Preparation method for extracting and separating ethyl alternatate from tree moss and application of ethyl alternatate

Abstract

The invention relates to the technical field of tobacco flavors, in particular to a preparation method for extracting and separating ethyl alternatate from tree moss, which comprises the following steps: step 1, placing tree moss raw material powder in an extractor, adding a solvent for hot reflux extraction, collecting an extracting solution part, and concentrating the extracting solution part into absolute oil S1; step 2, uniformly mixing the absolute oil S1 obtained in the step 1 with a solid carrier, adding the mixture into a supercritical CO2 extraction kettle, adding an entrainer at the same time, performing supercritical CO2 extraction, collecting extract liquor, performing freezing suction filtration on the extract liquor to obtain supernate, and concentrating the supernate to obtain tree moss absolute oil S2; 3, molecular distillation is conducted on the tree moss absolute oil S2 obtained in the step 2, needle-shaped crystals are generated on a molecular distillation condenser and a light component collector, after distillation is finished, the crystals on the molecular distillation condenser and the light component collector are dissolved with ethyl alcohol till the crystals are completely dissolved, and a crystal dissolving solution S3 is obtained from the molecular distillation condenser and the light component collector; and step 4, concentrating the crystal dissolving solution S3 obtained in the step 3 until no solvent is distilled off, taking out the crystal dissolving solution S3, and airing and volatilizing at normal temperature to remove the residual solvent, so as to obtain solid powder ethyl alternate.

Description

Technical Field

[0001] The present invention relates to the technical field of tobacco flavorings, and more particularly to a preparation method and application of ethyl erythritol extracted and separated from tree moss. Background Art

[0002] As an important tobacco additive in tobacco flavoring, tree moss absolute oil or extract can give tobacco a moss aroma, soften the smoke, improve the texture and comfort of tobacco, and also act as a fixative. In the prior art, tobacco tree moss absolute oil or extract is in the form of a viscous paste or wax, with a lot of pigments and wax, which leads to poor solubility, fluidity and appearance, and also makes its aroma purity and elegance poor. In addition, the color is too dark, which brings some negative effects.

[0003] At present, in the tobacco industry, there is no research on the preparation and application of ethyl erythritol isolated and purified from tree moss. Chinese patent CN 102041174B subjects tree moss extract to solvent dispersion and degassing, molecular distillation to obtain a primary fraction, and addition to cigarette tobacco; Chinese patent CN 105768198B disperses tree moss extract with ethanol and then molecular distills it, and the obtained fraction is applied to electronic cigarette oil; Chinese patent CN 105837442B dissolves tree moss extract in acetonitrile to obtain a supernatant, concentrates to remove the solvent, and then separates the ethyl erythritol component on a silica gel column; Chinese patent CN117016850A subjects tree moss raw material to ethanol ultrasonic extraction to obtain tree moss extract, and then uses a mixed solvent of n-hexane, ethyl acetate, and acetone to extract and remove insoluble matter to obtain tree moss absolute oil; Chinese patent CN 114806717A crushes tree moss and hydrolyzes it in an acidic environment to obtain a hydrolyzate and a filter residue, which is then subjected to supercritical extraction to obtain an extract, the hydrolyzate and the extract are combined and precipitated with ethanol, and concentrated to obtain a tree moss extract for flavoring tobacco; Chinese patent CN113180286B uses acetonitrile, dimethylformamide or dimethyl sulfoxide as a solvent to extract tree moss to obtain a crude macromolecular depsipeptide solid, which is then refluxed with acetic acid, dimethylformamide, ethylene glycol or dimethyl sulfoxide, cooled to precipitate the solid, and freeze-dried to obtain a pure macromolecular depsipeptide solid. Chinese patent CN 106350225A invented a method of extracting tree moss with an ethanol solution, performing double distillation on the filtrate obtained, precipitating a solid under low temperature conditions, and obtaining a solid tree moss extract for flavoring tobacco or thin slices; Chinese patent CN108192726A invented a method of homogenizing fresh tree moss with water, ultrasonically extracting it with an ethanol solution, concentrating the extract, and then concentrating it again to obtain a tree moss extract, and preparing tree moss absolute oil with molecular distillation; the literature [Jiang Chongyang. Study on the anticancer efficacy and mechanism of action of ethyl erythritol, an active compound of lichens, Kunming Medical University, 2017.] extracts lichens with an ethanol solution, precipitates the concentrate with alcohol to obtain an alcohol precipitate extract, extracts it with chloroform, and separates it by column chromatography to obtain the active ingredient ethyl erythritol, which has anticancer activity. The above studies have the problems of high solvent residues or the use of toxic solvents in many steps. The obtained tree moss absolute oil or extract has complex components or is in poor condition, and the process is not easy to industrialize.

