Winter flower essential oil, preparation method thereof, cigarette blasting bead and aerosol generating article

Abstract

Provided are a radix codonopsitis essential oil and a preparation method thereof, a smoking burst bead, and an aerosol generating article. The radix codonopsitis essential oil is prepared by a cell wall crushing technique, enzymatic hydrolysis of the cell wall, a low-temperature supercritical extraction process, and targeted selection of an essential oil solvent, and the radix codonopsitis essential oil obtained has a distinct spicy and herbal flavor, has a high yield, and has high quality. The method is easy to implement, can effectively solve the problem of loss of temperature-sensitive aroma of the radix codonopsitis in a water vapor distillation process, is relatively easy to apply to burst bead dripping, and has strong practicability.

Description

Technical Field

[0001] This patent relates to the field of tobacco flavoring extraction technology, specifically to coltsfoot flower essential oil and its preparation method, tobacco flavoring beads and aerosol products. Background Technology

[0002] Coltsfoot (Tussilago farfara) is a perennial herb belonging to the genus Tussilago in the family Asteraceae. Its flower buds, used medicinally, are called coltsfoot flowers, named for their delicate blooming amidst winter snow. As a traditional Chinese medicine, coltsfoot flowers are pungent and slightly bitter in taste, warm in nature, and enter the lung meridian. They have the effects of moistening the lungs, lowering qi, relieving cough, and resolving phlegm. Modern research shows that coltsfoot flowers contain various active ingredients such as volatile oils, sesquiterpenes, and flavonoids. The volatile oil components give it a unique pungent and herbal aroma.

[0003] Based on the efficacy and aroma characteristics of coltsfoot flowers, they have been developed into a tobacco flavoring and applied to cigarette flavoring capsules. This not only gives cigarette products a unique spicy and herbal aroma, but also allows them to exert their throat-soothing and lung-moistening effects, showing broad application prospects.

[0004] Currently, the main methods for extracting plant essential oils include steam distillation, organic solvent extraction, and pressing. Among these, steam distillation is the most traditional and commonly used method for extracting volatile oils from plants. However, steam distillation has several technical drawbacks when applied to the extraction of coltsfoot flower essential oil.

[0005] First, steam distillation requires prolonged reflux heating at high temperatures. Many key aroma components in coltsfoot, especially the terpenes that impart its spicy and herbal notes, such as carene, eugenol, β-caryophyllene, and β-bisabolene, are heat-sensitive. Under high temperatures, these components are prone to oxidation, polymerization, and hydrolysis, leading to a significant loss of aroma components. The resulting coltsfoot essential oil is watery and has a weak herbal and spicy aroma, failing to meet the requirements of high-quality cigarette products.

[0006] Secondly, steam distillation has low extraction efficiency, with an essential oil yield typically less than 1%, leaving a large amount of aromatic components in the residue, resulting in a serious waste of resources. Furthermore, coltsfoot essential oil extracted by steam distillation often contains a high water content, which not only affects the stability of the essential oil but also causes inconvenience for its subsequent storage and application.

[0007] To address the aforementioned shortcomings of steam distillation, researchers attempted to extract coltsfoot flower essential oil using organic solvent extraction. While organic solvent extraction can improve extraction efficiency to some extent, this method also has significant limitations.

[0008] First, the use of organic solvents poses a safety risk due to solvent residue, especially when applied to products like cigarette flavoring capsules that come into direct contact with the consumer's mouth, where the safety requirements for solvents are extremely stringent. Second, organic solvent extraction methods typically extract a significant amount of impurities, such as waxes, pigments, and fatty acids. The presence of these impurities affects the purity and aroma quality of the essential oils, requiring tedious impurity removal processes, which increases the complexity and cost of the process.

[0009] Supercritical fluid extraction (SFE) is a novel green extraction technology that has emerged in recent years. Supercritical CO2 extraction, in particular, has been widely used in the field of natural product extraction due to its advantages such as low extraction temperature, no solvent residue, and adjustable selectivity. However, directly applying supercritical CO2 extraction to the extraction of coltsfoot flower essential oil still faces some technical challenges.

[0010] On the one hand, the cell walls of coltsfoot flowers are dense, composed of cellulose, hemicellulose, and lignin, forming a physical barrier to the release of intracellular contents. Supercritical CO2 alone cannot completely destroy the cell walls, limiting extraction efficiency. On the other hand, the target aroma components in coltsfoot flowers are complex, including both non-polar terpenes and relatively polar oxygenated derivatives. Supercritical CO2 alone is insufficient for extracting certain polar components, requiring the use of entrainers. The type and dosage of entrainers, as well as the optimization of extraction parameters, all necessitate systematic research and screening tailored to the characteristics of coltsfoot flowers.

