A kind of sage oil and preparation method thereof

Abstract

The present invention provides a clary sage oil and a preparation method thereof. Compared with the prior art, the present invention simultaneously extracts clary sage essential oil and separates sclareol using high-speed countercurrent chromatography. The sclareol obtained by high-speed countercurrent chromatography is then added to the clary sage essential oil to produce a new clary sage oil. This new clary sage oil has a high sclareol content, is effective and targeted, and significantly improves the quality of the essential oil, with a more pronounced amber-ambergris aroma and better smoking performance. Application in cigarettes can significantly improve the smoking experience of cigarettes.

Description

Technical Field

[0001] The invention belongs to the technical field of tobacco flavorings, and in particular relates to clary sage oil and a preparation method thereof. Background Art

[0002] Sclarea oil is a light yellow to orange-yellow liquid at room temperature. Its main components include linalyl acetate, linalool, geraniol, terpineol, sclareol, nerolidol, nerolidol acetate, terpinene, phellandrene, etc., among which the content of sclareol is only about 0.9%.

[0003] Sclareol can be isolated from the stems and leaves of the natural Clary Sage plant. It has a faint amber aroma that diffuses strongly and lasts long, imparting a vivid, harmonious, and long-lasting fragrance to fragrances. Sclareol is primarily used in the synthesis of natural ambergris substitutes and, in smaller quantities, in the blending of fragrances. In recent years, with increasing interest in the bioactivity of natural products, sclareol has been shown to possess pharmacological activities such as anti-inflammatory, antimicrobial, bactericidal, and anticancer activity. Acute toxicity tests have also shown that sclareol is low in toxicity, demonstrating that the Clary Sage plant is a valuable medicinal raw material and also has promising applications as a flavoring in cigarettes.

[0004] However, the development of sclareol is currently in its early stages, with only products such as sclareol extract available on the market. Therefore, increasing the sclareol content in sclareol oil is of great significance for its development and utilization. Summary of the Invention

[0005] In view of this, the technical problem to be solved by the present invention is to provide a sclareol oil with a high sclareol content and a preparation method thereof.

[0006] The present invention provides a preparation method of clary sage oil, comprising the following steps:

[0007] S1) extracting one or more of the crushed sclarea raw materials by steam distillation to obtain sclarea essential oil and sclarea raw material residue; wherein the sclarea raw materials are selected from one or more of sclarea flowers, sclarea stems and sclarea leaves;

[0008] S2) mixing the sclarea raw material filter residue with an ethanol solution, and heating the mixture to obtain a sclarea crude extract;

[0009] S3) extracting and concentrating the crude clary sage extract with an organic solvent to obtain a clary sage extract;

[0010] S4) separating and purifying the Clerodendrum sclarea extract by high-speed countercurrent chromatography to obtain a sclareol solution; the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system;

[0011] S5) mixing the sclareol solution with sclareol essential oil to obtain sclareol oil.

[0012] Preferably, in step S1), the mass ratio of the crushed Clerodendrum sclareae raw material to water during steam distillation extraction is 1:(4-8);

[0013] The temperature of the steam distillation extraction is 100° C.; the time of the steam distillation extraction is 4 to 6 hours.

[0014] Preferably, the volume concentration of ethanol in the ethanol solution in step S2) is 60% to 85%;

[0015] The mass ratio of the sclarea raw material filter residue to the ethanol solution is 1: (4-6);

[0016] The heating treatment is heating under reflux; the time of the heating treatment is 2 to 4 hours.

[0017] Preferably, the organic solvent in step S3) is selected from ethyl acetate; and the concentration is performed to a relative density of 1.2 to 1.3.

[0018] Preferably, the two-phase ethyl acetate solvent system is propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution; the upper phase of the two-phase ethyl acetate solvent system is the stationary phase, and the lower phase is the mobile phase.

[0019] Preferably, the mass ratio of the propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution is (1-3):(4-6):(1-3):(4-6).

[0020] Preferably, the pumping speed of the stationary phase of the high-speed countercurrent chromatography is 2.5-3.0 mL / min; the main engine speed is 700-800 r / min; and the pumping speed of the mobile phase is 2.5-3.0 mL / min.

