style Cigarettes". All indicators were scored in units of 0.5 points. The evaluation team was established in accordance with the requirements of GB 5606.4. The score of each individual indicator of the cigarette was the arithmetic average of the scores of all evaluators. The results are shown in Table 1:

[0050] Table 1: Effects of adding high-theobromine tea extract to cigarettes on sensory evaluation results

[0051]

[0052] Note: The scores for the "Cooling Flavor," "Sun-Dried Tobacco Aroma," "Fruit Aroma," "Spicy Aroma," "Floral Aroma," "Herb Aroma," "Bean Aroma," "Cocoa Aroma," "Milk Aroma," and "Ointment Aroma" indicators for each evaluated cigarette were all 0. A higher score for the "Bitterness" indicator indicates a stronger bitter taste and a more severe adverse effect. For all other indicators, higher scores indicate better effects. The same applies below.

[0053] Table 1 shows that high-theobromine tea extract is superior to cocoa tea extract in increasing cigarette smoke density, richness, and punch, as well as masking off-flavors. It also does not increase smoke irritation, mouth residue / dryness, or astringency, and its refreshing, green, and sweet aromas are more prominent. The combined effect of high-theobromine tea extract and cocoa tea extract is significantly superior.

[0054] Test Example 2

[0055] The flavoring effect of the high-theobromine tea extract prepared by the present invention on cigarettes was tested, and the specific method is as follows:

[0056] The high-theobromine tea extract prepared in Example 1 and the high-theobromine tea extract prepared in Example 3 were subjected to vacuum distillation to remove ethanol; the cocoa tea aqueous extract prepared in Example 1 and the cocoa tea aqueous extract were diluted with water to form solutions with the same dry matter content, and used as cigarette paper coating liquids at a dry matter content of 0.5 g / m 2The coating amount of the coating was applied to ordinary cigarette paper, dried at low temperature to evaporate excess moisture, and then the cigarette paper was cut. The blank tobacco of the "Purple Air Comes from the East" cigarette leaf group was rolled into cigarettes and attached to filter rods to produce three sample cigarettes. Another cigarette made with ordinary cigarette paper using the same process served as a reference cigarette. The sample cigarettes and the reference cigarettes were subjected to sensory evaluation using the same method as in Experimental Example 1. The results are shown in Table 2:

[0057] Table 2: Effects of high-theobromine tea extract coated on ordinary cigarette paper on sensory evaluation results of cigarettes

[0058]

[0059]

[0060] Note: The scores of the “bitterness”, “coolness”, “floral aroma”, “herbal aroma”, “cocoa aroma” and “milky aroma” indicators of each evaluated cigarette are all 0.

[0061] As shown in Table 2, the composition of Example 3, obtained by mixing high-theobromine tea extract and cocoa tea aqueous extract in appropriate proportions, when applied to cigarette paper, also has an outstanding effect of improving cigarette comfort, specifically in terms of reducing oral and throat irritation, alleviating oral residue and astringency, and masking foreign odors. At the same time, it can also increase the aroma, richness and strength of the cigarette, and also enhance the characteristic aromas such as fresh fragrance, green fragrance and sweet fragrance.

[0062] Test Example 3

[0063] The flavoring effect of the high-theobromine tea extract prepared by the present invention on heat-not-burn cigarettes was tested, and the specific method is as follows:

[0064] The cocoa tea extract, high-theobromine tea extract prepared in Example 2, and the combination of high-theobromine tea extract prepared in Example 4 were diluted with water to form solutions with the same dry matter content. The solutions were then evenly sprayed onto unflavored and unadded heat-not-burn cigarette tobacco at a dry matter content of 50 μg / g to prepare sample tobacco. Another blank tobacco was sprayed with an equal amount of pure water as a reference tobacco. The sample and reference tobaccos were equilibrated under constant temperature and humidity conditions for more than 48 hours, and then each was made into a heat-not-burn cigarette. Sensory evaluation of the heat-not-burn sample and reference cigarettes was conducted with reference to YC / T 497-2014. The results are shown in Table 3:

[0065] Table 3: Effects of high-theobromine tea extract on sensory evaluation results of heat-not-burn cigarettes

[0066]

[0067]

[0068] Note: The scores of the indicators of "cool taste", "sun-dried tobacco aroma", "fruity aroma", "spicy aroma", "woody aroma", "floral aroma", "herbal aroma", "bean aroma", "cocoa aroma", "milky aroma" and "paste aroma" of each evaluated cigarette are all 0.