[0011] Furthermore, directly applying the obtained supercritical fluid extract of Coltsfoot flower to the preparation of cigarette flavor capsules presents a processing compatibility issue. Supercritical fluid extracts are typically viscous pastes or semi-fluids with poor flowability, making them difficult to use directly in high-speed flavor capsule dispensing equipment.

[0012] Meanwhile, the extract may contain trace amounts of insoluble particles, which can clog the precision drip nozzles during the dripping process, affecting the continuity of production and the stability of the product. Therefore, how to properly post-process the supercritical extract of Coltsfoot Flower to give it good flowability and purity to meet the requirements of industrial-scale production of popping beads is also a technical problem that urgently needs to be solved in this field.

[0013] In summary, current technologies lack a method for efficiently extracting the pungent and herbal aroma components from coltsfoot flower, while achieving high yield, good quality, and suitability for the industrial production of coltsfoot flower essential oil for cigarette flavor capsules. Therefore, developing a new process for preparing coltsfoot flower essential oil that effectively enhances its herbal aroma characteristics, retains a greater amount of aromatic substances, and meets the demand for high-aroma, high-quality coltsfoot flower essential oil in cigarette flavor capsule production has significant practical importance and application value. Summary of the Invention

[0014] This patent aims to solve the technical problems of existing methods for preparing coltsfoot flower essential oil, such as significant loss of aroma components, low yield, poor product quality, and difficulty in adapting to the industrial production of tobacco flavoring capsules. This patent provides the following technical solution: In a first aspect, a method for preparing coltsfoot flower essential oil is provided, the method comprising the following steps: Step S1: pre-treating coltsfoot flower raw material by cell wall breaking and enzymatic hydrolysis to obtain coltsfoot flower enzymatic hydrolysate wet material; Step S2: supercritical extraction of coltsfoot flower enzymatic hydrolysate wet material to obtain coltsfoot flower supercritical extract; Step S3: dissolving and filtering coltsfoot flower supercritical extract to obtain coltsfoot flower essential oil.

[0015] Further, step S1 includes the following steps: Step S11: The coltsfoot flower raw material is pulverized to obtain coltsfoot flower powder; Step S12: The coltsfoot flower powder is mixed with cellulase and buffer solution, stirred evenly, and allowed to stand to obtain coltsfoot flower enzymatic hydrolysate wet material.

[0016] Furthermore, in step S11, the rotation speed of the cell wall breaking pulverizer is 6000~10000 r / min; the particle size of the coltsfoot flower powder is 60~100 mesh; in step S12, the mass of cellulase is 1~5% of the mass of the coltsfoot flower powder; and the standing time is more than two days.

[0017] Further, step S2 includes the following steps: Step S21: The wet material of Tussilago farfara enzymatic hydrolysis is loaded into the extraction instrument and the extraction solvent and entrainer are injected and then pressurized to a supercritical state; Step S22: Tussilago farfara intermediate extract is extracted from the wet material of Tussilago farfara enzymatic hydrolysis under supercritical state; Step S23: Tussilago farfara intermediate extract is separated from the extraction solvent to obtain Tussilago farfara supercritical extract.

[0018] Furthermore, in step S21, the extraction solvent is carbon dioxide; the extraction pressure is 20~25MPa; the entrainer is anhydrous ethanol; the mass ratio of the entrainer to the wet hydrolysed coltsfoot flower is 1:16~1:20; the separation pressure is 3~7MPa; the extraction temperature is 40~45℃; and the extraction time is 2~3h.

[0019] Furthermore, in step S3, the supercritical extract of coltsfoot is dissolved in a non-polar solvent; the supercritical extract of coltsfoot is filtered through a ceramic membrane.

[0020] Furthermore, the non-polar solvent is edible olive oil and / or ODO; the pore size of the ceramic membrane is 0.8 μm.

[0021] Secondly, a coltsfoot flower essential oil, which is prepared by the above-mentioned preparation method.

[0022] Thirdly, a tobacco flavoring capsule, which includes the aforementioned coltsfoot essential oil.

[0023] Fourthly, an aerosol-generating product, comprising the aforementioned smoke capsules.

[0024] This patent has the following beneficial effects: 1. This invention provides a method for preparing coltsfoot flower essential oil, as well as a cigarette-grade popping bead and aerosol product. The method involves pulverizing the oil using cell wall breaking technology, enzymatically hydrolyzing the cell walls, employing low-temperature supercritical extraction, and selectively choosing the appropriate essential oil solvent. This yields coltsfoot flower essential oil with distinct pungent and herbal flavor characteristics, achieving a high yield and quality. The method is practical and easy to implement, effectively addressing the issue of aroma loss due to temperature sensitivity in coltsfoot flower produced by steam distillation. It is readily applicable to popping bead production, demonstrating strong practicality and ease of use.