[0021] Preferably, the mass ratio of the sclareol solution to the sclareol essential oil is (1-2):1.

[0022] The present invention also provides clary sage oil prepared by the above preparation method.

[0023] The present invention also provides a method for preparing a sclareol solution, comprising the following steps:

[0024] A1) extracting one or more of the crushed Clary Sage raw materials by steam distillation to obtain Clary Sage essential oil and Clary Sage raw material residue, wherein the Clary Sage raw materials are selected from one or more of Clary Sage flowers, Clary Sage stems, and Clary Sage leaves;

[0025] A2) mixing the sclarea raw material filter residue with an ethanol solution, and heating the mixture to obtain a sclarea crude extract;

[0026] A3) extracting and concentrating the crude clary sage extract with an organic solvent to obtain a clary sage extract;

[0027] A4) separating and purifying the sclareol extract by high-speed countercurrent chromatography to obtain a sclareol solution; the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system.

[0028] The invention provides a preparation method of sclarea oil, comprising the following steps: S1) extracting one or more crushed sclarea raw materials by steam distillation to obtain sclarea essential oil and sclarea raw material residue, wherein the sclarea raw materials are selected from one or more of sclarea flowers, sclarea stems and sclarea leaves; S2) mixing the sclarea raw material residue with an ethanol solution, and performing a heating treatment to obtain a sclarea crude extract; S3) extracting and concentrating the sclarea crude extract with an organic solvent to obtain a sclarea extract; S4) separating and purifying the sclarea extract by high-speed countercurrent chromatography to obtain a sclareol solution, wherein the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system; S5) mixing the sclareol solution with sclarea essential oil to obtain sclarea oil. Compared with the prior art, the present invention simultaneously carries out extraction of clary sage essential oil and separation of clary alcohol by high-speed countercurrent chromatography, and then adds clary sage alcohol using the essential oil as a solvent to obtain new clary sage oil, which has a high sclareol content. The preparation method is practical and effective, with strong perilla ... DETAILED DESCRIPTION

[0029] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0030] The invention provides a preparation method of a sclareol solution, comprising the following steps: A1) extracting one or more crushed sclareol raw materials by steam distillation to obtain sclareol essential oil and sclareol raw material residue, wherein the sclareol raw materials are selected from one or more of sclareol flowers, sclareol stems and sclareol leaves; A2) mixing the sclareol raw material residue with an ethanol solution, and heating the mixture to obtain a sclareol crude extract; A3) extracting and concentrating the sclareol crude extract with an organic solvent to obtain a sclareol extract; A4) separating and purifying the sclareol extract by high-speed countercurrent chromatography to obtain a sclareol solution, wherein the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system.

[0031] The present invention has no particular limitation on the sources of all raw materials, and any commercially available raw materials may be used.

[0032] Extracting one or more of the crushed clary sage raw materials by steam distillation to obtain clary sage essential oil and clary sage raw material residue; the clary sage raw material is one or more of clary sage flowers, clary sage stems and clary sage leaves, more preferably clary sage flowers, clary sage stems and clary sage leaves; the mass ratio of the clary sage flowers, clary sage stems and clary sage leaves is preferably 1:(1-5):(3-9), more preferably 1:(2-4):(4-8), more preferably 1:3:(5-7), and most preferably 1:3:6; the particle size of the crushed clary sage raw material is preferably 60-80 mesh; The mass ratio of the crushed Perilla frutescens raw material to water during steam distillation extraction is preferably 1:(4-8), more preferably 1:(4-7), and even more preferably 1:(4-6); in the embodiments provided by the present invention, it can be 1:4, 1:5, 1:6, 1:7, 1:8 or any value between 1:(4-8); the temperature of the steam distillation extraction is preferably 100°C; the time of the steam distillation extraction is preferably 4-6h; in the embodiments provided by the present invention, the time of the steam distillation extraction can be 4h, 5h, 6h or any value between 4 and 6.

