CN117942611A - Natural tobacco flavor, preparation method thereof and application thereof in heating cigarettes - Google Patents
Natural tobacco flavor, preparation method thereof and application thereof in heating cigarettes Download PDFInfo
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- 239000000796 flavoring agent Substances 0.000 title claims abstract description 67
- 235000019634 flavors Nutrition 0.000 title claims abstract description 67
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 57
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 36
- 238000010438 heat treatment Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 241000208125 Nicotiana Species 0.000 title claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 120
- 238000000605 extraction Methods 0.000 claims abstract description 111
- 239000000284 extract Substances 0.000 claims abstract description 99
- 238000003809 water extraction Methods 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 35
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- 240000002853 Nelumbo nucifera Species 0.000 claims abstract description 27
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims abstract description 27
- 235000006510 Nelumbo pentapetala Nutrition 0.000 claims abstract description 27
- 244000175448 Citrus madurensis Species 0.000 claims abstract description 25
- 235000017317 Fortunella Nutrition 0.000 claims abstract description 25
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 23
- 235000010254 Jasminum officinale Nutrition 0.000 claims abstract description 20
- 239000011812 mixed powder Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 240000005385 Jasminum sambac Species 0.000 claims abstract 3
- 239000004094 surface-active agent Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims 2
- 235000009508 confectionery Nutrition 0.000 abstract description 11
- 230000007794 irritation Effects 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 3
- 244000061176 Nicotiana tabacum Species 0.000 abstract 3
- 239000003205 fragrance Substances 0.000 description 20
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- 229920001213 Polysorbate 20 Polymers 0.000 description 18
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 18
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 18
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- 238000005303 weighing Methods 0.000 description 8
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- 150000001298 alcohols Chemical class 0.000 description 5
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- 238000011156 evaluation Methods 0.000 description 5
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- 244000025254 Cannabis sativa Species 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
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- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 description 3
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Landscapes
- Seasonings (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to the technical field of nature, in particular to a natural tobacco flavor, a preparation method thereof and application thereof in heating cigarettes. The preparation method comprises the following steps: lotus plumule, kumquat skin, white tea and jasmine flower are taken as raw materials to prepare mixed powder; alcohol extraction is carried out on the mixed powder to obtain alcohol extract and alcohol extraction residues; carrying out water extraction on the mixed powder to obtain water extract and water extraction residues; carrying out CO 2 supercritical extraction on the alcohol extraction residues and the water extraction residues, wherein the alcohol extraction liquid and the water extraction liquid are respectively used as entrainers in the extraction process; and (5) performing supercritical extraction to obtain the natural tobacco flavor. The natural tobacco flavor prepared by the method has obvious elegant flavor such as sweet flavor, flower flavor and the like, can increase the sweet flavor, reduce the irritation and obviously improve the coordination of the cigarette flavor when being used for heating cigarettes. The method has low cost and simple operation, does not need to carry out deep optimization on the extraction instrument, and is convenient for realizing industrial production and application.
Description
Technical Field
The invention relates to the technical field of nature, in particular to a natural tobacco flavor, a preparation method thereof and application thereof in heating cigarettes.
Background
The heated cigarette is used as a novel tobacco product, and the working temperature of the heated cigarette is lower than the combustion temperature of the traditional cigarette, so that the generated harmful components are greatly reduced, and the release amount of liquid of the flow measurement smoke and the environmental smoke is greatly reduced. In view of the above advantages, heated cigarettes have been increasingly popular with consumers in recent years. Compared with the traditional cigarettes, the tobacco sections of the heated cigarettes mainly adopt tobacco sheets, the heating temperature is low, the aroma contribution of the spice to the smoke is more obvious, and therefore, the higher requirements of the heated cigarettes on the spice are met.
The traditional extraction method of the natural tobacco flavor mainly comprises an alcohol extraction method and a water extraction method, wherein ethanol or water is mainly used as a solvent to extract the natural tobacco flavor, and then the extract is concentrated. Carbon dioxide supercritical extraction has been developed, and has been increasingly used in recent years because it can retain more natural aroma components with low boiling points. However, the richness and harmony of the aroma obtained by the method when the aroma is used for perfuming cigarettes still remain improved.
Disclosure of Invention
In order to solve or partially solve the problems in the related art, the invention provides a natural tobacco flavor, a preparation method thereof and application thereof in heating cigarettes.