[0025] 2. This patent effectively avoids the thermal degradation of aroma components caused by high temperatures in traditional steam distillation by employing low-temperature supercritical CO2 extraction technology. Headspace-gas chromatography analysis shows that the key aroma components in the coltsfoot flower essential oil prepared using this patented method are excellently preserved. Specifically, the total relative percentage content of the four main spicy and herbal characteristic components—carene, eugenol, β-caryophyllene, and β-bisabolene—is as high as over 50%. This high retention of components gives the coltsfoot flower essential oil prepared by this patent a distinct and pure spicy and herbal aroma, with prominent and easily identifiable aroma characteristics, providing a unique sensory experience for cigarette products. In contrast, the coltsfoot flower essential oil prepared by steam distillation in the comparative example suffers significant loss of these key aroma components due to high-temperature degradation, resulting in a significant decline in aroma quality.

[0026] 3. This patent achieves a breakthrough improvement in the yield of coltsfoot flower essential oil through the synergistic effect of cell wall disruption enzymatic hydrolysis pretreatment and supercritical CO2 extraction. Data from Examples 1-4 show that the yield of coltsfoot flower essential oil is close to 40%. In contrast, the yield of the comparative example using traditional steam distillation is only 0.4%. This significant improvement stems from two aspects: First, the cell wall disruption enzymatic hydrolysis pretreatment in step S1, through high-speed cell wall disruption pulverization, greatly increases the specific surface area of ​​the material. At the same time, cellulase hydrolyzes the cellulose skeleton of the plant cell wall in a suitable pH buffer environment, destroying the physical barrier that hinders the release of contents, thus fully exposing the essential oil components within the cells. Second, supercritical CO2, under optimized process parameters, efficiently extracts these exposed components. The synergistic effect of physical cell wall disruption and biological enzymatic hydrolysis, coupled with optimized extraction conditions, jointly achieves efficient extraction of coltsfoot flower essential oil, significantly improving raw material utilization and reducing production costs.

[0027] 4. Step S3 of this patent solves the processing compatibility problem of directly applying the supercritical fluid extract of coltsfoot flower to the preparation of popping beads through dissolution and filtration. First, a non-polar solvent is used to dissolve and dilute the viscous supercritical fluid extract of coltsfoot flower, transforming it into a homogeneous liquid with good flowability. ODO, as a food-grade, odorless, low-viscosity oily solvent, has good compatibility with the non-polar terpenoid components in coltsfoot flower essential oil and is odorless itself, so it will not interfere with or change the characteristic aroma of coltsfoot flower essential oil. The dissolved essential oil system is stable and can meet the material flowability requirements of high-speed popping bead dripping equipment. Second, a ceramic membrane with a pore size of 0.8μm is used to filter the dissolved essential oil, effectively removing micron-sized insoluble particles. If these particles are not removed, they may clog the precision dripping nozzle during the popping bead dripping process, causing production interruption, or precipitate during downstream storage, affecting the product appearance and quality. The essential oil filtered by the ceramic membrane has high purity, the dripping process is smooth, and the quality of the popping bead product is stable.

[0028] 5. This patent successfully applies the traditional Chinese medicinal herb coltsfoot flower to modern aerosol-generated products, endowing cigarette products with a unique health concept and sensory experience. Coltsfoot flower itself possesses lung-moistening, cough-relieving, and phlegm-reducing effects, which are delivered to consumers through the form of smoke, allowing cigarette products to provide satisfaction while also offering a certain throat-soothing and lung-moistening effect, thus enhancing the product's added value and market competitiveness. Simultaneously, the unique pungent and herbal aroma of coltsfoot flower enriches the aroma layers of cigarettes, providing consumers with a new sensory experience. Attached Figure Description

[0029] To more clearly illustrate the technical solutions of the embodiments of this patent, the drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this patent and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

[0030] Figure 1 This is a flowchart of the preparation method in this patent; Figure 2 This is the headspace-gas chromatography total ion chromatogram of the winterflower essential oil in Example 1 of this patent. Detailed Implementation

[0031] The detailed features and advantages of this patent are described below in the specific embodiments. The content is sufficient to enable any person skilled in the art to understand the technical content of this patent and implement it accordingly. Based on the specification, claims and drawings disclosed in this specification, a person skilled in the art can easily understand the related objectives and advantages of this patent.