[0004] Therefore, it is necessary to propose a preparation method and application of ethyl erythritol extracted and separated from tree moss to solve the above problems. Summary of the Invention

[0005] In order to overcome at least one defect (shortcoming) of the above-mentioned prior art, the present invention provides a preparation method and application of ethyl erythritol extracted and separated from tree moss.

[0006] To solve the above technical problems, the technical solution of the present invention is as follows: A preparation method for extracting and separating ethyl erythritol from tree moss, comprising the following steps:

[0007] Step 1: Place the tree moss raw material powder in an extractor, add a solvent for hot reflux extraction, collect the extract, and concentrate it into the pure oil S1;

[0008] Step 2: After uniformly mixing the absolute oil S1 obtained in step 1 with a solid carrier, the mixture is added to a supercritical CO2 extraction kettle, and an entrainer is added to perform supercritical CO2 extraction. The extract is collected and frozen and filtered to obtain a supernatant, which is then concentrated to obtain the tree moss absolute oil S2;

[0009] Step 3, molecular distilling the tree moss absolute oil S2 obtained in step 2, generating needle-shaped crystals on the molecular distillation condenser and the light component collector, dissolving the crystals on the molecular distillation condenser and the light component collector with ethanol after the distillation is completed until the crystals are completely dissolved, and obtaining a crystal dissolving liquid S3 from the molecular distillation condenser and the light component collector;

[0010] Step 4, concentrating the crystallization solution S3 obtained in step 3 until no solvent is distilled off, taking it out and drying it at room temperature to evaporate the residual solvent to obtain solid powder ethyl erythritol;

[0011] Furthermore, in step 1, the tree moss raw material powder is placed in an extractor, and a solvent with a mass ratio of 5 to 20 times is added to perform hot reflux extraction for 1 to 4 hours, 1 to 3 times of the extraction time, and concentrated into the pure oil S1.

[0012] Furthermore, the solvent used for extraction in step 1 is one or a mixture of petroleum ether, ethanol, and ethyl acetate.

[0013] Furthermore, in the step 2, the clean oil S1 obtained in the step 1 is evenly mixed with the solid carrier in a mass ratio of 1:0.5 to 5, and then added to a supercritical CO2 extraction kettle. The amount of entrainer is 10 to 40% of the mass of the clean oil S1, the extraction pressure is 10 to 50 MPa, the extraction temperature is 30 to 60°C, and the extraction time is 0.5 to 4 hours to obtain a supercritical extract, which is frozen at -20°C for 12 hours, filtered to obtain a supernatant, and the supernatant is concentrated to obtain the tree moss clean oil S2.

[0014] Furthermore, the solid carrier in step 2 is one of silica gel, macroporous resin, dextran gel, and alumina.

[0015] Furthermore, the entrainer in step 2 is 95% ethanol.

[0016] Furthermore, in step 3, the tree moss absolute oil S2 is molecularly distilled at a distillation temperature of 120-175° C., a distillation speed of 350-550 r / min, and a distillation vacuum of 0.05-4 mbr. Needle-shaped crystals are produced on the molecular distillation condenser and the light component collector. After the distillation is completed, 95% ethanol is used to dissolve the crystals on the molecular distillation condenser and the light component collector until all the crystals are dissolved, and a crystal dissolving liquid S3 is obtained from the molecular distillation condenser and the light component collector.

[0017] The present invention also discloses a preparation method for extracting and separating ethyl erythritol from tree moss, and application of the prepared ethyl erythritol in tobacco.