The invention provides a preparation method of a natural tobacco flavor, which comprises the following steps:
Lotus plumule, kumquat skin, white tea and jasmine flower are taken as raw materials to prepare mixed powder;
alcohol extraction is carried out on the mixed powder to obtain alcohol extract and alcohol extraction residues;
carrying out water extraction on the mixed powder to obtain water extract and water extraction residues;
Carrying out CO 2 supercritical extraction on the alcohol extraction residues and the water extraction residues, wherein the alcohol extraction liquid and the water extraction liquid are respectively used as entrainers in the extraction process; and (5) performing supercritical extraction to obtain the natural tobacco flavor.
Further, the mixing proportion of lotus plumule, kumquat skin, white tea and jasmine flower is (1-3): (0.4-2): (0.5-4): 1.
Further, the alcohol extraction is performed under heating conditions, and/or the water extraction is performed under heating conditions.
Further, the heating temperature is 50-65 ℃.
Further, the alcohol extraction is ultrasonic-assisted alcohol extraction, and/or the water extraction is ultrasonic-assisted water extraction.
Further, a surfactant is added in the alcohol extraction process, and/or a surfactant is added in the water extraction process.
Further, the alcohol extract is obtained according to the following method: centrifugally separating the extracted mixture; standing the centrifugally separated liquid at 0-4 ℃ overnight, and taking the upper liquid to obtain an alcohol extract; and/or the number of the groups of groups,
The water extract is obtained according to the following method: centrifugally separating the extracted mixture; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the water extract.
Further, the extraction temperature of the supercritical CO 2 extraction is 40-50 ℃, the extraction pressure is 28-35 MPa, and the extraction time is 1-3 h.
The invention also provides a natural tobacco flavor, which is prepared by the method according to any one of the above.
The invention also provides an application of the natural tobacco flavor in heating cigarettes, which comprises the following steps: the natural tobacco flavor is diluted and sprayed on the tobacco thin surface.
The preparation method of the natural tobacco flavor provided by the invention can have the following beneficial effects:
1. The lotus plumule, kumquat skin, white tea and jasmine flower are used as raw materials, and the lotus plumule and the white tea contain more flavonoid compounds, so that caramel fragrance, sweet fragrance and roast fragrance can be brought to smoke, the fragrance quantity and fragrance quality can be increased, the moist feeling of an oral cavity can be improved, and the irritation can be reduced; the white tea and kumquat contain more volatile aroma components, and can harmonize grass taste and bitter taste of lotus plumule and white tea.
2. In the supercritical extraction process, alcohol extraction residues and water extraction residues are put into an extraction kettle, and alcohol extraction liquid and water extraction liquid are respectively used as entrainers, so that on one hand, the extraction of fragrance components in the solid residues is realized; on the other hand, the purification of the flavor components in the water extract and the alcohol extract is realized, and further, the loss of the flavor components caused by concentration is avoided, so that the flavor components in the obtained natural tobacco flavor are rich, and especially the flavor components with small molecules rich in alcohols and esters are obtained.
3. The natural tobacco flavor prepared by the method has obvious elegant flavor such as sweet flavor and floral flavor, can increase the sweet flavor, reduce the irritation and obviously improve the coordination of the cigarette flavor when being used for heating cigarettes.
4. The method has low cost and simple operation, does not need to carry out deep optimization on the extraction instrument, and is convenient for realizing industrial production and application.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention as claimed.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 is a chromatographic fingerprint of natural perfume extract A prepared in example 1 of the present invention;
FIG. 2 is a chromatographic fingerprint of natural perfume extract B prepared in example 2 of the present invention;
FIG. 3 is a chromatographic fingerprint of natural perfume extract C prepared in example 3 of the present invention;
FIG. 4 is a chromatographic fingerprint of natural perfume extract D prepared in example 4 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
It should be understood that although the terms "first," "second," "third," etc. may be used in this disclosure to describe various information, these information should not be limited to these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the invention. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The embodiment of the invention provides a preparation method of a natural tobacco flavor, which comprises the following steps:
Lotus plumule, kumquat skin, white tea and jasmine flower are taken as raw materials to prepare mixed powder;
alcohol extraction is carried out on the mixed powder to obtain alcohol extract and alcohol extraction residues;
carrying out water extraction on the mixed powder to obtain water extract and water extraction residues;
Carrying out CO 2 supercritical extraction on the alcohol extraction residues and the water extraction residues, wherein the alcohol extraction liquid and the water extraction liquid are respectively used as entrainers in the extraction process; and (5) performing supercritical extraction to obtain the natural tobacco flavor.