[0032] It should be noted that in this specification, similar reference numerals and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0033] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this patent belongs. The terminology used herein in the specification of this patent is for the purpose of describing particular embodiments only and is not intended to be limiting of this patent. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0034] To make the objectives, technical solutions, and advantages of this patent clearer, the embodiments of this patent will be described in further detail below with reference to the accompanying drawings.

[0035] Please refer to Figure 1 A method for preparing coltsfoot flower essential oil, the method comprising the following steps: Step S1: Coltsfoot flower raw material is subjected to cell wall breaking enzymatic hydrolysis pretreatment to obtain coltsfoot flower enzymatic hydrolysate wet material.

[0036] Furthermore, step S1 includes the following steps: Step S11: The coltsfoot flower raw material is pulverized to obtain coltsfoot flower powder.

[0037] Specifically, the raw material of coltsfoot flower is weighed out. The raw material of coltsfoot flower is a dried medicinal material. After setting the blade speed, the raw material of coltsfoot flower is added and physically crushed to obtain coltsfoot flower powder.

[0038] In step S11, the rotation speed of the cell wall breaking pulverizer is 6000~10000 r / min; the particle size of the coltsfoot flower powder is 60~100 mesh.

[0039] Step S12: Mix the coltsfoot flower powder with cellulase and buffer solution, stir evenly, and let stand to obtain coltsfoot flower enzymatic hydrolysate wet material.

[0040] Specifically, coltsfoot powder, cellulase, and Tris-HCl 6.0 buffer are mixed and stirred until homogeneous. The mixture is then allowed to stand until the cellulase completely destroys the cell walls of the coltsfoot plant in order to facilitate extraction.

[0041] In step S12, the mass of cellulase is 1-5% of the mass of coltsfoot flower powder; the standing time is more than two days.

[0042] Step S2: Supercritical extraction is performed on the wet material of coltsfoot enzymatic hydrolysis to obtain coltsfoot supercritical extract.

[0043] Furthermore, step S2 includes the following steps: Step S21: Load the wet material of Tussilago farfara enzymatic hydrolysis into the extractor, inject the extraction solvent and entrainer, and pressurize it to a supercritical state.

[0044] Step S22: Extract the intermediate extract of coltsfoot flower from wet enzymatic hydrolysis material under supercritical conditions.

[0045] Step S23: After separating the coltsfoot flower intermediate extract from the extraction solvent, the supercritical extract of coltsfoot flower is obtained.

[0046] Specifically, the wet material of coltsfoot flower enzymatically hydrolyzed is placed in a material bag and then placed in the stainless steel material tank of a supercritical CO2 extractor. The parameters of the supercritical CO2 extractor are set, such as extraction vessel pressure, extraction temperature, separation vessel pressure, separation temperature, and extraction time. In the sealed extraction vessel, CO2 is injected and pressurized to a supercritical state, while an entrainer is added to enhance the extraction capacity. The supercritical CO2 fluid penetrates the raw material, dissolving the essential oil components in the coltsfoot flower. The CO2 fluid containing dissolved essential oil enters the separation vessel. By reducing the pressure and / or adjusting the temperature, the CO2 is converted back to ordinary gas, and its dissolving capacity for essential oil decreases sharply. The essential oil thus remains at the bottom of the separation vessel, while the vaporized CO2 is recycled or discharged, ultimately yielding a supercritical extract of coltsfoot flower essential oil.

[0047] In step S21, the extraction solvent is carbon dioxide; the extraction pressure is 20-25 MPa; the entrainer is anhydrous ethanol; the ratio of the entrainer to the coltsfoot flower raw material is 1:16-1:20; the separation pressure is 3-7 MPa; the extraction temperature is 40-45℃; and the extraction time is 2-3 h.

[0048] Step S3: Dissolve and filter the supercritical fluid extract of coltsfoot flower to obtain coltsfoot flower essential oil.

[0049] The supercritical extract of coltsfoot flower was dissolved in a non-polar solvent; the supercritical extract of coltsfoot flower was filtered through a ceramic membrane.

[0050] Specifically, the non-polar solvent is edible olive oil and / or glyceryl caprylate (ODO); the ceramic membrane has a pore size of 0.8 μm.

[0051] A coltsfoot flower essential oil, which is prepared by the above-described method.

[0052] A type of cigarette flavor capsule, comprising the aforementioned coltsfoot flower essential oil. Specifically, coltsfoot flower essential oil significantly enhances the spicy and herbal aroma, provides a good soothing effect on the throat and lungs, and effectively improves the quality of cigarette products.

[0053] An aerosol-generating product, comprising the aforementioned smoke capsules.

