Extraction method and application of essential oil

Abstract

The invention belongs to the technical field of essential oil extraction, and particularly relates to an extraction method and application of essential oil. The extraction method comprises the following steps: (1) obtaining crushed fructus forsythiae or chamomile; (2) weighing and sieving to obtain treated powder; (3) wrapping the powder and performing Soxhlet extraction to obtain treated slurry; and (4) carrying out rotary evaporation drying on the obtained treated slurry to obtain the essential oil. According to the method, the essential oil can be extracted more efficiently, the loss of active ingredients of fructus forsythiae or chamomile is obviously reduced, and the active ingredients of the extracted essential oil can be reserved to a higher degree, so that after the extracted essential oil is applied to cigarette products, the sensory evaluation of the cigarette products can be better improved, and the quality of the cigarette products is improved. The important application value is realized.

Description

Technical Field

[0001] The invention belongs to the technical field of essential oil extraction, and particularly relates to an essential oil extraction method and application. Background Art

[0002] The information disclosed in this background section is intended to enhance understanding of the overall background of the invention and should not necessarily be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art.

[0003] Chinese cigarettes are constantly improving the quality of their products in the development requirements of reducing tar and reducing harm in China, but there are also certain problems. While the tar content of cigarettes is reduced, the aroma and concentration of cigarettes are greatly reduced, which directly affects the comfort and physiological satisfaction of smoking cigarettes. It is particularly worth noting that the production and consumption of cigarettes in my country are mainly flue-cured tobacco, and the planting area and total output of flue-cured tobacco rank first in the world; flue-cured tobacco cigarettes have a high sugar content, a low proportion of free nicotine, and soft smoke. Therefore, it is more difficult to reduce the tar of Chinese low-tar cigarettes, and the problem of insufficient aroma of flue-cured tobacco is particularly prominent. To some extent, aroma compensation has become a technical bottleneck in the development of Chinese low-tar cigarette products. In order to give cigarette products a good aroma and taste and coordinate smoke, cigarette flavoring is a commonly used process at present, and flavor and fragrance technology has also become one of the core technologies of Chinese cigarettes, especially Chinese low-tar cigarettes. Tobacco flavors are divided into artificial synthetic flavors and natural flavors, and each flavor has its own advantages and characteristics. Synthetic flavors have a specific composition, so they are often used for flavoring with a strong purpose. The composition of natural flavors is relatively complex. When used in cigarette flavoring, the taste will be richer and more layered. However, because the composition of natural flavors is unknown and complex, they will produce miscellaneous odors and peculiar smells when used in cigarette flavoring, which will reduce the smoking quality of cigarette products. Therefore, the development and utilization of natural flavors still need further research. At present, domestic tobacco flavors are mainly divided into synthetic flavors and natural flavors. Among them, natural flavors have been widely used in recent years because of their unique layering, unique fragrance and some medicinal value when used in cigarette flavoring. However, the current natural plant flavoring raw materials are relatively single, and traditional flavors have not yet been truly developed and utilized.

[0004] Heated tobacco (English: Heated Tobacco Products, Electronic cigarette, Heat Not Burning, full name "heated tobacco products") is a tobacco product that heats tobacco to a high temperature of about 200-300℃ without burning. Among them, stick-type electronic cigarettes only need to insert the stick-shaped cigarette cartridge into the cigarette cartridge heating device for inhalation. The main principle is that the cigarette cartridge heating device heats the smoke agent, tobacco leaves and flavors to form an aerosol, which is inhaled by the smoker. The existing plant-based flavors are more complex in composition and cannot be completely volatilized at 200-300℃, resulting in the volatilized aerosol gradually clogging the inner wall and interface of the cigarette cartridge heating device, reducing the service life of the equipment. Summary of the invention

[0005] In view of the deficiencies in the prior art, a first object of the present invention is to provide a method for extracting essential oils.

[0006] The second object of the present invention is to provide the application of the essential oil extracted by the above method.

[0007] To achieve the above object, the present invention adopts the following technical solution:

[0008] A method for extracting essential oils, comprising the following steps:

[0009] (1) placing the plant sample in an alkaline solution for immersion, and then drying it by heat to obtain a dry sample;

[0010] Furthermore, in step (1), the plant sample is Forsythia suspensa or Chamomile.

[0011] Furthermore, in step (1), the alkaline solution is a sodium carbonate solution, and the feasible mass fraction is 3.0-5.0%.

[0012] Furthermore, in step (1), the mass ratio of the alkaline solution to the plant sample is 8 to 12:1.

[0013] Furthermore, in step (1), the soaking temperature is 30-35° C. and the soaking time is 8-12 min.

[0014] Furthermore, in step (1), the temperature of the heat drying is 45 to 55° C., and the time is 1 to 3 hours.

[0015] Furthermore, in step (1), the soaking is followed by washing with clean water.

[0016] (2) taking the dry sample obtained in step (1), freezing it, and then crushing it, sieving it, and obtaining a crushed material;

[0017] Furthermore, in step (2), the freezing treatment temperature is -40 to -30°C, and the treatment time is 15 to 25 minutes.