In the preparation method provided by the application, lotus plumule, kumquat skin, white tea and jasmine flower are used as raw materials. According to the application, lotus plumule and white tea which contain more flavonoid compounds are taken as raw materials, and preliminary researches show that the substances can generate furan substances and derivatives thereof after combustion and pyrolysis according to the molecular structural characteristics of the flavonoid substances and the strength of acting force between electrons, and the substances are main aroma components in smoke, so that caramel aroma, sweet aroma and roast aroma can be brought to the smoke, the aroma quantity and aroma quality can be increased, and the moist feel of an oral cavity can be improved. The inventor finds that although the spice prepared by taking lotus plumule and white tea as raw materials can enrich the aroma of smoke, the green grass taste and the bitter feel generated by the two raw materials can have adverse effects on the smoke. In order to reduce the influence of bad smoke, the inventor adds white tea and kumquat skin into raw materials, wherein the white tea and kumquat contain more volatile fragrance components, and the green grass taste and the bitter taste of lotus plumule and white tea can be blended. In addition, the volatile flavor components contained in the white tea and the kumquats can be volatilized at low temperature, and are more suitable to be used as flavor components for heating cigarettes.
As a preferable scheme of the embodiment, the mixing proportion of lotus plumule, kumquat skin, white tea and jasmine flower is (1-3): (0.4-2): (0.5-4): 1, the smoke coordination of the raw materials in the proportion is better. More preferably, the mixing ratio of lotus plumule, kumquat skin, white tea and jasmine flower is 1: (0.5-1): (1-1.5): 1. the above mixed powder is preferably prepared as follows: drying plumula Nelumbinis, pericarpium Citri Tangerinae, white tea and flos Jasmini sambac respectively at 40-50deg.C to constant weight, respectively micronizing to obtain single raw material powder with fineness of 10-20 μm, and mixing the single raw material powder according to preset mixing ratio.
After the mixed powder is prepared, a part of the mixed powder is subjected to alcohol extraction, and a part of the mixed powder is subjected to water extraction. The mass ratio of the mixed powder subjected to the alcohol extraction to the mixed powder subjected to the water extraction is preferably 1:1. the above alcohol extraction is preferably performed under heating conditions, and the inventors have found that by heating, more aroma components can be synthesized during the extraction, which have an effect on enriching the aroma and improving the smoke coordination. Preferably, the heating temperature is 50-65 ℃, the heating temperature is close to the heating temperature of the heated cigarettes, and the smoke coordination of the aroma components extracted at the heating temperature is better. In addition, the ethanol extraction is preferably carried out by adopting ultrasonic auxiliary ethanol extraction, more cellulose is contained in lotus plumule, kumquat peel, white tea and jasmine flower, and the ultrasonic auxiliary ethanol extraction is beneficial to fully dissolving out the fragrance components and improves the extraction efficiency. The times of ultrasonic auxiliary extraction are preferably 2-3 times, and the time of each extraction is preferably 20-40 min. More preferably, a surfactant, most preferably Tween20 (polysorbate-20), is added during the alcohol extraction process. The alcohol extraction is preferably performed with 90% alcohol, and the use of 90% alcohol relative to absolute ethanol prevents the actual concentration of the solvent from being inconsistent due to moisture absorption. Similar to the alcohol extraction, the water extraction is also preferably carried out under heating. Further, the water extraction is ultrasonic-assisted water extraction. Surfactants are also preferably added during the water extraction process. The specific preferred heating temperature, number of times of sonication, single extraction time and type of surfactant are the same as those described above for the alcohol extraction. The ratio of the ethanol extract to the water extract is preferably 1g (10 to 20 ml), more preferably 1g (10 to 15 ml).
And respectively collecting an alcohol extract and alcohol extract residues after alcohol extraction of the mixed powder, wherein the alcohol extract contains more weak polar and nonpolar aroma components, and the polar aroma components remain in the alcohol extract residues. The alcohol extract is obtained according to the following method: centrifugally separating the extracted mixture; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the alcohol extract. The alcohol extraction residues are obtained according to the following method: and drying the alcohol extraction residues obtained by centrifugal separation. The aqueous extract contains more polar aroma components, and the weak polar and nonpolar aroma components remain in the alcohol extraction residue. The water extract is obtained according to the following method: centrifugally separating the extracted mixture; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the water extract. The water extraction residues are obtained according to the following method: and drying the water extraction residues obtained by centrifugal separation. It will be appreciated by those skilled in the art that the steps of the above-described alcohol extraction and water extraction are not limited in order.