[0054] Table 1 lists the names of the raw materials and their suppliers used in the following examples and comparative examples.

[0055] Table 1. Names of Raw Materials and Suppliers

[0056] Example 1

[0057] S11: Weigh 100g of dried coltsfoot flower medicinal material, perform pretreatment with cell wall breaking technology, set the blade speed to 8000r / min to pulverize to 70 mesh, and obtain coltsfoot flower powder.

[0058] S12: Add 0.1 g of cellulase and 3 ml of Tris-HCl 6.0 buffer to the coltsfoot flower powder, mix and stir well, and let stand for 5 days to obtain the wet coltsfoot flower enzymatic hydrolysate for later use. The mass of cellulase is 1‰ of the mass of coltsfoot flower powder.

[0059] S21: The wet coltsfoot flower enzymatic hydrolysate mixed with cellulase obtained in step S12 is placed into a material bag and then placed in the stainless steel material container of a supercritical CO2 extractor. The extraction solvent is carbon dioxide, the entrainer is anhydrous ethanol, and the mass ratio of the entrainer to the wet coltsfoot flower enzymatic hydrolysate is 1:16.

[0060] S22: Set the parameters of the supercritical CO2 extractor to start extraction. The extraction vessel pressure is 25 MPa, the extraction temperature is 40℃, the separation vessel pressure is 6.0 MPa, the separation temperature is 45℃, and the extraction time is 2.5 h. The intermediate extract of coltsfoot flower is extracted from the wet material of enzymatic hydrolysis under supercritical conditions.

[0061] S23: Separate the intermediate extract of coltsfoot flower from the extraction solvent to obtain 3.88g of supercritical extract of coltsfoot flower.

[0062] S3: Dissolve the coltsfoot supercritical extract obtained in step S23 in 11 times its weight of edible olive oil, stir well, and then filter through a 0.8μm ceramic membrane to obtain 41.27g of coltsfoot essential oil, with an essential oil yield of 41.27% (essential oil weight / coltsfoot raw material weight × 100%).

[0063] Please refer to Figure 2 The coltsfoot flower essential oil prepared in this embodiment was subjected to headspace-gas chromatography for chemical composition analysis. The total ion chromatogram is shown below. Figure 2 As shown in Table 2, the analysis results are as follows.

[0064] Example 2

[0065] This embodiment provides a method for preparing coltsfoot flower essential oil, including the following steps: S11: Weigh 110g of dried coltsfoot flower medicinal material, perform pretreatment with cell wall breaking technology, set the blade speed to 9000r / min to pulverize to 60 mesh, and obtain coltsfoot flower powder.

[0066] S12: Add 0.1 g of cellulase and 4 ml of Tris-HCl 6.0 buffer to the coltsfoot flower powder, mix and stir well, and let stand for 6 days to obtain the wet coltsfoot flower enzymatic hydrolysate for later use. The mass of cellulase is 0.9‰ of the mass of coltsfoot flower powder.

[0067] S21: The wet hydrolysed coltsfoot flower obtained in step S12 is placed into a material bag and then placed in the stainless steel material container of a supercritical CO2 extractor. The extraction solvent is carbon dioxide, the entrainer is anhydrous ethanol, and the mass ratio of the entrainer to the wet hydrolysed coltsfoot flower is 1:18.

[0068] S22: Set the parameters of the supercritical CO2 extractor to start extraction. The extraction vessel pressure is 20 MPa, the extraction temperature is 42℃, the separation vessel pressure is 7.0 MPa, the separation temperature is 45℃, and the extraction time is 3.0 h. The intermediate extract of coltsfoot flower is extracted from the wet material of enzymatic hydrolysis under supercritical conditions.

[0069] S23: Separate the intermediate extract of coltsfoot flower from the extraction solvent to obtain 4.31g of supercritical extract of coltsfoot flower.

[0070] S3: Dissolve the coltsfoot supercritical extract obtained in step S23 in 11 times its mass of ODO, stir well, and then filter through a 0.8μm ceramic membrane to obtain 45.26g of coltsfoot essential oil, with an essential oil yield of 41.14%.

[0071] Example 3

[0072] This embodiment provides a method for preparing coltsfoot flower essential oil, including the following steps: S11: Weigh 130g of dried coltsfoot flower material, perform pretreatment with cell wall breaking technology, set the blade speed to 10000r / min to pulverize to 80 mesh, and obtain coltsfoot flower powder.

[0073] S12: Add 0.15 g of cellulase and 6 ml of Tris-HCl 6.0 buffer to the coltsfoot flower powder, mix and stir well, and let stand for 7 days to obtain the wet coltsfoot flower enzymatic hydrolysate for later use. The mass of cellulase is 1.15‰ of the mass of coltsfoot flower powder.