[0033] The clary sage raw material filter residue is mixed with an ethanol solution and subjected to heat treatment to obtain a clary sage crude extract; the volume concentration of ethanol in the ethanol solution is preferably 60% to 85%; in the embodiment provided by the present invention, the volume concentration of ethanol in the ethanol solution is specifically 60%, 70%, 80%, 85% or any value between 60% and 85%; the mass ratio of the clary sage raw material filter residue to the ethanol solution is preferably 1:(4 to 6); the heating treatment is preferably heating under reflux; the heating treatment time is preferably 2 to 4 hours, more preferably 2.5 to 3.5 hours, and even more preferably 3 to 3.5 hours; after the heating treatment, it is preferably filtered and concentrated to obtain a clary sage crude extract; the concentration is preferably concentrated under reduced pressure; in the present invention, it is preferably concentrated to a relative density of 1.05 to 1.09; in the embodiment provided by the present invention, it is specifically concentrated to a relative density of 1.07, 1.06, 1.05 or 1.09.

[0034] The crude clary sage extract is extracted and concentrated with an organic solvent to obtain a clary sage extract; the organic solvent is preferably ethyl acetate; in the present invention, the crude clary sage extract is preferably diluted with water and then extracted with an organic solvent; the concentration is preferably concentrated under reduced pressure; in the present invention, it is preferably concentrated to a relative density of 1.2 to 1.3, more preferably 1.24 to 1.27; in the embodiments provided by the present invention, it is specifically concentrated to a relative density of 1.25, 1.24, 1.26 or 1.27; in the present invention, unless otherwise specified, the relative density refers to the ratio of the density of a substance to the density of water under the same temperature and pressure conditions.

[0035] The sclareol extract is separated and purified by high-speed countercurrent chromatography to obtain a sclareol solution; the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system, preferably propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution; the mass ratio of the propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution is preferably (1-3):(4-6):(1-3):(4-6), more preferably (1.5-2.5):(4.5-5.5):(1.5-2.5):(4.5-5.5), and further preferably 2:5:2:5; in the present invention, the high-speed countercurrent chromatography preferably uses the upper phase of the two-phase ethyl acetate solvent system as the stationary phase and the lower phase as the mobile phase; the pumping speed of the stationary phase is preferably 2.5-3.0 mL / min; in the embodiments provided by the present invention The pumping speed of the stationary phase is specifically 2.5 mL / min, 3 mL / min, 2.8 mL / min or 2.6 mL / min; the main engine speed is preferably 700-800 r / min, more preferably 720-780 r / min, and more preferably 750-760 r / min; the pumping speed of the mobile phase is preferably 2.5-3.0 mL / min; in the embodiment provided by the present invention, the pumping speed of the mobile phase is specifically 2.5 mL / min, 3 mL / min, 2.8 mL / min or 2.6 mL / min; the sclarea extract is preferably first dissolved in the mobile phase and then injected for high-speed countercurrent chromatography separation and purification; the temperature of the high-speed countercurrent chromatography separation and purification is preferably 25°C to 28°C, more preferably 25°C to 26°C.

[0036] The present invention also provides a sclareol solution prepared by the above method; the content of sclareol in the sclareol solution is preferably 94% to 97%.

[0037] The present invention also provides a preparation method of sclarea oil, comprising the following steps: S1) extracting one or more crushed sclarea raw materials by steam distillation to obtain sclarea essential oil and sclarea raw material residue; the sclarea raw materials are selected from one or more of sclarea flowers, sclarea stems and sclarea leaves; S2) mixing the sclarea raw material residue with an ethanol solution, and heating the mixture to obtain a sclarea crude extract; S3) extracting and concentrating the sclarea crude extract with an organic solvent to obtain a sclarea extract; S4) separating and purifying the sclarea extract by high-speed countercurrent chromatography to obtain a sclareol solution; the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system; S5) mixing the sclareol solution with sclarea essential oil to obtain sclarea oil.

[0038] The preparation method of the sclareol solution in steps S1) to S4) is the same as described above and will not be repeated here.

[0039] The sclareol solution is mixed with sclareol essential oil to obtain sclareol oil; the mass ratio of the sclareol solution to sclareol essential oil is preferably (1-2):1, more preferably (1-1.5):1, further preferably (1-1.3):1, and most preferably (1-1.2):1.