[0018] Furthermore, in step (2), the rotation speed of the crushing is 2500 to 3500 r / min.

[0019] An organic solvent is added to the crushed material obtained in step (2), and then the mixture is heated for extraction, and then filtered and evaporated to obtain the essential oil.

[0020] Furthermore, in step (3), the organic solvent is at least one of anhydrous ethanol, petroleum ether, ethyl acetate and isopropanol.

[0021] Furthermore, in step (3), the heating extraction time is 4 to 6 hours.

[0022] Furthermore, in step (3), the mass volume ratio of the crushed material to the organic solvent is 1 g: 5.5-7.5 mL.

[0023] Furthermore, after obtaining the crushed material, the crushed material needs to be mixed with clean water and stirred to obtain a slurry.

[0024] In a preferred embodiment of the present invention, when the plant sample is chamomile, after obtaining the slurry, a treatment enzyme needs to be added to the slurry to perform enzymatic hydrolysis, and then heated for extraction to obtain the essential oil.

[0025] Furthermore, the mass ratio of the slurry to the treatment enzyme is (20-50):3.

[0026] Furthermore, the treatment enzymes are cellulase, pectinase and hemicellulase; the mass ratio of cellulase, pectinase and hemicellulase is (3-7):(0.5-1.5):(2-4).

[0027] The essential oil extracted by the above method can be used in the field of cigarette preparation.

[0028] After being frozen at low temperature, the impact toughness and elongation of forsythia and chamomile are reduced, that is, they become brittle. At the same time, the rapid cooling causes the uneven contraction of various parts and generates internal stress, which easily causes the weak parts of the material to be damaged and cracked, promotes the transmission and expansion of internal defects of the material, and leads to the reduction of the internal organization of the material. Therefore, when subjected to a certain impact force, the material is more likely to be broken into fine particles, and the particle size distribution of the powder is better, which is more convenient for the subsequent essential oil extraction process.

[0029] Beneficial effects: (1) The present invention adopts a freezing and pulverizing method to replace the conventional pulverization at room temperature. Compared with pulverization at room temperature, the color, aroma, taste and properties of active substances of Forsythia suspensa and chamomile after pulverization can be kept unchanged. By adopting the freezing and pulverizing method, the original molecular structure, composition and activity of nutrients in Forsythia suspensa and chamomile can be preserved to the greatest extent, thereby ensuring that the nutrients in the essential oil content are not lost; after subsequent enzymatic hydrolysis, it can be more conducive to the outflow of intracellular lysozymes of Forsythia suspensa and chamomile, thereby facilitating subsequent essential oil extraction and improving the essential oil yield; the present invention adopts the Soxhlet extraction method for extraction, which can prevent the solid sample from repeatedly contacting with the fresh solvent for many times, thereby improving the leaching rate of the analyte, and after continuous extraction, it is enriched in the flask, with high concentration and small amount of extractant.

[0030] (2) The present invention can extract essential oils more efficiently, and has a significantly reduced effect on the loss of active ingredients of Forsythia suspensa and chamomile, and can retain the active ingredients of the extracted chamomile essential oil to a higher degree. Therefore, after applying it to non-combustion cigarettes, it can better improve the sensory evaluation of non-combustion cigarettes.

[0031] (3) In the field of non-combustion cigarettes, the volatility of essential oils has a significant impact on the stability of the cartridges and the life of the cartridge heating device. According to prior art reports, natural plant essential oils are often prone to sedimentation and agglomeration during the prevention process due to their complex composition, affecting the smoking quality of the cartridges. It has been confirmed that the essential oil product provided by the present invention has good volatility, does not produce sedimentation and agglomeration after being placed, effectively prolongs the storage time, and has a high market value. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] The accompanying drawings constituting a part of the present invention are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. The embodiments of the present invention are described in detail below in conjunction with the accompanying drawings, wherein:

[0033] Figure 1 The total ion current chromatogram of volatile aroma components of the Forsythia suspensa essential oil extracted in Example 1 by GC-MS analysis;

[0034] Figure 2 The total ion current chromatogram of GC-MS analysis of volatile aroma components of chamomile essential oil extracted in Example 5;

[0035] Figure 3 is the extraction rate corresponding to different factor conditions in Example 6;

[0036] Figure 4 It is the extraction rate corresponding to different factor conditions in Example 7. DETAILED DESCRIPTION

[0037] The following description further describes the specific details of the present invention for a full understanding of the present invention. The terms used in the description of the present invention are only used to illustrate the advantages and features of the present invention and are not intended to limit the present invention.

[0038] Unless otherwise defined, all professional and scientific terms used in the present invention have the same meanings as those understood by technicians in the technical field of the present invention. Unless otherwise specified, the drugs or reagents used in the present invention are used in accordance with the product instructions or the conventional methods of use in the field. The technical solution of the present invention is further described according to the drawings and specific embodiments of the specification.