[0069] As shown in Table 3, the composition of Example 4 obtained by mixing high-theobromine tea extract and cocoa tea extract in an appropriate proportion is more effective in increasing the aroma, richness, smoke concentration and enhancing the fresh, green and sweet aromas of heat-not-burn cigarettes. At the same time, it can reduce the irritation and impurities of smoke, and does not increase oral residue, astringency and bitterness, resulting in a better overall effect.

[0070] In summary, compared to cocoa tea aqueous extract or cocoa tea extract, the high-theobromine tea extract prepared by the present invention has a theobromine content of 26-29% on a dry basis. When applied to tobacco products, it reduces cigarette irritation to the mouth, throat, and nasal cavity, alleviates oral residue and astringency, masks impurities, and increases sweetness. It also enhances the aroma, richness, and punch of the cigarette, achieving varying degrees of improvement compared to unenriched and separated tea extracts. The inventors also discovered that blending this high-theobromine tea extract with other tea extracts has a synergistic effect on tea extract, a natural tobacco flavoring, further enhancing the aroma, richness, sensory comfort, and characteristic aroma of the smoke, resulting in superior results.

[0071] Finally, it should be noted that the above embodiments are intended only to illustrate the technical solutions of the present invention and are not intended to limit the same. The basic principles and main features of the present invention have been described above using specific implementation schemes. Modifications or substitutions may be made based on the present invention, but such modifications or substitutions do not detract from the essence of the corresponding technical solutions from the scope of protection claimed by the present invention.

Claims

1. A method for preparing a high-theobromine tea extract, characterized in that: The high-theobromine tea extract is obtained by sequentially eluting with water and desorbing with an alcohol solution using a macroporous adsorption resin column, and collecting the desorbed liquid.

2. The method for preparing the high theobromine tea extract according to claim 1, wherein The tea leaves with a higher theobromine content than caffeine are selected from any one or more of cocoa tea, purple fruit tea, Yunnan-Myanmar tea, thick-axis tea, bald room tea, and red bud tea.

3. The method for preparing the high theobromine tea extract according to claim 1, wherein The amount of water used in the water elution is 1 to 3 BV; the alcohol solution is an ethanol aqueous solution with an ethanol volume fraction of 35% to 95%; the amount of the alcohol solution used in the alcohol solution desorption is 2 to 5 BV, and the elution flow rate is 1 to 4 BV / h.

4. A high-theobromine tea extract, characterized in that The extract is prepared by the method for preparing the high theobromine tea extract according to any one of claims 1 to 3.

5. A composition of high theobromine tea extract, characterized in that The invention comprises the high theobromine tea extract according to claim 4 and any other tea extract; the dry matter mass ratio of the high theobromine tea extract and the other any other tea extract is 1:(0.5-10).

6. Use of the high-theobromine tea extract according to claim 4 or the combination of the high-theobromine tea extract according to claim 5 in tobacco products.

7. The use according to claim 6, characterized in that The tobacco product is one of cigarettes, pipe tobacco, cigars and hookahs.

8. The use according to claim 7, characterized in that The high-theobromine tea extract or the high-theobromine tea extract composition is added to shredded tobacco in an amount of 0.0005% to 0.005% of the mass of the shredded tobacco based on dry matter.

9. The use according to claim 7, characterized in that The high-theobromine tea extract or the high-theobromine tea extract composition is applied to cigarette paper in an amount of 0.05-0.5 g / m2 based on dry matter. 2 .

10. A tobacco product, characterized in that The tobacco product contains the high-theobromine tea extract according to claim 4 or the combination of the high-theobromine tea extract according to claim 5.

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