[0074] S21: The wet hydrolysed coltsfoot flower obtained in step S12 is placed into a material bag and then placed in the stainless steel material container of a supercritical CO2 extractor. The extraction solvent is carbon dioxide, the entrainer is anhydrous ethanol, and the mass ratio of the entrainer to the wet hydrolysed coltsfoot flower is 1:20.

[0075] S22: Set the parameters of the supercritical CO2 extractor to start extraction. The extraction vessel pressure is 25 MPa, the extraction temperature is 43℃, the separation vessel pressure is 6.0 MPa, the separation temperature is 47℃, and the extraction time is 3.0 h. The intermediate extract of coltsfoot flower is extracted from the wet material of coltsfoot flower enzymatic hydrolysis under supercritical conditions.

[0076] S23: Separate the intermediate extract of coltsfoot flower from the extraction solvent to obtain 4.69g of supercritical extract of coltsfoot flower.

[0077] S3: Dissolve the coltsfoot supercritical extract obtained in step S23 in 10 times its weight of a mixture of ODO and edible olive oil (mass ratio 9:1), stir well, and then filter through a 0.8μm ceramic membrane to obtain 43.77g of coltsfoot essential oil, with an essential oil yield of 33.67%.

[0078] Example 4

[0079] This embodiment provides a method for preparing coltsfoot flower essential oil, including the following steps: S11: Weigh 120g of dried coltsfoot flower material, perform pretreatment with cell wall breaking technology, set the blade speed to 9000r / min to pulverize to 70 mesh, and obtain coltsfoot flower powder.

[0080] S12: Add 0.2 g of cellulase and 4 ml of Tris-HCl 6.0 buffer to the coltsfoot flower powder, mix and stir well, and let stand for 6 days to obtain the wet coltsfoot flower enzymatic hydrolysate for later use. The mass of cellulase is 1.67‰ of the mass of coltsfoot flower powder.

[0081] S21: The wet hydrolysed coltsfoot flower obtained in step S12 is placed into a material bag and then placed in the stainless steel material container of a supercritical CO2 extractor. The extraction solvent is carbon dioxide, the entrainer is anhydrous ethanol, and the mass ratio of the entrainer to the wet hydrolysed coltsfoot flower is 1:17.

[0082] S22: Set the parameters of the supercritical CO2 extractor to start extraction. The extraction vessel pressure is 24 MPa, the extraction temperature is 41℃, the separation vessel pressure is 5.5 MPa, the separation temperature is 46℃, and the extraction time is 3.0 h. The intermediate extract of coltsfoot flower is extracted from the wet material of enzymatic hydrolysis under supercritical conditions.

[0083] S23: Separate the intermediate extract of coltsfoot flower from the extraction solvent to obtain 5.13g of supercritical extract of coltsfoot flower.

[0084] S3: Dissolve the coltsfoot supercritical extract obtained in step S23 in 12 times its mass of ODO, stir well, and then filter through a 0.8μm ceramic membrane to obtain 52.11g of coltsfoot essential oil, with an essential oil yield of 43.42%.

[0085] Comparative Example

[0086] This comparative example uses the traditional steam distillation method to prepare coltsfoot flower essential oil, including the following steps: (1) Weigh 300g of raw coltsfoot flower (uncrushed) and place the coltsfoot flower in a 5000mL round-bottom flask; (2) After adding 3600g of deionized water to the round-bottom flask, reflux heating at 100°C for about 4.3 hours using an electric heating mantle. (3) After cooling, the coltsfoot essential oil and water in the oil-water separator separated into layers, yielding 1.2g of coltsfoot essential oil with an essential oil yield of 0.4%.

[0087] Experimental Example 1

[0088] The coltsfoot essential oil prepared in Example 1 was used to prepare burst beads using a conventional droplet-making process in the art. Specifically, the coltsfoot essential oil was used as the core liquid and dripped into a coagulation bath through a coaxial dropper to form burst beads. After collection, the beads were washed, dried, and screened to obtain cigarette burst beads containing coltsfoot essential oil. The prepared coltsfoot burst beads were then implanted into cigarette filter rods using conventional methods to obtain an aerosol-generated product, designated A1.

[0089] Experiment Example 2

[0090] The coltsfoot flower essential oil prepared in Example 3 was used to prepare burst beads using the same droplet preparation process as in Example 1. The prepared coltsfoot flower burst beads were then inserted into a cigarette filter rod to obtain an aerosol-generated product, designated A2.

