A method for extracting tree moss absolute oil for electronic cigarettes

Abstract

The present application relates to the technical field of natural flavor extraction, and specifically discloses a method for extracting tree moss absolute oil for electronic cigarettes; the method for extracting tree moss absolute oil for electronic cigarettes comprises the following steps: S1, preparing tree moss raw material: drying and crushing the tree moss to obtain tree moss powder; S2, preparing tree moss extract: ultrasonically extracting the tree moss powder, and concentrating the extract after extraction until no solvent is evaporated to obtain tree moss extract; S3, preparing tree moss absolute oil: S31, adding an extracting solution to the tree moss extract and stirring, stirring evenly to obtain a first solution; S32, freezing the first solution at a temperature of ‑10‑30°C for 10‑30 hours, filtering to remove insoluble matter, and obtaining a second solution; S33, concentrating the second solution until no solvent is evaporated to obtain tree moss absolute oil; the extracting solution is a mixture of n-hexane, ethyl acetate, and acetone; the tree moss absolute oil extraction method of the present application has a high extraction rate.

Description

Technical Field

[0001] The present application relates to the technical field of natural flavor extraction, and more specifically, to a method for extracting tree moss absolute oil for electronic cigarettes. Background Art

[0002] Tree moss, also known as clump-shaped tree flower or tree flower vegetable, is an epiphytic lichen found on pine, fir, oak, spruce, or fir trees. It possesses a unique, natural, green aroma and a rich, resinous flavor. Currently, tree moss extracts are widely used in daily chemicals, foods, and tobacco flavors. In particular, tobacco companies are increasingly using tree moss to impart unique aromas to their cigarettes.

[0003] Moss extract has a unique hay fragrance and rich resin aroma, while moss absolute has a long-lasting herbal flavor. Used in tobacco flavoring, it enhances the fragrance and natural flavor, masks unpleasant and earthy tobacco odors, and improves the taste of smoke.

[0004] Patent CN 106318617 A discloses a method for preparing low-As moss absolute. This method first extracts the oil using ethanol or petroleum ether, concentrates it, and produces a moss extract. The extract is then further extracted to produce the absolute. Moss absolute is prepared from commercially available moss absolute using molecular distillation. The process involves ethanol resolubilization and freeze separation, including freezing at -10-30°C for 8-24 hours. However, this method is complex and results in a low absolute extraction rate. Summary of the Invention

[0005] In order to improve the extraction rate of tree moss absolute oil, the present application provides a method for extracting tree moss absolute oil for electronic cigarettes.

[0006] In a first aspect, the present application provides a method for extracting tree moss absolute for electronic cigarettes, which adopts the following technical solution: A method for extracting tree moss absolute for electronic cigarettes, comprising the following steps:

[0007] S1. Preparation of tree moss raw material: drying the tree moss at a temperature of 65-85° C. for 12-36 hours, and then crushing the tree moss to obtain tree moss powder;

[0008] S2. Preparation of tree moss extract: adding ethanol to tree moss powder, ultrasonically extracting the tree moss powder, and concentrating the extract until no solvent is removed by distillation to obtain the tree moss extract;

[0009] S3. Preparation of moss absolute: S31. Add the extract to the moss extract and stir until uniformly mixed to obtain a first solution; S32. Freeze the first solution at -10-30°C for 10-30 hours, filter and remove insoluble matter to obtain a second solution; S33. Concentrate the second solution until no solvent is removed by distillation to obtain moss absolute;

[0010] The extract is a mixture of n-hexane, ethyl acetate and acetone.

[0011] By adopting the above technical solution, in this application, the tree moss is dried and recovered to produce tree moss powder, and then the tree moss powder is extracted with ethanol to produce tree moss extract, and then the tree moss extract is further extracted to produce tree moss absolute oil. The solvent used in the extraction should be able to fully dissolve the tobacco extract and be easy to separate and recover after extraction. Among them, the extracting liquid for extracting the tree moss absolute oil in this application is a mixture of n-hexane, ethyl acetate, and acetone. The polarity of n-hexane and acetone is very different. Ethyl acetate has moderate polarity compared with n-hexane and acetone. A mixture of three solvents with different polarities is used as the extracting liquid. After the three are mixed, the polarity of the extracting liquid also changes, and its ability to dissolve the extract also changes, which can accelerate the penetration of the extracting liquid into the raw material, and can fully dissolve and extract the effective ingredients in the tree moss extract, thereby improving the extraction rate of the tree moss absolute oil.