[0040] The invention simultaneously carries out extraction of sclareol essential oil and separation of sclareol by high-speed countercurrent chromatography, and then uses the essential oil as a solvent and adds sclareol to obtain new sclareol oil. The new sclareol oil has a high sclareol content, and the preparation method is practical, effective, and highly targeted. The quality of the essential oil is significantly improved, the amber-ambergris aroma is more pronounced, and the smoking effect is better. When applied to cigarettes, the smoking effect of the cigarettes can be greatly improved.

[0041] The present invention also provides a sclarea oil prepared by the above method; the yield of the sclarea oil is specifically 0.22% to 0.31%; and the content of sclareol in the sclarea oil is preferably 40% to 55%.

[0042] The present invention also provides application of the clary sage oil prepared by the method as a tobacco flavoring.

[0043] In order to further illustrate the present invention, the following describes in detail a Clary Sage oil and a preparation method thereof in conjunction with examples.

[0044] The reagents used in the following examples are all commercially available; the particle size of the crushed Clerodendrum sclarea plant material used in the examples is 60 mesh; the mass ratio of flowers, stems, and leaves in the Clerodendrum sclarea plant material is 1:3:6.

[0045] Example 1

[0046] (1) Weigh 800 g of crushed Clerodendrum sclarea plant material, add 4000 g of deionized water into an essential oil extraction device, heat at 100 ° C, collect Clerodendrum sclarea essential oil after the droplets begin to reflux for 4.5 hours, and obtain 1.03 g of Clerodendrum sclarea essential oil.

[0047] (2) Collect the filtered clary sage raw material residue, add 3000 g of 70% ethanol, heat and reflux for 3 h, filter, and concentrate under reduced pressure to a relative density of 1.07 to obtain a clary sage crude extract; then dilute the clary sage crude extract with 600 ml of water, extract with ethyl acetate, separate the liquids, and concentrate under reduced pressure to a relative density of 1.25 to obtain 3.74 g of clary sage extract.

[0048] (3) Weigh 5 L of propylene glycol-ethyl acetate-methanol-0.5% acetic acid (2:5:2:5) solution, shake it thoroughly, and let it stand to separate into layers. The upper layer is the stationary phase and the lower layer is the mobile phase. Dissolve the sclarea extract in 80 mL of the mobile phase to obtain the injection solution for high-speed countercurrent chromatography separation.

[0049] (4) The high-speed countercurrent chromatography separation process conditions are as follows: the upper phase (stationary phase) is pumped in at a flow rate of 2.5 mL / min, the separation temperature is 25°C, the main engine speed is 700 r / min, and the lower phase (mobile phase) is pumped in at a flow rate of 2.5 mL / min. After the mobile phase flows out of the column outlet and the baseline is stable, the injection solution is injected from the injection loop. The components are manually collected according to the different elution times to obtain 1.14 g of sclareol solution with a sclareol content of 95.2%.

[0050] (5) 1.14 g of sclareol solution was added to 1.03 g of sclareol essential oil to obtain 2.17 g of new sclareol oil, whose sclareol content was 50.2%. The yield of the new sclareol oil was 0.27%.

[0051] Example 2

[0052] (1) Weigh 900 g of crushed Clerodendrum sclarea plant material, add 4000 g of deionized water into an essential oil extraction device, heat at 100 ° C, collect Clerodendrum sclarea essential oil after the droplets begin to reflux for 5.0 h, and obtain 1.15 g of Clerodendrum sclarea essential oil.

[0053] (2) The filtered clary sage raw material residue was collected, 4000 g of 80% ethanol was added, and the mixture was heated under reflux for 3 h, filtered, and concentrated under reduced pressure to a relative density of 1.06 to obtain a clary sage crude extract; the clary sage crude extract was then diluted with 500 mL of water, extracted with ethyl acetate, separated, and concentrated under reduced pressure to a relative density of 1.24 to obtain 4.04 g of clary sage extract.

[0054] (3) Weigh 6 L of propylene glycol-ethyl acetate-methanol-0.5% acetic acid (2:5:2:5) solution, shake it thoroughly, and let it stand to separate into layers. The upper layer is the stationary phase and the lower layer is the mobile phase. Dissolve the sclarea extract in 90 mL of the mobile phase to obtain the injection solution for high-speed countercurrent chromatography separation.