[0039] Example 1

[0040] The method for extracting Forsythia suspensa essential oil comprises the following steps:

[0041] (1) The intact Forsythia suspensa was immersed in a 3.5% sodium carbonate solution at 32°C for 10 min, taken out, and rinsed with clean water for 15 min. After rinsing with clean water, the Forsythia suspensa was taken out and dried with hot air at a temperature of 50°C for 2 h. The mass ratio of the sodium carbonate solution to the Forsythia suspensa was 10:1.

[0042] (2) taking 100 g of the forsythia obtained in step (1) and freezing it at -35°C for 20 min, taking it out and directly adding it to a high-speed universal grinder for grinding, the speed of the grinder is set to 3000 r / min, and then passing it through a 40-mesh sieve to obtain a forsythia grind;

[0043] (3) Wrapping the Forsythia suspensa powder obtained in step (2) with filter paper, placing it in a Soxhlet extractor, adding anhydrous ethanol and heating it with an electric furnace, the material-liquid ratio of the Forsythia suspensa powder to anhydrous ethanol is 1 g:5.5 mL; after extraction for 4 hours, filtering the extract through filter paper, adding it to a rotary evaporator, evaporating the water, and obtaining an extract;

[0044] (4) 250 mL of the extract obtained in step (3) was taken, 2 mL of dichloromethane was added, 1 mL of the mixed solution was taken, and filtered through a filter membrane. 0.75 mL of the filtrate after passing through the filter membrane was extracted and added to a chromatographic bottle, and then 0.25 mL of trans-dihexenoic acid was added, and then an internal standard was added for GC-MS analysis;

[0045] The GC-MS conditions were as follows: carrier gas was He; carrier gas flow rate was 1.5 mL / min, constant flow mode; injection port temperature was 250 °C; column temperature was 40 °C, kept for 4 min, increased at 6 °C / min to 100 °C, and increased at 4 °C / min to 250 °C, kept for 5 min, without splitting;

[0046] The GC-MS mass spectrometry parameters were as follows: interface temperature was 280°C; ion source temperature was 230°C; mass scanning range was m / z 50-550, quadrupole temperature was 150°C; electron ionization source, electron energy was 70 eV.

[0047] Figure 1 This is the total ion current chromatogram of the GC-MS analysis of the Fructus Forsythiae essential oil extracted in Example 1.

[0048] Example 2

[0049] A method for extracting Forsythia suspensa extract comprises the following steps:

[0050] (1) Soak the intact Forsythia suspensa in a 3.0% sodium carbonate solution with a mass ratio of sodium carbonate to Forsythia suspensa of 8:1 at a soaking temperature of 30°C for 12 min, then rinse with clean water for 15 min, take out after rinsing with clean water, and dry with hot air at a temperature of 55°C for 1 h;

[0051] (2) taking 100 g of the forsythia obtained in step (1) and freezing it at -30°C for 15 min, taking it out and adding it to a high-speed universal grinder for crushing at a speed of 3500 r / min, and passing it through a 60-mesh sieve to obtain a forsythia crushed material;

[0052] (3) Wrapping the Forsythia suspensa powder obtained in step (2) with filter paper, placing it in a Soxhlet extractor, adding anhydrous ethanol, and heating it with an electric furnace, the material-liquid ratio of the Forsythia suspensa powder to anhydrous ethanol is 1 g: 6.5 mL; after extraction for 6 hours, filtering the extract through filter paper, adding it to a rotary evaporator, and evaporating the water to obtain an extract;

[0053] (5) 250 mL of the extract obtained in step (3) was taken, 2 mL of dichloromethane was added, 1 mL of the mixed solution was taken, and the mixture was filtered through a filter membrane. 0.75 mL of the filtrate after passing through the filter membrane was extracted and added to a chromatographic bottle, and then 0.25 mL of trans-dihexenoic acid was added, and then an internal standard was added for GC-MS analysis;

[0054] GC-MS conditions were as follows: carrier gas was He; carrier gas flow rate was 1.5 mL / min, constant flow mode; injection port temperature was 250°C; column temperature was 40°C, kept for 4 min, increased at 6°C / min to 100°C, and increased at 4°C / min to 250°C, kept for 5 min, without splitting;

[0055] The GC-MS mass spectrometry parameters were as follows: interface temperature was 280°C; ion source temperature was 230°C; mass scanning range was m / z 50-550; quadrupole temperature was 150°C; electron ionization source, electron energy was 70 eV.