[0018] Furthermore, the prepared erythritol ethyl ester is dissolved in ethanol, triacetin, caprylic decanoic acid glyceride, and propylene glycol solvents to obtain a mixed solution. When used for flavoring cigarettes, 0.01-3% of the mixed solution is added according to the mass of tobacco cut; when used for flavoring mouth rod tow, 1-10% of the mixed solution is added according to the mass of the plasticizer; when used for flavoring popping beads, 1-25% of the mixed solution is added according to the popping bead solution; when used for flavoring electronic cigarette oil, 0.5-15% of the mixed solution is added according to the mass of the electronic cigarette oil solution; when used for flavoring HNB, 0.05-2% of the mixed solution is added according to the mass of the sheet.

[0019] Compared with the prior art, the beneficial effects of the technical solution of the present invention are:

[0020] The invention discloses a preparation method for extracting and separating ethyl erythritol from tree moss. The method uses tree moss raw materials as research objects, obtains pure oil through solvent extraction, and then uses a carrier to adsorb the pure oil for supercritical extraction to remove wax and pigment, thereby obtaining the tree moss pure oil free of wax and pigment and performing molecular distillation. The method can effectively prevent wax or pigment from adhering to the wall of the distiller during the molecular distillation process, and can also prevent the clogging of the heavy component receiver, and is conducive to the crystallization of ethyl erythritol. During the molecular distillation process, needle-shaped crystals appear on the condenser and the light component collector, and the crystals are then dissolved with a solvent to obtain a crystallization solution, and the crystallization solution is collected. The solid powder is concentrated to obtain the main component of ethyl erythritol. The preparation process is simple, no toxic solvent is used, and ethyl erythritol with a content of more than 75% can be obtained without column chromatography separation and purification. The problem of viscosity, poor fluidity, and poor solubility of tree moss absolute oil or extract, as well as poor aroma elegance and rough smoke when used in tobacco, is solved. The obtained product has a unique moss fragrance, elegant aroma, and good solubility. When used in the tobacco field, it can impart a comfortable moss fragrance, soft smoke, and improved smoking quality. It has good application effects and can be industrially produced. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a structural schematic diagram of the present invention.

[0022] Figure 2 This is the GC-MS total ion current diagram of the volatile components of the target product in Example 2 of the present invention.

[0023] Figure 3 It is the crystal of ethyl erythritol produced in the molecular distillation process of the present invention. DETAILED DESCRIPTION

[0024] The accompanying drawings are for illustrative purposes only and are not to be construed as limitations on this patent. To better illustrate this embodiment, some components of the accompanying drawings may be omitted, enlarged, or reduced in size, and do not represent the actual dimensions of the product. For those skilled in the art, it is understandable that some well-known structures and their descriptions may be omitted from the accompanying drawings.

[0025] In the description of the present invention, it should be noted that, unless otherwise expressly specified or limited, the terms "installation" and "connection" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium, which can be considered as internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on the specific circumstances. The technical solution of the present invention is further described below with reference to the accompanying drawings and embodiments.

[0026] like Figures 1 to 3 As shown, a preparation method for extracting and separating ethyl erythritol from tree moss comprises the following steps:

[0027] Step 1: Place the tree moss raw material powder in an extractor, add a solvent for hot reflux extraction, collect the extract, and concentrate it into the pure oil S1;

[0028] Step 2: After uniformly mixing the absolute oil S1 obtained in step 1 with a solid carrier, the mixture is added to a supercritical CO2 extraction kettle, and an entrainer is added to perform supercritical CO2 extraction. The extract is collected and frozen and filtered to obtain a supernatant, which is then concentrated to obtain the tree moss absolute oil S2;

[0029] Step 3, molecular distilling the tree moss absolute oil S2 obtained in step 2, generating needle-shaped crystals on the molecular distillation condenser and the light component collector, dissolving the crystals on the molecular distillation condenser and the light component collector with ethanol after the distillation is completed until the crystals are completely dissolved, and obtaining a crystal dissolving liquid S3 from the molecular distillation condenser and the light component collector;

[0030] Step 4, concentrating the crystallization solution S3 obtained in step 3 until no solvent is distilled off, taking it out and drying it at room temperature to evaporate the residual solvent to obtain solid powder ethyl erythritol;

[0031] In step 1 of the present invention, tree moss raw material powder is placed in an extractor, and a solvent with a mass ratio of 5 to 20 times is added for hot reflux extraction for 1 to 4 hours, and the extraction times are 1 to 3 times, and the oil is concentrated into pure oil S1, wherein the solvent used for extraction in step 1 is one or a mixture of petroleum ether, ethanol, and ethyl acetate.