[0055] (4) The high-speed countercurrent chromatography separation process conditions are as follows: the upper phase (stationary phase) is pumped in at a flow rate of 3.0 mL / min, the separation temperature is 26°C, the main engine speed is 750 r / min, and the lower phase (mobile phase) is pumped in at a flow rate of 3.0 mL / min. After the mobile phase flows out of the column outlet and the baseline is stable, the injection solution is injected from the injection loop, and the components are manually collected to obtain 1.40 g of sclareol solution with a sclareol content of 95.6%.

[0056] (5) 1.40 g of sclareol solution was added to 1.15 g of sclareol essential oil to obtain 2.57 g of new sclareol oil, whose sclareol content was 51.7%, and the yield of new sclareol oil was 0.32%.

[0057] Example 3

[0058] (1) Weigh 700 g of crushed Clerodendrum sclarea plant material, add 3500 g of deionized water into an essential oil extraction device, heat at 100 ° C, collect Clerodendrum sclarea essential oil after the droplets begin to reflux for 5.0 h, and obtain 0.87 g of Clerodendrum sclarea essential oil.

[0059] (2) The filtered clary sage raw material residue was collected, 3500 g of 85% ethanol was added, and the mixture was heated under reflux for 3.5 h, filtered, and concentrated under reduced pressure to a relative density of 1.05 to obtain a clary sage crude extract; the clary sage crude extract was then diluted with 400 mL of water, extracted with ethyl acetate, separated, and concentrated under reduced pressure to a relative density of 1.26 to obtain 3.25 g of clary sage extract.

[0060] (3) Weigh 5.4 L of propylene glycol-ethyl acetate-methanol-0.5% acetic acid (2:5:2:5) solution, shake it thoroughly, and let it stand to separate into layers. The upper layer is the stationary phase and the lower layer is the mobile phase. Dissolve the sclarea extract in 80 mL of the mobile phase to obtain the injection solution for high-speed countercurrent chromatography separation.

[0061] (4) The high-speed countercurrent chromatography separation process conditions are as follows: the upper phase (stationary phase) is pumped in at a flow rate of 2.8 mL / min, the separation temperature is 26°C, the main engine speed is 760 r / min, and the lower phase (mobile phase) is pumped in at a flow rate of 2.8 mL / min. After the mobile phase flows out of the column outlet and the baseline is stable, the injection solution is injected from the injection loop, and the components are manually collected to obtain 0.91 g of sclareol solution with a sclareol content of 95.3%.

[0062] (5) 0.91 g of sclareol solution was added to 0.87 g of sclareol essential oil to obtain 1.78 g of new sclareol oil, whose sclareol content was 48.7%. The yield of the new sclareol oil was 0.25%.

[0063] Example 4

[0064] (1) Weigh 850 g of crushed Clary Sage plant raw material, add 4500 g of deionized water into an essential oil extraction device, heat at 100 ° C, and collect Clary Sage essential oil after the droplets begin to reflux for 5.0 h to obtain 1.11 g of Clary Sage essential oil.

[0065] (2) The filtered clary sage raw material residue was collected, 4000 g of 60% ethanol was added, and the mixture was heated under reflux for 3.5 h, filtered, and concentrated under reduced pressure to a relative density of 1.09 to obtain a clary sage crude extract; the clary sage crude extract was then diluted with 600 mL of water, extracted with ethyl acetate, separated, and concentrated under reduced pressure to a relative density of 1.27 to obtain 3.91 g of clary sage extract.

[0066] (3) Weigh 5 L of propylene glycol-ethyl acetate-methanol-0.5% acetic acid (2:5:2:5) solution, shake it thoroughly, and let it stand to separate into layers. The upper layer is the stationary phase and the lower layer is the mobile phase. Dissolve the sclarea extract in 80 mL of the mobile phase to obtain the injection solution for high-speed countercurrent chromatography separation.