[0012] Preferably, the extract comprises the following components in parts by weight: 5-10 parts of n-hexane, 5-15 parts of ethyl acetate, and 1-5 parts of acetone.

[0013] By adopting the above technical solution, the present application prepares an extracting liquid from n-hexane, ethyl acetate and acetone for the extraction of tree moss absolute oil. By optimizing the ratio between n-hexane, ethyl acetate and acetone, the prepared extracting liquid can fully extract the effective ingredients in the tree moss extract to prepare the tree moss absolute oil. When the ratio between n-hexane, ethyl acetate and acetone is 8:10:3, the extraction efficiency of the raw material after the extracting liquid is high, and the extracted tree moss absolute oil in the electronic cigarette has a rich and refreshing aroma; a pure aftertaste, and a good flavoring effect.

[0014] Preferably, the extract further comprises 5-10 parts by weight of tert-butanol.

[0015] By adopting the above technical solution, the extract of the present application also includes a certain weight portion of tert-butanol. Tert-butanol has a lower boiling point and is less polar than ethyl acetate and acetone. It can be fully evaporated during evaporation, leaving less residue, thereby improving the extraction rate of tree moss absolute oil.

[0016] Preferably, the amount of the extract added in step S31 is 5-10 times the amount of the tree moss extract.

[0017] By adopting the above technical solution, the amount of extract used in this application is 5-10 times that of the tree moss extract. Compared with other extracts, the usage amount is less, and the final extraction rate of the tree moss is higher. When used within the dosage range specified in this application, the extraction rate of the tree moss absolute oil is high.

[0018] Preferably, the average particle size of the tree moss powder is 20-60 mesh.

[0019] By adopting the above technical solution, the smaller the average particle size of the tree moss powder is, the better its solubility in the extract during extraction, and the effective ingredients therein can be fully dissolved and extracted, thereby improving the extraction rate of the tree moss absolute oil. In addition, the extracted tree moss absolute oil in the electronic cigarette has a rich and refreshing aroma; the aftertaste is pure, and the flavoring effect is better.

[0020] Preferably, the step S2 is carried out at a temperature of 40-50° C., with each ultrasonic extraction lasting 30-60 minutes and the extractions being performed 2-3 times.

[0021] By adopting the above-mentioned technical solution, the preparation method of tree moss absolute oil for electronic cigarettes of the present application uses ultrasonic extraction on the tree moss raw material, which can enable the solvent to quickly enter the interior of the cells and fully extract the effective ingredients. Moreover, the process is carried out under low temperature conditions, which can avoid the effective ingredients from being destroyed by heat and improve the aroma quality of the product.

[0022] Preferably, the amount of ethanol added is 4-6 times that of the tree moss powder.

[0023] By adopting the above technical solution, the present application further limits the amount of ethanol added relative to the tree moss powder in step S2. Within this range, the amount of ethanol added has no obvious effect on the preparation of the tree moss extract and the final extraction rate of the tree moss absolute oil.

[0024] Preferably, low-temperature vacuum concentration is adopted in step S33, and the temperature during concentration is 40-50°C.

[0025] By adopting the above technical solution, the present application further limits the temperature during concentration in step S33. When the temperature during concentration is within this range, it has no significant effect on the final extraction rate of the tree moss absolute oil.

[0026] Preferably, in step S33, molecular distillation is used to obtain tree moss absolute.

[0027] In summary, this application has the following beneficial effects:

[0028] 1. In the present application, the tree moss is dried and recovered to produce tree moss powder, and then the tree moss powder is extracted with ethanol to produce tree moss extract, and then the tree moss extract is further extracted to produce tree moss absolute oil. The solvent used in the extraction should be able to fully dissolve the tobacco extract and be easy to separate and recover after extraction. Among them, the extracting liquid for extracting the tree moss absolute oil in the present application is a mixture of n-hexane, ethyl acetate, and acetone. The polarity of n-hexane and acetone is very different. Ethyl acetate has moderate polarity compared with n-hexane and acetone. A mixture of three solvents with different polarities is used as the extracting liquid. After the three are mixed, the polarity of the extracting liquid also changes, and its ability to dissolve the extract also changes, which can accelerate the penetration of the extracting liquid into the raw material, and can fully dissolve and extract the effective ingredients in the tree moss extract, thereby improving the extraction rate of the tree moss absolute oil.