[0032] In step 2 of the present invention, the clean oil S1 obtained in step 1 is evenly mixed with a solid carrier in a mass ratio of 1:0.5-5, and then added to a supercritical CO2 extraction kettle, the amount of the entrainer is 10-40% of the mass of the clean oil S1, the extraction pressure is 10-50 MPa, the extraction temperature is 30-60°C, and the extraction time is 0.5-4h to obtain a supercritical extract, which is frozen at -20°C for 12h, filtered to obtain a supernatant, and the supernatant is concentrated to obtain the tree moss clean oil S2, wherein the solid carrier in step 2 is one of silica gel, macroporous resin, dextran gel, and alumina, and the entrainer in step 2 is 95% ethanol.

[0033] In step 3 of the present invention, the tree moss absolute oil S2 is molecularly distilled at a distillation temperature of 120-175° C., a distillation speed of 350-550 r / min, and a distillation vacuum of 0.05-4 mbr. Needle-shaped crystals are generated on the molecular distillation condenser and the light component collector. After the distillation is completed, 95% ethanol is used to dissolve the crystals on the molecular distillation condenser and the light component collector until all the crystals are dissolved, and a crystal dissolving liquid S3 is obtained from the molecular distillation condenser and the light component collector.

[0034] The present invention also discloses a method for extracting and separating ethyl erythritol from tree moss, and the use of the prepared ethyl erythritol in tobacco. When used, the prepared ethyl erythritol is dissolved in ethanol, triacetin, caprylic decanoic acid glyceride, and propylene glycol solvents to obtain a mixed solution. When used for flavoring cigarettes, 0.01 to 3% of the mixed solution is added based on the mass of tobacco shreds; when used for flavoring mouth rod tow, 1 to 10% of the mixed solution is added based on the mass of the plasticizer; when used for flavoring popping beads, 1 to 25% of the mixed solution is added based on the popping bead solution; when used for flavoring electronic cigarette oil, 0.5 to 15% of the mixed solution is added based on the mass of the electronic cigarette oil solution; and when used for flavoring HNB, 0.05 to 2% of the mixed solution is added based on the mass of the flakes.

[0035] Example 1:

[0036] Take 5kg of tree moss raw material powder and place it in an extractor, add 5 times petroleum ether (mass ratio) and heat under reflux for 4h, repeat the extraction 3 times, collect the extract, and concentrate it under reduced pressure to obtain clean oil S1. Take clean oil S1 and silica gel according to a mass ratio of 1:3 and mix them evenly so that the clean oil S1 is fully adsorbed on the silica gel, add it to the supercritical CO2 extraction kettle, and add 95% ethanol to the entrainer tank at the same time. The entrainer amount is 30% of the mass of the clean oil S1. The supercritical CO2 extraction pressure is 35MPa, the extraction temperature is 45℃, the extraction time is 3h, the extract is collected and frozen at -20℃ for 12h, and the supernatant is filtered. The liquid was concentrated under reduced pressure to obtain tree moss pure oil S2, 200 g of the tree moss pure oil S2 was taken for molecular distillation, the distillation temperature was 160° C., the distillation speed was 400 r / min, and the distillation vacuum degree was 0.9 mbr. After the distillation, 95% ethanol was used to dissolve the crystals on the molecular distillation condenser and the light component collector until the crystals were completely dissolved, and the crystal dissolving liquid S3 was collected from the molecular distillation condenser and the light component collector; the crystal dissolving liquid S3 was concentrated under reduced pressure until no solvent was distilled out, and the solid powder was taken out and dried at room temperature to remove the residual solvent to obtain the red star itaconic acid ethyl ester of the present invention. GC-MS detection showed that the red star itaconic acid ethyl ester content was 78.31%.

[0037] The ethyl erythritol prepared above was dissolved in 95% ethanol to form a 1% ethanol solution with flavoring essence, and added to the tobacco of a certain tobacco leaf group, adding 0.1% according to the mass of the tobacco. The solution was evaluated by smoking experts. Compared with the control sample, the solution can significantly give the cigarette a fresh moss fragrance, the smoke is soft and comfortable, and the texture is improved.