[0067] (4) The high-speed countercurrent chromatography separation process conditions are as follows: the upper phase (stationary phase) is pumped in at a flow rate of 2.6 mL / min, the separation temperature is 25°C, the main engine speed is 700 r / min, and the lower phase (mobile phase) is pumped in at a flow rate of 2.6 mL / min. After the mobile phase flows out of the column outlet and the baseline is stable, the injection solution is injected from the injection loop, and the components are manually collected to obtain 1.16 g of sclareol solution with a sclareol content of 95.5%.

[0068] (5) 1.16 g of sclareol solution was added to 1.11 g of sclareol essential oil to obtain 2.27 g of new sclareol oil, whose sclareol content was 49.2%. The yield of the new sclareol oil was 0.26%.

[0069] Comparative Example 1

[0070] (1) Weigh 840 g of crushed Clary Sage plant raw material, add 4500 g of deionized water into an essential oil extraction device, heat at 100 ° C, and collect Clary Sage essential oil after the droplets begin to reflux for 5.0 h to obtain 1.07 g of Clary Sage essential oil.

[0071] (2) The filtered clary sage raw material residue was collected, 4000 g of 70% ethanol was added, and the mixture was heated under reflux for 3.5 h, filtered, and concentrated under reduced pressure to a relative density of 1.08 to obtain a clary sage crude extract; the clary sage crude extract was then diluted with 500 mL of water, extracted with ethyl acetate, separated, and concentrated under reduced pressure to a relative density of 1.23 to obtain 4.12 g of clary sage extract.

[0072] (3) Dissolve the clary sage extract in 500 g of 95% ethanol; slowly pass the dissolved clary sage extract solution through a chromatography column packed with 1000 g of AB-8 weakly polar macroporous resin, and track the effluent by gas chromatography until no substances other than the solvent flow out;

[0073] (4) Elution was then performed with 2000 g of dichloromethane until no sclareol was detected; the solvent in the eluate was evaporated under reduced pressure to obtain 1.21 g of gray solid sclareol with a purity of 84%.

[0074] (5) 1.21 g of sclareol powder was added to 1.07 g of sclareol essential oil to obtain 2.27 g of new sclareol oil, whose sclareol content was 44.7%. The yield of the new sclareol oil was 0.27%.

[0075] Comparative Example 2

[0076] (1) Weigh 850 g of crushed Clary Sage plant raw material, add 4500 g of deionized water into an essential oil extraction device, heat at 100 ° C, and collect Clary Sage essential oil after the droplets begin to reflux for 5.0 h to obtain 1.07 g of Clary Sage essential oil.

[0077] (2) The filtered clary sage raw material residue was collected, 4500 g of 80% ethanol was added, and the mixture was heated under reflux for 4.0 h, filtered, and concentrated under reduced pressure to a relative density of 1.05 to obtain a clary sage crude extract; the clary sage crude extract was then diluted with 600 mL of water, extracted with n-butanol, separated, and concentrated under reduced pressure to a relative density of 1.19 to obtain 4.35 g of clary sage extract.

[0078] (3) Weigh 4.5 L of ethyl acetate-n-butanol-methanol-water (1:4:0.5:5) solution, shake it thoroughly, and let it stand to separate the layers. The upper layer is the stationary phase and the lower layer is the mobile phase. Dissolve the sclarea extract in 100 mL of the mobile phase to obtain the injection solution for high-speed countercurrent chromatography separation.

[0079] (4) The high-speed countercurrent chromatography separation process conditions are as follows: the upper phase (stationary phase) is pumped in at a flow rate of 2.4 mL / min, the separation temperature is 25°C, the main engine speed is 800 r / min, and the lower phase (mobile phase) is pumped in at a flow rate of 2.4 mL / min. After the mobile phase flows out of the column outlet and the baseline is stable, the injection solution is injected from the injection loop, and the components are manually collected to obtain 1.27 g of sclareol solution with a sclareol content of 35.5%.

[0080] (5) 1.27 g of sclareol solution was added to 1.07 g of sclareol essential oil to obtain 2.34 g of new sclareol oil, whose sclareol content was 19.3%. The yield of the new sclareol oil was 0.28%.