After the alcohol extract, the alcohol extract residue, the water extract and the water extract residue are obtained, the alcohol extract residue and the water extract residue are combined and then subjected to CO 2 supercritical extraction, and the alcohol extract and the water extract are respectively used as entrainers in the supercritical extraction process; and obtaining the natural tobacco flavor after supercritical extraction. In this embodiment, the alcohol extract and the water extract are used as entrainers, and compared with the traditional mode of using water or ethanol as entrainers, the alcohol extract and the water extract are not added into the extraction kettle as the extractant, and the essence is that the alcohol extract and the water extract are added into the extraction kettle as the purified feed liquid in the mode of entrainers, and in the supercritical CO 2 extraction process: the alcohol extract and the water extract respectively enter the extraction kettle from the entrainer inlet at the upper part at a certain flow rate; the CO 2 fluid is firstly contacted with entrainer (alcohol extract/water extract), in the process, some weak polar and nonpolar and some other volatile flavor components in the entrainer are extracted by CO 2, so that the flavor components in the alcohol extract and the water extract are purified and enter an extraction kettle; then, the CO 2 fluid is contacted with the solid residue at the bottom of the extraction kettle, and natural fragrance components in the alcohol extraction residue and the water extraction residue are extracted. The CO 2 fluid carries the aroma components extracted from the entrainer and the aroma components extracted from the solid residues into a separation kettle, and the aroma components are separated to obtain the natural tobacco flavor
Therefore, in the method provided by the embodiment, the CO 2 supercritical extraction of the solid residue by using the alcohol extract and the water extract as the entrainer has the following effects: on one hand, the extraction of the fragrance components in the solid residues is realized; on the other hand, the purification of the flavor components in the water extract and the alcohol extract is realized, and further, the loss of the flavor components caused by concentration is avoided, so that the flavor components in the obtained natural tobacco flavor are rich, and especially the flavor components with small molecules rich in alcohols and esters are obtained. The extraction temperature of the supercritical CO 2 extraction is preferably 40-50 ℃, the extraction pressure is preferably 28-35 MPa, and the extraction time is preferably 1-3 h. The entrainer can be introduced into the alcohol extract and then into the water extract, or into the water extract and then into the alcohol extract.
From the above, the preparation method of the natural tobacco flavor provided by the embodiment of the invention has the following advantages:
1. The lotus plumule, kumquat skin, white tea and jasmine flower are used as raw materials, and the lotus plumule and the white tea contain more flavonoid compounds, so that caramel fragrance, sweet fragrance and roast fragrance can be brought to smoke, the fragrance quantity and fragrance quality can be increased, the moist feeling of an oral cavity can be improved, and the irritation can be reduced; the white tea and kumquat contain more volatile aroma components, and can harmonize grass taste and bitter taste of lotus plumule and white tea.
2. In the supercritical extraction process, alcohol extraction residues and water extraction residues are put into an extraction kettle, and alcohol extraction liquid and water extraction liquid are respectively used as entrainers, so that on one hand, the extraction of fragrance components in the solid residues is realized; on the other hand, the purification of the flavor components in the water extract and the alcohol extract is realized, and further, the loss of the flavor components caused by concentration is avoided, so that the flavor components in the obtained natural tobacco flavor are rich, and especially the flavor components with small molecules rich in alcohols and esters are obtained.
3. The natural tobacco flavor prepared by the method has obvious elegant flavor such as sweet flavor and floral flavor, can increase the sweet flavor, reduce the irritation and obviously improve the coordination of the cigarette flavor when being used for heating cigarettes.
4. The method has low cost and simple operation, does not need to carry out deep optimization on the extraction instrument, and is convenient for realizing industrial production and application.
The embodiment of the invention also provides the natural tobacco flavor which is prepared according to the method, has obvious elegant flavors such as sweet taste and floral taste, is used for heating cigarettes, can increase the sweet taste, reduces the irritation, and obviously improves the coordination of the cigarette fragrance.