[0056] Example 3

[0057] A method for extracting Fructus Forsythiae extract comprises the following steps:

[0058] (1) Soak the intact Forsythia suspensa in a sodium carbonate solution with a mass fraction of 5.0%, the mass ratio of the sodium carbonate solution to the Forsythia suspensa is 12:1, the soaking temperature is 35°C, the soaking time is 8 minutes, then take it out, rinse it with clean water for 15 minutes, take it out after rinsing with clean water, use hot air to dry it, the hot air temperature is 45°C, and the drying time is 3 hours;

[0059] (2) taking 100 g of Forsythia suspensa and freezing it at -40°C for 25 min, taking it out and directly adding it to a high-speed universal grinder for crushing at a speed of 3500 r / min, and passing it through a 100-mesh sieve after crushing to obtain Forsythia suspensa crushed material;

[0060] (3) Wrapping the Forsythia suspensa powder obtained in step (2) with filter paper, placing it in a Soxhlet extractor, adding anhydrous ethanol and heating it with an electric furnace, the material-liquid ratio of the Forsythia suspensa powder to the solvent is 1 g:7.5 mL; extracting for 5 hours, filtering the extract through filter paper, adding it to a rotary evaporator, evaporating the water, and obtaining an extract;

[0061] (4) 250 mL of the extract obtained in step (3) was taken and 2 mL of dichloromethane was added, 1 mL of the mixed solution was taken and filtered through a filter membrane, 0.75 mL of the filtrate after passing through the filter membrane was extracted and added to a chromatographic bottle, and then 0.25 mL of trans-dihexenoic acid was added, and then an internal standard was added for GC-MS analysis;

[0062] The GC-MS conditions were as follows: carrier gas was He; carrier gas flow rate was 1.5 mL / min, constant flow mode; injection port temperature was 250 °C; column temperature was 40 °C, kept for 4 min, increased at 6 °C / min to 100 °C, and increased at 4 °C / min to 250 °C, kept for 5 min, without splitting;

[0063] The GC-MS mass spectrometry parameters were as follows: interface temperature was 280°C; ion source temperature was 230°C; mass scanning range was m / z 50-550, quadrupole temperature was 150°C; electron ionization source, electron energy was 70 eV.

[0064] Example 4

[0065] A method for extracting Fructus Forsythiae extract comprises the following steps:

[0066] (1) The intact Forsythia suspensa was immersed in a sodium carbonate solution with a mass fraction of 3.5%, the mass ratio of the sodium carbonate solution to Forsythia suspensa was 10:1, the immersion temperature was 32°C, the time was 10 min, then taken out, rinsed with clean water for 15 min, and then taken out and dried with hot air at a temperature of 50°C for 2 h.

[0067] (2) taking 100 g of the forsythia obtained in step (1) and freezing it at -35°C for 20 min, taking it out and adding it to a high-speed universal grinder for crushing at a speed of 3000 r / min, and passing it through a 60-mesh sieve to obtain a forsythia crushed material;

[0068] (3) Wrapping the Forsythia suspensa powder obtained in step (2) with filter paper, placing it in a Soxhlet extractor, adding anhydrous ethanol, and heating it with an electric furnace. The heating temperature is such that the material-liquid ratio of the Forsythia suspensa powder to anhydrous ethanol is 1 g:7.5 mL, and extracting for 4 hours to obtain an extract;

[0069] (4) 250 mL of the extract obtained in step (3) was taken and 2 mL of dichloromethane was added. 1 mL of the mixed solution was taken and filtered through a filter membrane. 0.75 mL of the filtrate after passing through the filter membrane was extracted and added to a chromatographic bottle. 0.25 mL of trans-dihexenoic acid was added, and then an internal standard was added for GC-MS analysis.

[0070] GC-MS conditions were as follows: carrier gas was He; carrier gas flow rate was 1.5 mL / min, constant flow mode; injection port temperature was 250°C; column temperature was 40°C, kept for 4 min, increased at 6°C / min to 100°C, and increased at 4°C / min to 250°C, kept for 5 min, without splitting;

[0071] The GC-MS mass spectrometry parameters are as follows: interface temperature is 280°C; ion source temperature is 230°C; mass scanning range is m / z 50-550; quadrupole temperature is 150°C; electron ionization source, electron energy is 70 eV.

[0072] Comparative Example 1

[0073] In this embodiment, another method for extracting Forsythia suspensa essential oil is provided, which is different from that in Embodiment 1 in that, in step (2), 100 g of the Forsythia suspensa obtained in step (1) is placed in an oven and dried at 45° C. for 35 min. The Forsythia suspensa essential oil is taken out and directly added to a high-speed universal grinder for crushing. The speed of the grinder is set to 3000 r / min. The Forsythia suspensa essential oil is then passed through a 40-mesh sieve to obtain a Forsythia suspensa crushed material.

[0074] Comparative Example 2

[0075] In this embodiment, another method for extracting Forsythia suspensa essential oil is provided, which is different from that in Embodiment 1 in that, before step (1), the Forsythia suspensa is placed in an oven and heated at 105° C. for 15 minutes to perform “fixing”.

[0076] Example 5

[0077] (1) Select intact chamomile and soak it in a 3.5% sodium carbonate solution for 10 minutes at a temperature of 32°C and a mass ratio of sodium carbonate solution to chamomile of 10:1. Rinse it with clean water for 15 minutes. After rinsing with clean water, take it out and blow dry it with hot air at a temperature of 50°C for 2 hours.