[0081] The smoking effects of the clary sage essential oil extracted by steam distillation in step (1) of Example 2 and the clary sage oil prepared in Example 2 were compared, and the results are shown in Table 1. As can be seen from Table 1, the clary sage oil prepared in Example 2 has a more pronounced amber (baked, sweet, floral, woody aroma)-ambergris (clear, herbal aroma) aroma, can mask the spicy taste of cigarettes, improve the smoking taste, and has a better smoking effect.

[0082] Table 1 Comparison results of smoking effects of cigarettes

[0083]

[0084]

[0085] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A method for preparing sage oil, characterized in that: The following steps are involved: S1) extracting one or more of the crushed sclarea raw materials by steam distillation to obtain sclarea essential oil and sclarea raw material residue; wherein the sclarea raw materials are selected from one or more of sclarea flowers, sclarea stems and sclarea leaves; S2) mixing the sclarea raw material filter residue with an ethanol solution, and heating the mixture to obtain a sclarea crude extract; S3) extracting and concentrating the crude clary sage extract with an organic solvent to obtain a clary sage extract; S4) separating and purifying the sclareol extract by high-speed countercurrent chromatography to obtain a sclareol solution; the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system; the two-phase ethyl acetate solvent system is propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution; the upper phase of the two-phase ethyl acetate solvent system is used as the stationary phase, and the lower phase is used as the mobile phase; the mass ratio of the propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution is (1-3):(4-6):(1-3):(4-6); the pumping speed of the stationary phase of the high-speed countercurrent chromatography is 2.5-3.0 mL / min; the main engine speed is 700-800 r / min; the pumping speed of the mobile phase is 2.5-3.0 mL / min; the temperature of the high-speed countercurrent chromatography separation and purification is 25° C. to 28° C.; S5) mixing the sclareol solution with sclareol essential oil to obtain sclareol oil; the mass ratio of the sclareol solution to the sclareol essential oil is (1-2):

1.

2. The preparation method according to claim 1, characterized in that In the step S1), the mass ratio of the crushed Clerodendrum sclareae raw material to water during steam distillation extraction is 1:(4-8); The temperature of the steam distillation extraction is 100° C.; the time of the steam distillation extraction is 4 to 6 hours.

3. The preparation method according to claim 1, characterized in that The volume concentration of ethanol in the ethanol solution in step S2) is 60% to 85%; The mass ratio of the sclarea raw material filter residue to the ethanol solution is 1: (4-6); The heating treatment is heating under reflux; the time of the heating treatment is 2 to 4 hours.

4. The preparation method according to claim 1, characterized in that The organic solvent in step S3) is selected from ethyl acetate; and the concentration is performed to a relative density of 1.2 to 1.

3.

5. Clary sclarea oil prepared by the preparation method according to any one of claims 1 to 4.

6. A method for preparing a sclareol solution, characterized in that: The following steps are involved: A1) extracting one or more of the crushed Clary Sage raw materials by steam distillation to obtain Clary Sage essential oil and Clary Sage raw material residue, wherein the Clary Sage raw materials are selected from one or more of Clary Sage flowers, Clary Sage stems, and Clary Sage leaves; A2) mixing the sclarea raw material filter residue with an ethanol solution, and heating the mixture to obtain a sclarea crude extract; A3) extracting and concentrating the crude clary sage extract with an organic solvent to obtain a clary sage extract; A4) separating and purifying the sclareol extract by high-speed countercurrent chromatography to obtain a sclareol solution; the solvent system of the high-speed countercurrent chromatography is a two-phase ethyl acetate solvent system; the two-phase ethyl acetate solvent system is propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution; the upper phase of the two-phase ethyl acetate solvent system is used as the stationary phase, and the lower phase is used as the mobile phase; the mass ratio of the propylene glycol-ethyl acetate-methanol-0.5% acetic acid aqueous solution is (1-3):(4-6):(1-3):(4-6); the stationary phase is pumped at a speed of 2.5-3.0 mL / min for the high-speed countercurrent chromatography; the main engine speed is 700-800 r / min; the mobile phase is pumped at a speed of 2.5-3.0 mL / min; and the temperature for the high-speed countercurrent chromatography separation and purification is 25°C to 28°C.

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