[0038] Example 2:

[0039] Take 5kg of tree moss raw material powder and place it in an extractor, add 10 times (mass ratio) of 95% ethanol and heat under reflux for 2h, repeat the extraction twice, collect the extract, and concentrate it under reduced pressure to obtain clean oil S1. Take the clean oil S1 and alumina according to a mass ratio of 1:0.5 and mix them evenly so that the clean oil S1 is fully adsorbed on the alumina, add it to the supercritical CO2 extraction kettle, and add 95% ethanol to the entrainer tank at the same time. The entrainer amount is 40% of the mass of the clean oil S1. The supercritical CO2 extraction pressure is 50MPa, the extraction temperature is 30℃, the extraction time is 0.5h, and the extract is collected and frozen at -20℃ for 12h. The supernatant is filtered and concentrated under reduced pressure to obtain tree moss pure oil S2. 200 g of tree moss pure oil S2 is taken for molecular distillation at a distillation temperature of 175° C., a distillation speed of 500 r / min, and a distillation vacuum of 4 mbr. After the distillation is completed, 95% ethanol is used to dissolve the crystals on the molecular distillation condenser and the light component collector until all the crystals are dissolved. The crystal dissolving liquid S3 is collected from the molecular distillation condenser and the light component collector, and the crystal dissolving liquid S3 is concentrated under reduced pressure until no solvent is distilled out. The solid powder is taken out and dried at room temperature to obtain the ethyl ester of the present invention. GC-MS detection shows that the content of ethyl ester of the present invention is 85.72%.

[0040] The ethyl ester of red star itchitonate prepared above was dissolved in glyceryl caprylate to form a 1% popping bead essence, and 15% was added according to the mass of the popping bead solution. The smoke was evaluated by smoking experts. Compared with the control sample, it significantly gave the smoke a fresh moss fragrance, soft smoke, reduced irritation, and a clean aftertaste.

[0041] Table 1 GC-MS test results of volatile components of target product of Example 2

[0042] Serial number Retention time (min) Compound name Peak area normalized percentage content (%) 1 20.54 Morinaldehyde 1.24 2 24.02 Mossinoic acid 1.49 3 24.35 Ethyl acetate 85.72 4 25.19 Ethyl hydantoin 2.03 5 28.36 Ethyl palmitate 2.12 6 30.96 Ethyl linoleate 1.67

[0043] Example 3:

[0044] Take 5kg of tree moss raw material powder and place it in an extractor, add 20 times (mass ratio) of ethyl acetate and heat under reflux for 3h, extract once, collect the extract, and concentrate it under reduced pressure to obtain pure oil S1. Take pure oil S1 and macroporous resin and mix them evenly in a mass ratio of 1:5, add them to a supercritical CO2 extraction kettle, and add 95% ethanol to the entrainer tank at the same time. The entrainer amount is 10% of the mass of the pure oil S1. The supercritical CO2 extraction pressure is 10MPa, the extraction temperature is 60℃, the extraction time is 2h, the extract is collected and frozen at -20℃ for 12h, and the supernatant is filtered to obtain the supernatant. The tree moss pure oil S2 was obtained by vacuum concentration. 200 g of the tree moss pure oil S2 was molecularly distilled at a distillation temperature of 120° C., a distillation speed of 350 r / min, and a distillation vacuum of 0.05 mbr. After the distillation, 95% ethanol was used to dissolve the crystals on the molecular distillation condenser and the light component collector until all the crystals were dissolved. The crystal dissolution liquid S3 was collected from the molecular distillation condenser and the light component collector. The crystal dissolution liquid was vacuum concentrated until no solvent was distilled out, and the solid powder was taken out and dried at room temperature to obtain the ethyl ester of the present invention. GC-MS detection showed that the ethyl ester content was 75.28%.

[0045] The ethyl erythritol prepared above was dissolved in triacetin to form a 1% filter rod flavoring essence, and 2% was added according to the mass of the plasticizer. The smoke was evaluated by smoking experts. Compared with the control sample, the smoke gave the cigarette a mossy aroma, which was elegant and clean, with a long aftertaste.