[0078] (2) taking 100 g of the chamomile obtained in step (1) and freezing it at a temperature of -35°C for 20 min, then taking it out and directly adding it to a high-speed universal grinder for crushing at a crushing speed of 3000 r / min, and passing it through a 60-mesh sieve to obtain a chamomile crushed material;

[0079] (3) adding the chamomile crushed material obtained in step (2) and clean water at room temperature to a stirring tank for stirring and mixing, stirring at a speed of 500 r / min for 30 min to obtain a chamomile slurry; the mixing mass ratio of the chamomile crushed material to the clean water is 1:30;

[0080] (4) adding the chamomile slurry obtained in step (3) to an enzymolysis tank for treatment, adding a treatment enzyme to the enzymolysis tank, performing enzymolysis treatment on the chamomile slurry, stirring and mixing evenly, and stirring at a speed of 150 r / min; then adjusting the treatment temperature to 38° C., keeping warm and stirring for 6 hours, and then naturally cooling to room temperature to obtain a treated slurry; wherein the chamomile slurry and the treatment enzyme are mixed in a mass ratio of 40:3. The treatment enzymes are cellulase, pectinase and hemicellulase; the cellulase, pectinase and hemicellulase are mixed in a mass ratio of 5:1:3.

[0081] (5) subjecting the treated slurry prepared in step (4) to rotary evaporation and drying, and then crushing and passing through a 60-mesh sieve to obtain a treated powder;

[0082] (6) The treated powder prepared above was wrapped with filter paper and placed in a Soxhlet extractor. Anhydrous ethanol was added to the flask. Different conditions were numbered as EtOH.1 to 9. The orthogonal test results were subjected to range analysis, as shown in the following figure:

[0083] Table 1 shows that the R value factor 2>factor 1>factor 3, and it can be concluded that the solid-liquid ratio of 8 has the greatest impact on the extraction rate of chamomile essential oil, followed by the chamomile mesh number, and the extraction time has the lowest impact on the extraction rate of chamomile essential oil. As can be seen from the chart, the best process condition combination for Soxhlet extraction of chamomile is anhydrous ethanol as solvent, chamomile mesh 40, solid-liquid ratio 1:7.5g / mL, and extraction time 6h. The highest extraction rate of chemical components of chamomile is 39.02%.

[0084] Table 1

[0085]

[0086] Table 2

[0087]

[0088] Example 6

[0089] Orthogonal experimental results and analysis under petroleum ether conditions include the following steps:

[0090] (1) Soak intact chamomile in a 3.0% sodium carbonate solution, the mass ratio of the sodium carbonate solution to the chamomile being 12:1, the soaking temperature being 30°C, the soaking time being 12 minutes, then take it out, rinse it with clean water for 15 minutes, take it out after rinsing with clean water, dry it with hot air, the hot air temperature being 50°C, and the hot air drying time being 2 hours;

[0091] (2) taking 100 g of the chamomile obtained in step (1) and freezing it at -40°C for 15 min, then taking it out and directly adding it to a high-speed universal grinder for crushing at a crushing speed of 2500 r / min; passing it through an 80-mesh sieve to obtain a chamomile crushed material;

[0092] (3) adding the chamomile crushed material obtained in step (2) and clean water at room temperature to a stirring tank for stirring and mixing; stirring at a speed of 500 r / min for 30 minutes to obtain a chamomile slurry; the mixing mass ratio of the chamomile crushed material to the clean water is 1.6:30;

[0093] (4) adding the chamomile slurry obtained in step (3) to an enzymolysis tank for treatment, adding a treatment enzyme to the enzymolysis tank, the mass ratio of the chamomile slurry to the treatment enzyme being 42:3, performing enzymolysis treatment on the chamomile slurry, stirring and mixing evenly, the stirring speed being 150 r / min, and then adjusting the treatment temperature to 39° C., keeping warm and stirring for 6.5 hours, and then naturally cooling to room temperature to obtain a treated slurry; the treatment enzymes are cellulase, pectinase and hemicellulase; the mass ratio of cellulase, pectinase and hemicellulase is 5:1:3.

[0094] (5) subjecting the treated slurry obtained in step (4) to rotary evaporation and drying, and then crushing and sieving to obtain a treated powder;

[0095] (6) The treated powder prepared in step (5) is wrapped with filter paper and placed in a Soxhlet extractor. Anhydrous ethanol is added to the flask. Different conditions are numbered as EtOH.1 to 9. The orthogonal test results are subjected to range analysis, as shown in the following numbering design table and extraction rate result analysis table:

[0096] By comparison, it can be found that when petroleum ether is used as solvent, the extraction rate of chemical components of chamomile is the highest, which is 11.84%, under the conditions of chamomile size of 100 mesh, solid-liquid ratio of 1:7.5 g / mL, and extraction time of 4 h.

[0097] In addition, Table 3 shows that under the same mesh size, the extraction rate of chamomile essential oil basically shows an upward trend with the increase of solvent volume and extraction time, and the extraction effect of chamomile under various conditions is not much different, and the maximum extraction rate and the minimum extraction rate only differ by 2.37%. Under the condition of 100 mesh, the extraction rate of chamomile essential oil increases rapidly, and the extraction rate of chamomile essential oil is generally low when petroleum ether is used as solvent, and the extraction effect is poor.