[0029] 2. In this application, an extracting liquid prepared by combining n-hexane, ethyl acetate and acetone is used for the extraction of tree moss absolute oil. By optimizing the ratio between n-hexane, ethyl acetate and acetone, the prepared extracting liquid can fully extract the effective ingredients in the tree moss extract to prepare the tree moss absolute oil. When the ratio between n-hexane, ethyl acetate and acetone is 8:10:3, the extraction efficiency of the raw material after the extracting liquid is higher, and the extracted tree moss absolute oil in the electronic cigarette has a rich and refreshing aroma; the aftertaste is pure, and the flavoring effect is better.

[0030] 3. The final extraction rate and flavoring effect of the tree moss absolute oil for electronic cigarettes prepared in this application were tested, and it was found that the extraction rate could reach up to 13.9%. The flavoring effect of the prepared tree moss absolute oil in cigarettes is rich and fresh; the aftertaste is pure and sweet, and the flavoring effect is better. DETAILED DESCRIPTION

[0031] The present application is further described in detail below with reference to the embodiments.

[0032] raw material

[0033] The raw materials used in this application are all common commercially available materials.

[0034] Preparation Example

[0035] Preparation Examples 1-3

[0036] An extract of Preparation Example 1-3 was prepared using the following raw materials and their amounts as shown in Table 1:

[0037] Weigh the raw materials according to the amounts in Table 1, and then stir them evenly to obtain the extract.

[0038] Table 1 Raw materials and amounts of each raw material used in the extracts of Preparation Examples 1-3 (kg)

[0039] Preparation Example 1 Preparation Example 2 Preparation Example 3 n-hexane 5 8 10 Ethyl acetate 15 10 5 acetone 1 3 5

[0040] Example

[0041] Example 1

[0042] A method for extracting tree moss absolute for electronic cigarettes comprises the following steps:

[0043] S1. Preparation of tree moss raw material: drying the tree moss at 80° C. for 36 h, and then crushing the tree moss into particles with an average particle size of 20 mesh to obtain tree moss powder;

[0044] S2. Preparation of tree moss extract: Add 95% ethanol by mass to the tree moss powder, the amount of ethanol added being 4 times the amount of the tree moss powder. Ultrasonic extraction is performed on the tree moss powder at 40°C for 30 minutes each time, for two extractions. After the extraction, the extract is concentrated under reduced pressure until no solvent is removed by distillation to obtain the tree moss extract.

[0045] S3. Preparation of tree moss absolute oil: S31. Add extracting solution to tree moss extract and stir it. The amount of extracting solution added is 5 times the amount of tree moss extract. Stir evenly to obtain a first solution. S32. Freeze the first solution at -10°C for 10 hours, filter out insoluble matter, and obtain a second solution. S33. Concentrate the second solution until no solvent is evaporated to obtain tree moss absolute oil.

[0046] The extract is from Preparation Example 1.

[0047] Example 2

[0048] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that the extract in step S3 comes from Preparation Example 2, and the remaining steps are the same as those in Example 1.

[0049] Example 3

[0050] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that the extract in step S3 comes from Preparation Example 3, and the remaining steps are the same as those in Example 1.

[0051] Example 4

[0052] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that the extract further includes 5 kg of tert-butanol, and the remaining steps are the same as those in Example 1.

[0053] Example 5

[0054] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that the extract further includes 8 kg of tert-butanol, and the remaining steps are the same as those in Example 1.

[0055] Example 6

[0056] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that the extract further includes 10 kg of tert-butanol, and the remaining steps are the same as those in Example 1.

[0057] Example 7

[0058] A method for extracting tree moss absolute oil for electronic cigarettes is different from that of Example 5 in that the total amount of the extract added in step S3 is 8 times the amount of the tree moss extract, and the remaining steps are the same as those of Example 5.

[0059] Example 8

[0060] A method for extracting tree moss absolute oil for electronic cigarettes is different from that of Example 5 in that the total amount of the extract added in step S3 is 10 times the amount of the tree moss extract, and the remaining steps are the same as those of Example 5.

[0061] Example 9

[0062] A method for extracting tree moss absolute oil for electronic cigarettes is different from that of Example 7 in that the average particle size of the tree moss powder is 40 mesh, and the remaining steps are the same as those of Example 7.

[0063] Example 10

[0064] A method for extracting tree moss absolute oil for electronic cigarettes is different from that of Example 7 in that the average particle size of the tree moss powder is 60 mesh, and the remaining steps are the same as those of Example 7.

[0065] Example 11

[0066] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 10 in that, in step S2, the tree moss powder is ultrasonically extracted, each ultrasonic extraction lasts 30 minutes, and the extraction is performed three times. The remaining steps are the same as those in Example 10.

[0067] Example 12

[0068] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 10 in that, in step S2, the tree moss powder is ultrasonically extracted, each ultrasonic extraction lasts 60 minutes, and the extraction is performed twice. The remaining steps are the same as those in Example 10.