[0091] Experimental Example 3

[0092] The coltsfoot flower essential oil prepared in the comparative example was first diluted 20 times with ODO, and then the burst beads were prepared using the same burst bead dripping process as in Experimental Example 1. The prepared coltsfoot flower burst beads were implanted into a cigarette filter rod to obtain an aerosol-generated product, numbered D1.

[0093] Chemical composition analysis of coltsfoot flower essential oil

[0094] The coltsfoot flower essential oil from Example 1 was used for headspace-gas chromatography chemical composition analysis. The total ion chromatogram is shown below. Figure 2 As shown in Table 2, the analysis results are as follows.

[0095] Table 2. Headspace-gas chromatography analysis results of Example 1

[0096] Conclusion: As can be seen from the headspace-gas chromatography analysis results in Table 2, the key aroma components in the coltsfoot flower essential oil prepared by the method of this patent were well preserved and enriched.

[0097] Among them, the relative percentage of carene is as high as 27.55%, making it the main component; the content of β-bisabolene reaches 14.42%, making it the second main component; the content of β-caryophyllene is 5.75%; and the content of eugenol is 4.19%.

[0098] Carene has a unique pine-like aroma and spicy undertone, and is an important source of the spicy characteristics of coltsfoot flower; eugenol presents a rich clove spiciness and is the core contributor to the spicy aroma; β-caryophyllene has spicy and woody notes, which can enrich the layers of aroma; β-bisabolene has a warm herbal aroma and is the key component of herbal aroma characteristics.

[0099] The total relative percentage of these four main spicy and herbal aroma components is as high as 52.91%, exceeding 50%. In addition, components such as D-limonene (1.75%) and anethole (0.52%) also contribute to the aroma. These key aroma components in high content together constitute the unique and rich spicy and herbal aroma of coltsfoot flower essential oil.

[0100] Compared to the high-temperature steam distillation method used in the comparative example, the low-temperature supercritical CO2 extraction process of this patent is crucial for avoiding the degradation and loss of these heat-sensitive terpenoid components, resulting in a purer and stronger aroma profile in the final product, thus producing unexpected technical effects. This analytical result, at the chemical composition level, confirms the significant advantage of this patented method in preserving the characteristic aroma components of coltsfoot flower, providing a solid material basis for the coltsfoot flower essential oil prepared in this patent to provide unique spiciness and herbal aroma to cigarette products.

[0101] Atmospheric evaluation experiment

[0102] Sensory evaluation experiments were conducted on experimental examples A1 and A2, and comparative example D1, using a 100-point scale. Evaluation indicators included aroma, smoke, strength, irritation, aftertaste, and evenness, with maximum scores of 25, 20, 10, 20, 15, and 10 respectively, for a total score of 100. Higher scores for each indicator indicated better vaping experience. Three batches of samples were randomly selected for each evaluation item, and nine judges evaluated and scored the samples. The average score was then calculated. The sensory quality evaluation results are shown in Table 3 below.

[0103] Table 3 Sensory evaluation results of experimental examples A1, A2 and comparative example D1

[0104] Conclusion: As can be seen from the sensory evaluation results in Table 3, the cigarette flavoring beads (experimental examples A1 and A2) made from coltsfoot essential oil prepared by the method of this patent have significantly better sensory quality than comparative example D1 after being added to the cigarette filter rod.

[0105] In terms of aroma, A1 scored 22 points and A2 scored 23 points, both significantly higher than D1's 21 points, an increase of 1-2 points. This indicates that the coltsfoot essential oil prepared by this patent brings a richer and purer spicy and herbal aroma to cigarette products, with more prominent and easily identifiable aroma characteristics, and good harmony with the tobacco aroma. When the capsule containing this patented coltsfoot essential oil is popped, the spicy and herbal aroma is instantly released, perfectly blending with the smoke and enriching the aroma layers of the cigarette.

[0106] In terms of smoke quality indicators, A1 scored 18 points and A2 scored 19 points, significantly higher than D1's 17 points, with an improvement of 1-2 points. This indicates that the coltsfoot flower essential oil prepared in this patent has a positive impact on smoke quality, making the smoke more abundant, delicate, and full-bodied. This may be due to the good interaction between the terpenoid components in the coltsfoot flower essential oil and the smoke components, improving the physical properties and sensory experience of the smoke.

[0107] In terms of irritation index, both A1 and A2 scored 18 points, higher than D1's 17 points, an increase of 1 point. This indicates that the coltsfoot flower essential oil prepared by this patent reduces the irritation and burning sensation of cigarettes to a certain extent, which may be related to the lung-moistening and qi-regulating effects of coltsfoot flower itself, or it may be due to the removal of certain irritating impurities by the method of this patent.