[0098] Table 3

[0099]

[0100] Example 7

[0101] Orthogonal experimental results and analysis under ethyl acetate conditions, comprising the following steps:

[0102] (1) placing intact chamomile in a sodium carbonate solution with a mass fraction of 5.0%, the mass ratio of the sodium carbonate solution to the chamomile is 12:1, the soaking temperature is 35°C, the soaking time is 12 minutes, then taking it out, rinsing it with clean water for 15 minutes, taking it out after rinsing with clean water, and drying it with hot air at a temperature of 50°C and a hot air drying time of 2 hours;

[0103] (2) taking 100 g of the chamomile obtained in step (1) and freezing it at -30°C for 25 min, then taking it out and directly adding it to a high-speed universal grinder for crushing at a speed of 3000 r / min, and passing it through an 80-mesh sieve to obtain a chamomile crushed material;

[0104] (3) adding the chamomile crushed material obtained in step (2) and clean water at room temperature to a stirring tank for stirring and mixing: stirring at a speed of 500 r / min for 30 minutes to obtain a chamomile slurry; the mass ratio of the chamomile crushed material to the clean water is 1.5:30;

[0105] (4) adding the chamomile slurry obtained in step (3) to an enzymolysis tank for treatment, adding a treatment enzyme to the enzymolysis tank, performing enzymolysis treatment on the chamomile slurry, stirring and mixing evenly, the stirring speed is 150 r / min, the mass ratio of the chamomile slurry and the treatment enzyme is 43:3, and then adjusting the treatment temperature to 39°C, keeping warm and stirring for 7 hours, and then naturally cooling to room temperature to obtain a treated slurry; the treatment enzymes are cellulase, pectinase and hemicellulase; the mass ratio of cellulase, pectinase and hemicellulase is 5:1:3.

[0106] (5) subjecting the treated slurry obtained in step (4) to rotary evaporation and drying, and then crushing and passing through a 60-mesh sieve to obtain a treated powder;

[0107] (6) The treated powder obtained in step (5) is wrapped with filter paper and placed in a Soxhlet extractor. Anhydrous ethanol is added to the flask. Different conditions are numbered as EtOH.1 to 9. The orthogonal test results are subjected to range analysis, as shown in the following numbering design table and extraction rate result analysis table:

[0108] By comparison, it was found that when ethyl acetate was used as the solvent, the extraction rate of the chemical components of chamomile was the highest, which was 21.09%, under the conditions of chamomile size of 100 mesh, solid-liquid ratio of 1:6.5, and extraction time of 5h.

[0109] In addition, Table 4 shows that under the conditions of 40 mesh and 60 mesh, the extraction rate of chamomile essential oil showed an upward trend with the increase of solvent volume and extraction time. Under the condition of 100 mesh, the extraction rate of chamomile essential oil first increased and then decreased. The extraction effects of each condition were quite different, with the maximum extraction rate and the minimum extraction rate differing by 9.68%, but the overall extraction rate was generally higher than that when petroleum ether was used as solvent, and the extraction effect of this solvent was average.

[0110] Table 4

[0111]

[0112] Example 8

[0113] Orthogonal experimental results and analysis under ethyl acetate conditions, comprising the following steps:

[0114] (1) placing intact chamomile in a sodium carbonate solution with a mass fraction of 3.5%, the mass ratio of the sodium carbonate solution to the chamomile being 10:1, the soaking temperature being 32° C., the soaking time being 10 min, then taking it out, and rinsing it with clean water for 15 min. After rinsing with clean water, taking it out, and drying it with hot air at a hot air temperature of 50° C. and a hot air drying time of 2 h.

[0115] (2) taking 100 g of the chamomile obtained in step (1) and freezing it at a temperature of -35°C for 20 min, then taking it out and directly adding it to a high-speed universal grinder for crushing at a crushing speed of 3000 r / min, and passing it through an 80-mesh sieve to obtain a chamomile crushed material;

[0116] (3) adding the chamomile crushed material obtained in step (2) and clean water at room temperature to a stirring tank for stirring and mixing; stirring at a speed of 500 r / min for 30 minutes to obtain a chamomile slurry; the mixing mass ratio of the chamomile crushed material to the clean water is 1.8:30;

[0117] (4) adding the chamomile slurry obtained in step (3) to an enzymolysis tank for treatment, adding a treatment enzyme to the enzymolysis tank, performing enzymolysis treatment on the chamomile slurry, stirring and mixing evenly, and then adjusting the treatment temperature to 38.5°C, keeping warm and stirring for 7 hours, and then naturally cooling to room temperature to obtain a treated slurry; wherein the stirring speed is 150r / min; the mixed mass ratio of chamomile slurry and treatment enzyme is 44:3. The treatment enzyme includes cellulase, pectinase, and hemicellulase; wherein the mixed mass ratio of cellulase, pectinase, and hemicellulase is 5:1:3;

[0118] (5) subjecting the treated slurry obtained in step (4) to rotary evaporation and drying, and then crushing and passing through a 60-mesh sieve to obtain a treated powder;

[0119] (6) Wrap the treated powder obtained in step (5) with filter paper and place it in a Soxhlet extractor. Add anhydrous ethanol to the flask, number the different conditions as EtOH.1 to 9, and perform range analysis on the orthogonal test results, as shown in the numbering design table and extraction rate result analysis table below.

