Method for subcritically extracting spearmint essential oil and application

Abstract

The invention belongs to the technical field of perfume extraction, and particularly relates to a method for subcritical extraction of spearmint essential oil and application of the spearmint essential oil, the extraction method comprises the following steps: drying spearmint whole herb, crushing, adding spearmint whole herb powder into a subcritical extraction tank, using propane as an extraction agent, and collecting subcritical extraction fluid; adding the collected subcritical extraction fluid into an evaporation tank, and carrying out reduced pressure evaporation to obtain spearmint extract; and carrying out molecular distillation on the obtained spearmint extract, and collecting light components to obtain the spearmint essential oil. The subcritically extracted spearmint essential oil is purified by adopting a molecular distillation method, component separation of the spearmint essential oil can be realized at a relatively low temperature, and high-purity and high-quality spearmint essential oil is obtained while natural aroma components of the spearmint essential oil are reserved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of spice extraction, and particularly relates to a method for subcritical extraction of spearmint essential oil and application. BACKGROUND

[0002] Spearmint (Mentha spicata L), also known as green mint or fragrant herb, is a kind of erect perennial herbaceous plant of Labiatae, mainly distributed in North China, Northeast China and Northwest China, and is a kind of medicine and food homologous plant with great development potential and local characteristics, which is widely used in folk for treating coronary heart disease, high blood pressure, cold and other diseases. Spearmint is also an important spice plant. The extraction of stems and leaves can obtain spearmint essential oil, which has a fresh, cool and sweet smell, and can be widely used as a natural food additive and essence and spice in the food and cosmetic industries. When added to cigarettes, it can enrich tobacco aroma, cover up odors, improve the fresh feeling of smoke and improve the taste.

[0003] At present, the main method for extracting spearmint essential oil from spearmint plants is steam distillation, but this method has problems such as long extraction time, low efficiency, and easy destruction of heat-sensitive components. Organic solvent extraction is also a commonly used extraction method, but this method requires the use of a large amount of organic solvent and has the problem of solvent residue. The extraction of spearmint essential oil by supercritical extraction technology requires professional high-pressure equipment, which has high equipment cost and high energy consumption. Subcritical extraction technology is a separation technology that uses solvents in a subcritical state to extract substances. Compared with traditional extraction technology, it has milder operating conditions, is suitable for the extraction of heat-sensitive components, and has high efficiency and environmental protection. It can efficiently extract volatile essential oils, antioxidants, pigments, medicinal ingredients and lipids, and is suitable for many fields such as food, medicine and cosmetics. SUMMARY

[0004] The purpose of the present application is to provide a method for subcritical extraction of spearmint essential oil and application, which aims to extract and purify spearmint essential oil by subcritical extraction technology and molecular distillation technology, to efficiently extract spearmint while minimizing the destruction of heat-sensitive components and the loss of flavor components, and to obtain a high-quality spearmint essential oil. When added to cigarettes, it can effectively improve the taste of cigarettes, enhance the fresh feeling of smoke, enrich tobacco aroma, cover up odors, and improve the smoking quality of cigarettes.

[0005] To achieve the above-mentioned purpose, the present application is realized by the following technical scheme:

[0006] A method for subcritical extraction of spearmint essential oil, comprising the following steps:

[0007] S1, taking spearmint whole grass, drying and crushing to 20-40 mesh;

[0008] S2, add the whole herb of Mentha haplocalyx powder into a subcritical extraction tank, use propane as an extractant, and cyclically extract 3-5 times to collect the subcritical extraction fluid;

[0009] S3, add the subcritical extraction fluid collected in step S2 into an evaporation tank, perform evaporation under reduced pressure to recover propane and obtain Mentha haplocalyx extract;

[0010] S4, perform molecular distillation on the Mentha haplocalyx extract obtained in step S3 to collect light components, i.e., obtain Mentha haplocalyx essential oil.

[0011] Further, in step S2, the solid-liquid ratio of the whole herb of Mentha haplocalyx powder to propane is 1: (15-20).

[0012] Further, the extraction temperature is 45-50℃, the extraction pressure is 2.8-3.2 MPa, and each extraction lasts for 30 min.

[0013] Further, in step S3, the setting pressure of the evaporation under reduced pressure is -0.08— -0.1 MPa.

[0014] Further, in step S4, the molecular distillation specifically comprises the following steps: setting the vacuum degree to -0.06 ~ -0.08 MPa, the scraping film rotating speed to 100 ~ 120 r / min, the feeding evaporator temperature to 45 ~ 50℃, the feeding speed to 1 ~ 2 mL / min, and the evaporator temperature to 80 ~ 100℃.

[0015] An application, the Mentha haplocalyx essential oil prepared according to any one of the above applications is applied in cigarettes.

[0016] Further, a 1% Mentha haplocalyx essential oil ethanol solution is prepared and added to the cigarettes.

[0017] Further, the added amount of each cigarette is 1 uL.