Correspondingly, another embodiment of the invention also provides an application of the natural tobacco flavor in heating cigarettes, which comprises the following steps: the natural tobacco flavor is diluted and sprayed on the tobacco thin surface. Specifically, the natural tobacco flavor can be diluted with 95% ethanol, sprayed into tobacco sheets in a spraying manner according to the addition amount of 5% of the weight of the tobacco sheets, and then rolled into the heated cigarette.
The technical scheme of the invention is further described below with reference to specific examples:
Example 1
(1) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 1:1:1:1 weighing natural perfume powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting 90% ethanol as extractant, extracting at 60 deg.C for 30 min/time, and ultrasonically assisted extracting for 3 times. Centrifugally separating the mixture obtained by extraction, and collecting alcohol extraction residues; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the alcohol extract.
(2) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 1:1:1:1 weighing natural perfume powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting deionized water as extractant, extracting at 60 deg.C for 30 min/time, and ultrasonically assisted extracting for 3 times. Centrifugally separating the mixture obtained by extraction, and collecting water extraction residues; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the water extract.
(3) Drying the alcohol extraction residue after the extraction of the alcohol extract and the water extraction residue after the extraction of the water extract, putting the dried alcohol extraction residue and the water extraction residue into a supercritical extraction kettle, taking CO 2 as an extractant, and separating in the extraction kettle at the temperature of 40-50 ℃ under the extraction pressure of 28-35 MPa for 3 hours. In the process, respectively adding the alcohol extract and the water extract into an extraction kettle from an entrainer inlet, and performing supercritical extraction to obtain an extract which is the natural spice extract A.
(4) Diluting the natural perfume extract A with 95% ethanol, oscillating and extracting, filtering, and performing GC-MS analysis under GC conditions: DB-5MS (60 m x 0.25mm i.d. x 0.25 mu m d.f.) chromatographic column, sample inlet temperature of 250 ℃, split ratio of 15:1, sample feeding amount of 1 mu L, column flow of helium, constant flow mode of 1mL/min, temperature programming: the initial temperature is 50 ℃, after the temperature is kept for 2min, the temperature is increased to 280 ℃ at the speed of 8 ℃/min, and the temperature is kept for 15min; the transmission line temperature was 280 ℃. The chromatographic fingerprint is shown in FIG. 1, and the volatile components in the perfume are shown in Table 1.
(5) According to the addition amount of 5% of the weight of the tobacco sheet, the tobacco sheet is sprayed into the tobacco sheet in a spray mode, and then the tobacco sheet is rolled into a heated cigarette sample A'.
Example 2
(1) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 1:2:4:1 weighing natural spice powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting 90% ethanol as extractant, extracting at 60 deg.C for 30 min/time at a feed-liquid ratio of 1:10 (g/ml), extracting with ultrasonic assistance for 3 times, centrifuging the mixture, and collecting ethanol extraction residue; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the alcohol extract.
(2) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 1:2:4:1 weighing natural perfume powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting deionized water as extractant, extracting at 60 deg.C for 30 min/time, and ultrasonically assisted extracting for 3 times. Centrifugally separating the mixture obtained by extraction, and collecting water extraction residues; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the water extract.
(3) Drying the alcohol extraction residue after the extraction of the alcohol extract and the water extraction residue after the extraction of the water extract, putting the dried alcohol extraction residue and the water extraction residue into a supercritical extraction kettle, taking CO 2 as an extractant, and separating in the extraction kettle at the temperature of 40-50 ℃ under the extraction pressure of 28-35 MPa for 3 hours. In the process, respectively adding the alcohol extract and the water extract into an extraction kettle from an entrainer inlet, and performing supercritical extraction to obtain an extract which is the natural spice extract B.
(4) Diluting the natural perfume extract B with 95% ethanol, oscillating and extracting, filtering, and performing GC-MS analysis under GC conditions: DB-5MS (60 m x 0.25mm i.d. x 0.25 mu m d.f.) chromatographic column, sample inlet temperature of 250 ℃, split ratio of 15:1, sample feeding amount of 1 mu L, column flow of helium, constant flow mode of 1mL/min, temperature programming: the initial temperature is 50 ℃, after the temperature is kept for 2min, the temperature is increased to 280 ℃ at the speed of 8 ℃/min, and the temperature is kept for 15min; the transmission line temperature was 280 ℃. The chromatographic fingerprint is shown in FIG. 2, and the volatile components in the perfume are shown in Table 1.