[0108] In terms of total score, A1 scored 88 points and A2 scored 90 points, both significantly higher than D1's 85 points. A2's score was slightly higher than A1, which is related to the different non-polar solvent ratios used in Example 3. This indicates that the choice of solvent has a certain impact on the sensory quality of the final product, providing direction for further product optimization.

[0109] In terms of aftertaste, strength, and uniformity, the differences among the experimental cases were not significant, indicating that the coltsfoot flower essential oil prepared by this patent maintains at least a level comparable to that of traditional methods in these aspects.

[0110] Based on comprehensive sensory evaluation results, the coltsfoot flower essential oil prepared in this patent, when added to cigarettes, significantly enhances the spicy and herbal aromas, improves the richness and fullness of the smoke, and reduces irritation, thereby comprehensively improving the sensory quality of cigarettes and effectively increasing the added value and market competitiveness of cigarette products. This significant improvement in sensory quality is closely related to the efficient retention of key aroma components in coltsfoot flowers by the method of this patent.

[0111] All the raw materials listed in this invention, as well as the upper and lower limits and ranges of the raw materials and the upper and lower limits and ranges of the process parameters (such as temperature, time, etc.), can realize this invention. Examples are not listed one by one here.

[0112] The above description is merely a preferred embodiment of the present invention, and should not be construed as limiting the scope of the invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications are also considered to be within the scope of protection of the present invention.

[0113] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable way without contradiction. In order to avoid unnecessary repetition, this patent will not describe the various possible combinations separately.

[0114] Furthermore, various implementations of this patent can be combined in any way, and as long as they do not violate the spirit of this patent, they should also be regarded as the content disclosed in this patent.

Claims

1. A method for preparing coltsfoot flower essential oil, characterized in that, The preparation method includes the following steps: Step S1: The raw material of coltsfoot flower is pretreated by cell wall breaking and enzymatic hydrolysis to obtain wet material of coltsfoot flower enzymatic hydrolysis; Step S2: The wet material of the enzymatic hydrolysate of coltsfoot flower is subjected to supercritical extraction to obtain coltsfoot flower supercritical extract; Step S3: Dissolve and filter the coltsfoot flower supercritical extract to obtain the coltsfoot flower essential oil.

2. The preparation method according to claim 1, characterized in that, Step S1 includes the following steps: Step S11: The coltsfoot flower raw material is pulverized to obtain coltsfoot flower powder; Step S12: Mix the coltsfoot powder with cellulase and buffer solution, stir evenly, and let stand to obtain the coltsfoot enzymatic hydrolysate wet material.

3. The preparation method according to claim 2, characterized in that, In step S11, the rotation speed of the cell wall breaking and pulverizing process is 6000~10000 r / min; The particle size of the coltsfoot flower powder is 60-100 mesh; In step S12, the mass of the cellulase is 1-5% of the mass of the coltsfoot flower powder; The resting period is longer than two days.

4. The preparation method according to claim 1, characterized in that, Step S2 includes the following steps: Step S21: The wet material of the coltsfoot flower enzymatic hydrolysis is loaded into the extraction instrument and the extraction solvent and entrainer are injected, and then pressurized to a supercritical state; Step S22: Extracting the intermediate extract of coltsfoot flower from the wet enzymatic hydrolysate under the supercritical state; Step S23: The coltsfoot flower intermediate extract is separated from the extraction solvent to obtain the coltsfoot flower supercritical extract.

5. The preparation method according to claim 4, characterized in that, In step S21, the extraction solvent is carbon dioxide; The extraction pressure is 20~25MPa; The entrainer is anhydrous ethanol; The mass ratio of the entrainer to the wet coltsfoot flower degradation material is 1:16 to 1:

20. The separation pressure is 3~7MPa; The extraction temperature is 40~45℃; The extraction time is 2-3 hours.

6. The preparation method according to claim 1, characterized in that, In step S3, the coltsfoot flower supercritical extract is dissolved in a non-polar solvent; The coltsfoot flower supercritical extract is filtered through a ceramic membrane.

7. The preparation method according to claim 6, characterized in that, The non-polar solvent is edible olive oil and / or ODO; The ceramic membrane has a pore size of 0.8 μm.

8. A coltsfoot flower essential oil, characterized in that, The coltsfoot flower essential oil is prepared by the preparation method described in any one of claims 1 to 7.

9. A cigarette flavor capsule, characterized in that, The cigarette capsule includes coltsfoot essential oil as described in claim 8.

10. An aerosol-generating product, characterized in that, The aerosol-generating product includes the tobacco capsules as described in claim 9.

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