[0120] By comparison, it was found that when isopropanol was used as the solvent, the extraction rate of the chemical components of chamomile was the highest, which was 28.51%, under the conditions of chamomile size of 100 mesh, solid-liquid ratio of 1:6.5 g / mL, and extraction time of 5 h.

[0121] In addition, Table 5 shows that under the condition of 40 mesh, the extraction rate of chamomile essential oil showed an upward trend with the increase of solvent volume and extraction time. Under the conditions of 60 mesh and 100 mesh, the extraction of chamomile essential oil first increased and then decreased. The extraction effects of each condition were quite different, with the maximum extraction rate and the minimum extraction rate differing by 13.91%, but the overall extraction rate was high, and the solvent extraction effect was good.

[0122] Table 5

[0123]

[0124] Comparative Example 3

[0125] In this embodiment, another method for extracting chamomile essential oil is provided, which is different from that of Example 5 in that, in step (2), 100 g of the chamomile obtained in step (1) is placed in an oven and dried at 45° C. for 35 min. The chamomile is taken out and directly added to a high-speed universal grinder for crushing. The speed of the grinder is set to 3000 r / min, and then passed through a 40-mesh sieve to obtain a Forsythia suspensa crushed material.

[0126] Comparative Example 4

[0127] In this embodiment, another method for extracting chamomile essential oil is provided, which is different from that in Embodiment 1 in that, before step (1), the chamomile is placed in an oven and heated at 105° C. for 15 minutes to perform a similar “killing” operation.

[0128] Performance Testing

[0129] 1. Chemical composition detection

[0130] The Forsythia suspensa essential oil extracted in Example 1 and the chamomile essential oil extracted in Example 5 were detected by gas chromatography-mass spectrometry. The results are shown in Tables 6 and 7.

[0131] Table 6 GC-MS analysis of Forsythia suspensa essential oil

[0132]

[0133]

[0134] Table 7 GC-MS analysis of chamomile essential oil

[0135]

[0136]

[0137]

[0138]

[0139] As can be seen from Table 1, the chamomile essential oil extracted by the present invention contains a variety of active ingredients. The above active ingredients are rich in various short-chain esters and derivatives of acids, aldehydes, and ketones, etc., which make the cigarette present a pleasant fruit and flower aroma and have a significant flavor enhancement effect.

[0140] 2. Calculation of extraction rate

[0141] Extraction rate = (mass of extract / mass of Forsythia suspensa) × 100%. The results are shown in Tables 8 and 9.

[0142] Table 8 Extraction rate of Example 1-Example 4

[0143] Essential oil yield% Example 1 12.02 Example 2 12.51 Example 3 16.21 Example 4 14.32 Comparative Example 1 11.91 Comparative Example 2 5.55

[0144] Table 9 Extraction rate of Example 5-Example 8

[0145] Essential oil yield% Example 5 39.02 Example 6 31.84 Example 7 31.09 Example 8 38.51 Comparative Example 1 25.23 Comparative Example 2 16.25

[0146] According to prior art reports, natural essential oils extracted from plants as raw materials have rich pleasant aromas such as fruity, floral, woody, and tea aromas as spices, but they are also prone to "astringency". In order to obtain better extraction effects, the present invention draws on the "steaming green" process of traditional tea leaves, and introduces high temperature treatment before and after water addition (Comparative Examples 1-4) to remove the astringency of natural essential oils. The essential oil extraction results of the above process are shown in Tables 8 and 9. It can be seen that the present invention adopts a freeze-drying treatment method compared to a heat treatment method, which significantly improves the extraction efficiency of essential oil extraction. According to observations, this may be related to the fact that freeze-drying can fully destroy the wood fiber structure in plants, so that volatile substances can be fully dissolved.

[0147] 3. Evaluation of the volatility of essential oils in cigarette cartridges

[0148] The same batch of tobacco leaves are made into reconstituted tobacco leaves by a coating thick pulp method, cut into shreds, and rolled into cigarette paper in bundles to make cigarette cartridges. The cigarette cartridges contain 9% of shredded tobacco raw materials, 0.1% of the essential oil prepared in the above embodiment or comparative example, and the remaining 90.9% of glycerin, propylene glycol smoke-generating agents, and exogenous wood pulp fibers.