[0069] Example 13

[0070] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 10 in that, in step S2, the tree moss powder is ultrasonically extracted, each ultrasonic extraction lasts 60 minutes, and the extraction is performed three times. The remaining steps are the same as those in Example 10.

[0071] Comparative Example

[0072] Comparative Example 1

[0073] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that an equal amount of n-hexane (i.e., 21 kg of n-hexane) is used as the extract in step S3, and the remaining steps are the same as those in Example 1.

[0074] Comparative Example 2

[0075] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that an equal amount of ethyl acetate (i.e., 21 kg of ethyl acetate) is used as the extract in step S3, and the remaining steps are the same as those in Example 1.

[0076] Comparative Example 3

[0077] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 1 in that an equal amount of acetone (i.e., 21 kg of acetone) is used as the extract in step S3, and the remaining steps are the same as those in Example 1.

[0078] Comparative Example 4

[0079] A method for extracting tree moss absolute oil for electronic cigarettes is different from that in Example 2 in that the amount of the mixed solution of n-hexane, ethyl acetate and acetone added in step S3 is twice the amount of the tree moss extract, and the remaining steps are the same as those in Example 2.

[0080] Comparative Example 5

[0081] A method for extracting tree moss absolute oil for electronic cigarettes is different from that of Example 13 in that, in step S2, the tree moss powder is ultrasonically extracted, each ultrasonic extraction lasts for 90 minutes, and the extraction is performed three times. The remaining steps are the same as those of Example 13.

[0082] Comparative Example 6

[0083] A method for extracting tree moss absolute oil for electronic cigarettes is different from that of Example 13 in that, in step S2, the tree moss powder is ultrasonically extracted, each ultrasonic extraction lasts for 90 minutes, and the extraction is performed four times. The remaining steps are the same as those of Example 10.

[0084] Performance testing

[0085] Detection method / test method

[0086] The following performance tests were performed on the tree moss absolute for electronic cigarettes prepared in Examples 1-13 and Comparative Examples 1-6. The test results are shown in Tables 2 and 3.

[0087] Determination of the extraction rate of tree moss absolute oil: extraction rate of tree moss absolute oil = (mass of tree moss absolute oil / mass of tree moss powder) × 100%.

[0088] Table 2 Extraction rate of tree moss absolute oil of Examples 1-13 and Comparative Examples 1-6

[0089]

[0090]

[0091] The flavoring effect of tree moss absolute oil: dilute the tree moss absolute oil with 95% ethanol to a 5% tree moss absolute oil solution, weigh shredded tobacco and spray it evenly on the shredded tobacco at a dosage of 0.02% (based on the weight of the shredded tobacco), seal the flavored shredded tobacco for 4 hours, dry it in an oven at 100°C to make cigarettes, and equilibrate them in a constant temperature and humidity chamber (temperature 22°C ± 1°C, relative humidity 60% ± 2%) for 24 hours. Ask the smoking experts from the Yunnan Tobacco Science Research Institute to conduct smoking evaluation according to the method specified in YC / T138-1998.

[0092] Table 3 Test results of Examples 1-13 and Comparative Examples 1-6

[0093]

[0094]

[0095] Combined with the test results in Tables 2 and 3 of Examples 1-3, it can be seen that in the process of preparing the tree moss absolute, when the amounts of n-hexane, ethyl acetate, and acetone added to the extract in step S3 are 8 kg, 10 kg, and 3 kg, respectively, the extraction rate of the obtained tree moss absolute is high, and the flavoring effect of the tree moss absolute prepared in Example 2 in cigarettes is rich and fresh; the aftertaste is pure, and the effect is good.

[0096] Combining the test results of Example 2 and Examples 4-6 in Table 2 and Table 3, it can be seen that the addition of tert-butanol to the extract is beneficial to improving the extraction rate of the tree moss absolute oil. As the amount of tert-butanol added increases, the extraction rate of the tree moss absolute oil gradually increases. When the amount of tert-butanol added is 8 kg or more, the extraction rate of the obtained tree moss absolute oil is relatively high, and the extraction rate can reach 7.4%. The flavoring effect of the obtained tree moss absolute in cigarettes is rich and fresh; the aftertaste is pure, and the effect is good.

[0097] Combined with the test results of Examples 5 and 7-8 in Tables 2 and 3, it can be seen that in the process of preparing the tree moss absolute, when the total amount of the extract added in the preparation step S3 is 8 times the amount of the tree moss extract, the extraction rate of the obtained tree moss absolute is higher, and the flavoring effect of the tree moss absolute prepared in Example 7 in cigarettes is rich and fresh; the aftertaste is pure, and the effect is better.