[0046] Example 4:

[0047] Take 5kg of tree moss raw material powder and place it in an extractor, add 8 times (mass ratio) of ethyl acetate and heat under reflux for 2h, extract twice, and concentrate under reduced pressure to obtain pure oil S1. Take pure oil S1 and dextran gel according to a mass ratio of 1:1 and mix them evenly, add them to a supercritical CO2 extraction kettle, and add 95% ethanol to the entrainer tank at the same time. The entrainer amount is 20% of the mass of the pure oil S1. The supercritical CO2 extraction pressure is 20MPa, the extraction temperature is 40℃, the extraction time is 1.5h, the extract is collected and frozen at -20℃ for 12h, the supernatant is filtered, and the supernatant is concentrated under reduced pressure. The method comprises the following steps: obtaining tree moss pure oil S2, taking 200 g of the tree moss pure oil S2 for molecular distillation at a distillation temperature of 140° C., a distillation speed of 550 r / min, and a distillation vacuum degree of 1 mbr. After the distillation, dissolving the crystals on the molecular distillation condenser and the light component collector with 95% ethanol until all the crystals are dissolved, collecting the crystal dissolving liquid S3 from the molecular distillation condenser and the light component collector, concentrating the crystal dissolving liquid under reduced pressure until no solvent is distilled out, taking out and drying at room temperature to obtain a solid powder, which is the ethyl ester of the present invention. GC-MS detection shows that the ethyl ester content is 81.87%.

[0048] The ethyl erythritol prepared above was dissolved in 95% ethanol to form a 10% ethanol solution, which was then diluted with propylene glycol to a concentration of 1%. The solution was then added to the e-cigarette oil at a concentration of 1% based on the mass of the e-cigarette oil solution. The control sample was the e-cigarette oil to which this component was not added. The e-cigarette oil was evaluated by smoking experts. Compared with the control sample, the e-cigarette oil had a light mossy and earthy aroma, which was elegant and comfortable.

[0049] Example 5:

[0050] Take 5kg of tree moss raw material powder and place it in an extractor, add 15 times (mass ratio) petroleum ether: 95% ethanol (3:2), heat and reflux for 1h, extract twice, and concentrate under reduced pressure to obtain pure oil S1; take the pure oil and silica gel according to the mass ratio of 1:2, mix and stir evenly, add it to the supercritical CO2 extraction kettle, and add 95% ethanol to the entrainer tank at the same time. The entrainer amount is 15% of the mass of the pure oil S1, the supercritical CO2 extraction pressure is 30MPa, the extraction temperature is 50℃, the extraction time is 4h, the extract is collected and frozen at -20℃ for 12h, the supernatant is filtered, and the supernatant is decompressed The tree moss pure oil S2 is concentrated, and 200 g of the tree moss pure oil S2 is subjected to molecular distillation at a distillation temperature of 130° C., a distillation speed of 450 r / min, and a distillation vacuum degree of 0.5 mbr. After the distillation is completed, 95% ethanol is used to dissolve the crystals on the molecular distillation condenser and the light component collector until the crystals are completely dissolved. The crystal dissolution liquid S3 is collected from the molecular distillation condenser and the light component collector, and the crystal dissolution liquid is reduced in pressure and concentrated until no solvent is distilled out. The solid powder is taken out and dried at room temperature to obtain the ethyl ester of the present invention. GC-MS detection shows that the ethyl ester content is 83.65%.

[0051] The ethyl ester of erythritol prepared above was dissolved in 95% ethanol to form a 10% solution, which was then diluted with propylene glycol to a concentration of 0.5% for HNB flavoring. 0.6% was added according to the mass of the flakes. The control sample was a flake without this component added. When smoked by a smoking expert, the smoke had a light mossy, refreshing and woody aroma compared to the control sample, with a soft smoke and a clean aftertaste.

[0052] In the figure, the description of the positional relationship is only for illustrative purposes and should not be understood as a limitation on this patent; obviously, the above embodiments of the present invention are only examples for clearly illustrating the present invention, and are not limitations on the implementation methods of the present invention. For ordinary technicians in the relevant field, other different forms of changes or modifications can be made on the basis of the above description. It is not necessary and impossible to list all the implementation methods here. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the claims of the present invention.