(5) According to the addition amount of 5% of the weight of the tobacco sheet, the tobacco sheet is sprayed into the tobacco sheet in a spray mode, and then the tobacco sheet is rolled into a heated cigarette sample B'.
Example 3
(1) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 2:1:3:2 weighing natural perfume powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting 90% ethanol as extractant, extracting at 60 deg.C for 30 min/time, and ultrasonically assisted extracting for 3 times. Centrifugally separating the mixture obtained by extraction, and collecting alcohol extraction residues; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the alcohol extract.
(2) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 2:1:3:2 weighing natural spice powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting deionized water as extractant, extracting at 60 ℃ for 30 min/time and 3 times under ultrasonic assistance, centrifuging the mixture, and collecting water extraction residues; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the water extract.
(3) Drying the alcohol extraction residue after the extraction of the alcohol extract and the water extraction residue after the extraction of the water extract, putting the dried alcohol extraction residue and the water extraction residue into a supercritical extraction kettle, taking CO 2 as an extractant, and separating in the extraction kettle at the temperature of 40-50 ℃ under the extraction pressure of 28-35 MPa for 3 hours. In the process, respectively adding the alcohol extract and the water extract into an extraction kettle from an entrainer inlet, and performing supercritical extraction to obtain an extract which is a natural spice extract C.
(4) Diluting the natural perfume extract C with 95% ethanol, oscillating and extracting, filtering, and performing GC-MS analysis under GC conditions: DB-5MS (60 m x 0.25mm i.d. x 0.25 mu m d.f.) chromatographic column, sample inlet temperature of 250 ℃, split ratio of 15:1, sample feeding amount of 1 mu L, column flow of helium, constant flow mode of 1mL/min, temperature programming: the initial temperature is 50 ℃, after the temperature is kept for 2min, the temperature is increased to 280 ℃ at the speed of 8 ℃/min, and the temperature is kept for 15min; the transmission line temperature was 280 ℃. The chromatographic fingerprint is shown in FIG. 3, and the volatile components in the perfume are shown in Table 1.
(5) According to the addition amount of 5% of the weight of the tobacco sheet, the tobacco sheet is sprayed into the tobacco sheet in a spray mode, and then the tobacco sheet is rolled into a heated cigarette sample C'.
Example 4
(1) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 1:3:3:2 weighing natural spice powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting 90% ethanol as extractant, extracting at 60 ℃ for 30 min/time at a feed-liquid ratio of 1:10 (g/ml), extracting for 3 times with ultrasonic assistance, centrifuging the mixture obtained by extraction, and collecting ethanol extraction residues; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the alcohol extract.
(2) According to the mass ratio of lotus plumule, kumquat skin, white tea and jasmine flower of 1:3:3:2 weighing natural spice powder 40g in total, adding 0.2g of surfactant Tween20 (polysorbate-20), selecting deionized water as extractant, extracting at 60 ℃ for 30 min/time and 3 times under ultrasonic assistance, centrifuging the mixture, and collecting water extraction residues; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the water extract.
(3) Drying the alcohol extraction residue after the extraction of the alcohol extract and the water extraction residue after the extraction of the water extract, putting the dried alcohol extraction residue and the water extraction residue into a supercritical extraction kettle, taking CO 2 as an extractant, and separating in the extraction kettle at the temperature of 40-50 ℃ under the extraction pressure of 28-35 MPa for 3 hours. In the process, respectively adding the alcohol extract and the water extract into an extraction kettle from an entrainer inlet, and performing supercritical extraction to obtain an extract which is the natural spice extract D.
(4) Diluting the natural perfume extract D with 95% ethanol, oscillating and extracting, filtering, and performing GC-MS analysis under GC conditions: DB-5MS (60 m x 0.25mm i.d. x 0.25 mu m d.f.) chromatographic column, sample inlet temperature of 250 ℃, split ratio of 15:1, sample feeding amount of 1 mu L, column flow of helium, constant flow mode of 1mL/min, temperature programming: the initial temperature is 50 ℃, after the temperature is kept for 2min, the temperature is increased to 280 ℃ at the speed of 8 ℃/min, and the temperature is kept for 15min; the transmission line temperature was 280 ℃. The chromatographic fingerprint is shown in FIG. 4, and the volatile components in the perfume are shown in Table 1.