[0098] From the test results of Examples 7, 9-10 in Tables 2 and 3, it can be seen that the smaller the average particle size of the tree moss powder, the higher the extraction rate of the tree moss absolute oil obtained. When the average particle size of the tree moss powder is 60 mesh, the extraction rate of the tree moss absolute oil is 10.2%. The flavoring effect of the tree moss absolute oil prepared in Example 7 in cigarettes is rich and fresh; the aftertaste is pure and sweet, and the effect is better.

[0099] Combined with the test results of Example 10 and Examples 11-13 in Table 2 and Table 3, it can be seen that when ultrasonic extraction of tree moss powder is performed, the longer the ultrasonic extraction time and the more extraction times, the higher the extraction rate of the tree moss absolute oil finally obtained. When the ultrasonic extraction time is 60 minutes each time and the extraction is performed 3 times, the extraction rate of the obtained tree moss absolute oil is 13.9%. The flavoring effect of the tree moss absolute oil prepared in Example 10 in cigarettes is rich and fresh; the aftertaste is pure and sweet, and the effect is better.

[0100] Combined with the test results of Example 10 and Comparative Examples 5-6, it can be seen that the extraction rate of tree moss absolute oil reaches the optimal value when the ultrasonic extraction time is 60 min and the extraction is performed 3 times. Increasing the ultrasonic time and the number of ultrasonic times will not increase the extraction rate of tree moss absolute oil, indicating that the ultrasonic extraction of 60 min and 3 times in this application is the optimal process step.

[0101] Combining the test data of Example 1 and Comparative Examples 1-3, it can be seen that when the extracting liquid is a mixture of n-hexane, acetone, and ethyl acetate, the extraction rate of the obtained tree moss absolute oil is higher, indicating that the use of a mixture of n-hexane, acetone, and ethyl acetate is more effective than using any one of the components alone as an extracting liquid. This further demonstrates that n-hexane, acetone, and ethyl acetate have a synergistic effect, which is beneficial to improving the extraction rate of the tree moss absolute oil.

[0102] Combining the test data of Example 2 and Comparative Example 4, it can be seen that when the amount of the extract is twice the amount of the moss extract, the extraction rate of the moss absolute is low, and the extraction of the moss absolute is ultimately insufficient; and when the amount of the extract is 5 times the amount of the moss extract, the extraction rate of the moss absolute is the highest, indicating that this amount is the optimal amount.

[0103] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A method for extracting tree moss absolute for electronic cigarettes, characterized in that: The following steps are involved: S1. Preparation of tree moss raw material: drying the tree moss at a temperature of 65-85° C. for 12-36 hours, and then crushing the tree moss to obtain tree moss powder; S2. Preparation of tree moss extract: adding ethanol to tree moss powder, ultrasonically extracting the tree moss powder at a temperature of 40-50° C., performing ultrasonic extraction for 30-60 minutes each time, and performing extraction 2-3 times. After the extraction, the extract is concentrated until no solvent is removed by distillation to obtain the tree moss extract; S3. Preparation of moss absolute: S31. Add the extract to the moss extract and stir until uniformly mixed to obtain a first solution; S32. Freeze the first solution at -10-30°C for 10-30 hours, filter and remove insoluble matter to obtain a second solution; S33. Concentrate the second solution until no solvent is removed by distillation to obtain moss absolute; The extract comprises the following components in parts by weight: 5-10 parts of n-hexane, 5-15 parts of ethyl acetate, 1-5 parts of acetone, and 5-10 parts of tert-butanol.

2. The method for extracting tree moss absolute for electronic cigarettes according to claim 1, characterized in that: The amount of the extract added in step S31 is 5-10 times the amount of the tree moss extract.

3. The method for extracting tree moss absolute for electronic cigarettes according to claim 1, characterized in that: The average particle size of the tree moss powder is 20-60 meshes.

4. The method for extracting tree moss absolute for electronic cigarettes according to claim 1, characterized in that: The amount of ethanol added is 4-6 times that of the tree moss powder.

5. The method for extracting tree moss absolute for electronic cigarettes according to claim 1, characterized in that: In step S33, low-temperature vacuum concentration is adopted, and the temperature during concentration is 40-50°C.

6. The method for extracting tree moss absolute for electronic cigarettes according to claim 1, characterized in that: In step S33, molecular distillation is used to obtain tree moss absolute.

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