Claims

1. A method for extracting and separating ethyl erythritol from tree moss, characterized in that: The following steps are involved: Step 1: Place the tree moss raw material powder in an extractor, add a solvent for hot reflux extraction, collect the extract, and concentrate it into the pure oil S1; Step 2: After uniformly mixing the absolute oil S1 obtained in step 1 with a solid carrier, the mixture is added to a supercritical CO2 extraction kettle, and an entrainer is added to perform supercritical CO2 extraction. The extract is collected and frozen and filtered to obtain a supernatant, which is then concentrated to obtain the tree moss absolute oil S2; Step 3, molecular distilling the tree moss absolute oil S2 obtained in step 2, generating needle-shaped crystals on the molecular distillation condenser and the light component collector, dissolving the crystals on the molecular distillation condenser and the light component collector with ethanol after the distillation is completed until the crystals are completely dissolved, and obtaining a crystal dissolving liquid S3 from the molecular distillation condenser and the light component collector; Step 4: Concentrate the crystallization solution S3 obtained in step 3 until no solvent is distilled out, take it out and dry it at room temperature to evaporate and remove the residual solvent to obtain solid powder ethyl erythritol.

2. The method for extracting and separating ethyl erythritol from tree moss according to claim 1, wherein: In the step 1, the tree moss raw material powder is placed in an extractor, and a solvent with a mass ratio of 5 to 20 times is added to perform hot reflux extraction for 1 to 4 hours, the extraction times are 1 to 3 times, and the oil is concentrated into the pure oil S1.

3. The method for extracting and separating ethyl erythritol from tree moss according to claim 1, wherein: The solvent used for extraction in step 1 is one or a mixture of petroleum ether, ethanol, and ethyl acetate.

4. The method for extracting and separating ethyl erythritol from tree moss according to claim 1, wherein: In the step 2, the clean oil S1 obtained in the step 1 is evenly mixed with the solid carrier in a mass ratio of 1:0.5-5, and then added to a supercritical CO2 extraction kettle. The amount of entrainer used is 10-40% of the mass of the clean oil S1, the extraction pressure is 10-50 MPa, the extraction temperature is 30-60°C, and the extraction time is 0.5-4h to obtain a supercritical extract, which is frozen at -20°C for 12h, filtered to obtain a supernatant, and the supernatant is concentrated to obtain the tree moss clean oil S2.

5. The method for extracting and separating ethyl erythritol from tree moss according to claim 1, wherein: The solid carrier in step 2 is one of silica gel, macroporous resin, dextran gel and alumina.

6. The method for extracting and separating ethyl erythritol from tree moss according to claim 1, wherein: The entrainer in step 2 is 95% ethanol.

7. The method for extracting and separating ethyl erythritol from tree moss according to claim 1, wherein: In the step 3, the tree moss absolute oil S2 is molecularly distilled at a distillation temperature of 120 to 175° C., a distillation speed of 350 to 550 r / min, and a distillation vacuum of 0.05 to 4 mbr. Needle-shaped crystals are generated on the molecular distillation condenser and the light component collector. After the distillation is completed, 95% ethanol is used to dissolve the crystals on the molecular distillation condenser and the light component collector until all the crystals are dissolved, and a crystal dissolving liquid S3 is obtained from the molecular distillation condenser and the light component collector.

8. Use of ethyl erythritol prepared by the method for extracting and separating ethyl erythritol from tree moss according to any one of claims 1 to 6 in tobacco.

9. The use of ethyl erythritol in tobacco according to claim 7, characterized in that: The prepared erythritol ethyl ester is dissolved in ethanol, triacetin, caprylic decanoic acid glyceride and propylene glycol solvents to obtain a mixed solution. When used for flavoring cigarettes, 0.01-3% of the mixed solution is added based on the weight of tobacco cut; when used for flavoring mouth rod tow, 1-10% of the mixed solution is added based on the weight of the plasticizer; when used for flavoring popping beads, 1-25% of the mixed solution is added based on the popping bead solution; when used for flavoring electronic cigarette oil, 0.5-15% of the mixed solution is added based on the weight of the electronic cigarette oil solution; and when used for flavoring HNB, 0.05-2% of the mixed solution is added based on the weight of the flakes.

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