[0149] The prepared cigarette cartridges were placed in polyethylene bags, each of which was individually packaged and placed in a constant temperature box at 40°C for a placement experiment. The cigarette cartridges were taken out at regular intervals to check their status. During the inspection, the cigarette cartridges were placed on white paper, rolled with a glass roller, and then observed for their status. Ten experts observed the status on the paper and gave independent scores without knowing the group. The scoring criteria are as follows:

[0150] Table 10 Evaluation criteria for volatility of essential oils in cigarette cartridges

[0151] Rating Range Evaluation Criteria 7-10 points After crushing, the cigarette cartridges are evenly dispersed in sand or powder form 4 to 7 points (not including 7) After rolling, obvious agglomerates can be seen 1 to 4 points (not including 4) Obvious oil stains, lumps, etc. appear on the paper after rolling

[0152] Table 11

[0153]

[0154]

[0155] The above scoring results show that the essential oil provided in Example 4 and Example 8 is a mixed component with good volatility. The components in the essential oil can show a relatively consistent volatilization rate under the same heating conditions, and there will be no obvious precipitation, agglomeration or oily residue, which is more suitable for addition to non-heating cigarette cartridges.

[0156] 4. Sensory evaluation of cigarettes

[0157] The same batch of tobacco leaves are made into reconstituted tobacco leaves through a coating thick pulp method, cut into shreds, and rolled into cigarette paper in bundles to make cigarette cartridges. The cigarette cartridge contains 9% of the tobacco raw materials that have been shredded, 0.1% of the forsythia essential oil of Example 4 or the chamomile essential oil extracted in Example 8, and the remaining 90.9% of glycerol, propylene glycol smoke-generating agents, and exogenous wood pulp fibers. The cigarette cartridge heating equipment is a central electric heating non-combustion cigarette smoking device produced by Yunnan China Tobacco Industry Co., Ltd., and heats the cigarette cartridge in the range of 250 to 300°C.

[0158] The sensory evaluation of heat-not-burn tobacco was completed by 10 smoking experts with cigarette sensory quality evaluation qualifications from the Technical Center of Yunnan China Tobacco Industrial Co., Ltd. Table 12 shows the scoring criteria.

[0159] According to the Yunnan China Tobacco Enterprise Standard “Sensory Evaluation Method for New Cigarettes” (Q / YNZY.J04.022—2015), the aroma, flavor, strength, harmony, and taste were evaluated and scored, and the average value was taken; the results are shown in Tables 13-14.

[0160] Table 12 Scoring criteria

[0161]

[0162] Table 13 Sensory scores of the Forsythia suspensa essential oil extracted from Example 4

[0163] serial number Aroma Momentum Coordination Taste Example 4 27.5 9.2 9.6 23.4

[0164] Table 14 Sensory scores of the Forsythia suspensa essential oil extracted from Example 8

[0165] serial number Aroma Momentum Coordination Taste Example 8 29.2 9.8 9.5 26.2

[0166] The results show that the sensory evaluations of the non-burning cigarettes after the introduction of the forsythia essential oil or chamomile essential oil of the present invention are all high.

[0167] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable ordinary technicians in the field to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made based on the essence of the content of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for extracting essential oils, characterized in that: The extraction method comprises the following steps: (1) placing the plant sample in an alkaline solution for immersion, and then drying it by heat to obtain a dry sample; (2) taking the dry sample obtained in step (1), freezing it, and then crushing it, sieving it, and obtaining a crushed material; (3) adding an organic solvent to the crushed material obtained in step (2) and performing heating extraction, and then filtering and evaporating to obtain the essential oil.

2. The extraction method according to claim 1, characterized in that In step (1), the plant sample is Forsythia suspensa or Chamomile; The alkaline solution is a sodium carbonate solution with a mass fraction of 3.0 to 5.0%; The mass ratio of the alkaline solution to the plant sample is 8-12:

1.

3. The extraction method according to claim 1, characterized in that In step (1), the soaking temperature is 30-35° C. and the soaking time is 8-12 min; The temperature of the hot drying is 45-55°C and the time is 1-3h; After the soaking, clean water is needed for washing.

4. The extraction method according to claim 1, characterized in that In step (2), the freezing treatment temperature is -40 to -30°C, and the treatment time is 15 to 25 minutes; The rotation speed of the crushing is 2500-3500 r / min.

5. The extraction method according to claim 1, characterized in that After obtaining the crushed material, the crushed material needs to be mixed with clean water and stirred to obtain slurry.

6. The extraction method according to claim 5, characterized in that When the plant sample is chamomile, after obtaining the slurry, a treatment enzyme needs to be added to the slurry to perform enzymatic hydrolysis, and then heat extraction is performed to obtain the essential oil.

7. The extraction method according to claim 6, characterized in that The mass ratio of the slurry and the treated enzyme is (20-50):3; The treatment enzymes are cellulase, pectinase and hemicellulase; the mass ratio of cellulase, pectinase and hemicellulase is (3-7):(0.5-1.5):(2-4).

8. The extraction method according to claim 1, characterized in that In step (3), the organic solvent is at least one of anhydrous ethanol, petroleum ether, ethyl acetate and isopropanol; and the extraction time is 3 to 8 hours.

9. The extraction method according to claim 1, characterized in that The mass volume ratio of the crushed material to the organic solvent is 1g: (3.5-8.5)mL.

10. Application of the essential oil extracted by any one of the methods of claims 1 to 9 in the field of cigarettes, characterized in that: The essential oil is used for preparing non-burning cigarettes.

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