(5) According to the addition amount of 5% of the weight of the tobacco sheet, the tobacco sheet is sprayed into the tobacco sheet in a spray mode, and then the tobacco sheet is rolled into a heated cigarette sample D'.
Example 5
The difference from example 1 is that both the step (1) and the step (2) are carried out at normal temperature, and the rest is the same as example 1, to obtain a natural perfume extract E, and the volatile components in the perfume are listed in Table 1.
TABLE 1 analysis of volatile components in fragrances
| Numbering device | A | B | C | D | E |
| Alcohols | 2 | 3 | 7 | 4 | 2 |
| Esters of | 5 | 4 | 5 | 6 | 2 |
| Pyridines/pyrroles | 2 | 1 | 3 | 3 | 1 |
| Furanones | 3 | 2 | 4 | 4 | 2 |
| Others | 5 | 4 | 7 | 5 | 8 |
| Totals to | 17 | 14 | 26 | 22 | 15 |
As can be seen from Table 1, the natural perfume prepared in the examples of the present invention is rich in volatile components of alcohols, esters, pyridines/pyrroles and furanones. And, the heating in the alcohol extraction and the water extraction helps to synthesize more aroma components.
The heated cigarette samples prepared in examples 1 to 4 were subjected to sensory evaluation by referring to "YC/T497-2014 method for sensory evaluation of style of chinese cigarette for cigarettes", 0 for none, 1 for minute, 2 for minute, 3 for intense, wherein the minimum integral unit was 0.5 minutes. The sensory evaluation results are shown in tables 2 to 4.
Table 2 table of the odor index of fragrance style
TABLE 3 fragrance style evaluation index scoring table
TABLE 4 flavor smoke characteristic index evaluation score
As can be seen from tables 2 to 4: the natural spice prepared by the embodiment of the invention has obvious elegant aroma such as sweet aroma and floral aroma, can increase the sweet aroma, reduce the irritation and obviously improve the coordination of the aroma of the cigarettes when being applied to heating the cigarettes.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. The terminology used herein was chosen in order to best explain the principles of the embodiments, the practical application, or the improvement of technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. The preparation method of the natural tobacco flavor is characterized by comprising the following steps:
Lotus plumule, kumquat skin, white tea and jasmine flower are taken as raw materials to prepare mixed powder;
alcohol extraction is carried out on the mixed powder to obtain alcohol extract and alcohol extraction residues;
carrying out water extraction on the mixed powder to obtain water extract and water extraction residues;
Carrying out CO 2 supercritical extraction on the alcohol extraction residues and the water extraction residues, wherein the alcohol extraction liquid and the water extraction liquid are respectively used as entrainers in the extraction process; and (5) performing supercritical extraction to obtain the natural tobacco flavor.
2. The preparation method of claim 1, wherein the mixing ratio of lotus plumule, kumquat skin, white tea and jasmine flower is (1-3): (0.4-2): (0.5-4): 1.
3. The preparation method according to claim 2, wherein the alcohol extraction is performed under heating conditions and/or the water extraction is performed under heating conditions.
4. A method of preparation according to claim 3 wherein the heating is at a temperature of 50 ℃ to 65 ℃.
5. A method of preparation according to claim 3, wherein the alcohol extraction is an ultrasound-assisted alcohol extraction and/or the water extraction is an ultrasound-assisted water extraction.
6. A method of preparation according to claim 3, wherein a surfactant is added during the alcohol extraction and/or a surfactant is added during the water extraction.
7. The preparation method according to claim 5, wherein the alcohol extract is obtained by the following method: centrifugally separating the extracted mixture; standing the centrifugally separated liquid at 0-4 ℃ overnight, and taking the upper liquid to obtain an alcohol extract; and/or the number of the groups of groups,
The water extract is obtained according to the following method: centrifugally separating the extracted mixture; and (3) placing the centrifugally separated liquid in an environment of 0-4 ℃ for standing overnight, and taking the upper liquid to obtain the water extract.
8. The method according to claim 5, wherein the supercritical CO 2 extraction is performed at a temperature of 40-50deg.C under a pressure of 28-35 MPa for 1-3 h.
9. A natural tobacco flavour, characterized in that it is prepared according to the method of any one of claims 1 to 8.
10. Use of a natural tobacco flavor according to claim 9 for heating cigarettes, comprising: the natural tobacco flavor of claim 9 is diluted and sprayed onto the tobacco sheet surface.
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