[0018] The beneficial effects of the present application are:

[0019] 1. The present application adopts subcritical extraction technology to extract Mentha haplocalyx, which has lower extraction temperature and shorter extraction time than traditional extraction methods, can minimize the destruction of heat-sensitive components, retain the flavor components in Mentha haplocalyx, and improve the extraction rate and extraction efficiency.

[0020] 2. The present application uses propane as a subcritical extraction solvent. Propane is a gas at room temperature and pressure, which is easy to separate from the extract, and can be recycled by compression, condensation and other methods, reducing solvent consumption and emissions. Compared with organic solvent extraction method, it avoids the pollution of a large amount of organic solvents to the environment, and has no solvent residue and other problems, which meets the current requirements of green chemistry and sustainable development.

[0021] 3. This invention uses molecular distillation to purify spearmint essential oil through subcritical extraction. This method can achieve component separation of spearmint essential oil at a relatively low temperature, while preserving the natural aroma components of spearmint essential oil, thus obtaining high-purity, high-quality spearmint essential oil. Detailed Implementation

[0022] The technical solutions of the present invention will be described in detail below through embodiments. The following embodiments are merely exemplary and can only be used to explain and illustrate the technical solutions of the present invention, and should not be construed as limiting the technical solutions of the present invention.

[0023] Example 1

[0024] 1000 g of whole spearmint herb was crushed and passed through a 20-mesh sieve. The spearmint powder was added to a subcritical extraction tank, using propane as the extractant at a material-to-liquid ratio of 1:15. The temperature was set at 50℃ and the extraction pressure at 3.0 MPa. Each extraction lasted 30 min, and the extraction was repeated 3 times. The subcritical extract fluids were collected and combined. The subcritical extract fluids were added to an evaporator, and the pressure was reduced to -0.1 MPa for vacuum evaporation to recover propane and obtain spearmint extract. The spearmint extract was subjected to molecular distillation, with a vacuum of -0.08 MPa, a scraper rotation speed of 100 ~ 120 r / min, a feed evaporator temperature of 45 ℃, a feed rate of 1.5 mL / min, and an evaporator temperature of 100 ℃. The light fractions were collected to obtain spearmint essential oil. 0.1 g of spearmint essential oil was weighed and diluted 100 times with 95% ethanol to prepare a 1% spearmint essential oil solution. This solution was then injected into blank cigarettes using a cigarette flavoring injection machine, with 1 μL injected into each cigarette. The flavored sample cigarettes and blank cigarettes were placed in a constant temperature and humidity chamber at (22 ± 2)℃ and (60 ± 5)% relative humidity for 48 h for equilibration before evaluation. The evaluation results showed that the spearmint essential oil prepared by this method can impart a cool, minty aroma to cigarettes, increase aroma richness, reduce irritation, mask off-flavors, and improve the aftertaste.

[0025] Example 2

[0026] 1000 g of whole spearmint herb was crushed and passed through a 40-mesh sieve. The spearmint powder was added to a subcritical extraction tank, using propane as the extractant at a material-to-liquid ratio of 1:20. The temperature was set at 45℃ and the extraction pressure at 2.8 MPa. Each extraction lasted 30 min, and the extraction was repeated 5 times. The subcritical extract fluids were collected and combined. The subcritical extract fluids were added to an evaporator, and the pressure was reduced to -0.08 MPa for vacuum evaporation to recover propane and obtain spearmint extract. The spearmint extract was subjected to molecular distillation, with a vacuum of -0.08 MPa, a scraper rotation speed of 100 ~ 120 r / min, a feed evaporator temperature of 50 ℃, a feed rate of 1.5 mL / min, and an evaporator temperature of 100 ℃. The light fractions were collected to obtain spearmint essential oil. 0.1 g of spearmint essential oil was weighed and diluted 100 times with 95% ethanol to prepare a 1% spearmint essential oil solution. This solution was then injected into blank cigarettes using a cigarette flavoring injection machine, with 1 μL injected into each cigarette. The flavored sample cigarettes and blank cigarettes were placed in a constant temperature and humidity chamber at (22 ± 2)℃ and (60 ± 5)% relative humidity for 48 h for equilibration before evaluation. The evaluation results showed that the spearmint essential oil prepared by this method can impart a cool, minty aroma to cigarettes, increase aroma richness, reduce irritation, mask off-flavors, and improve the aftertaste.

[0027] Example 3

[0028] 1000 g of whole spearmint herb was crushed and passed through a 30-mesh sieve. The spearmint powder was added to a subcritical extraction tank, using propane as the extractant at a material-to-liquid ratio of 1:18. The temperature was set at 48℃ and the extraction pressure at 3.2 MPa. Each extraction lasted 30 min, and the extraction was repeated 5 times. The subcritical extract fluids were collected and combined. The subcritical extract fluids were added to an evaporator, and the pressure was reduced to -0.1 MPa for vacuum evaporation to recover propane and obtain spearmint extract. The spearmint extract was subjected to molecular distillation, with a vacuum of -0.08 MPa, a scraper rotation speed of 100 ~ 120 r / min, a feed evaporator temperature of 50 ℃, a feed rate of 1.5 mL / min, and an evaporator temperature of 100 ℃. The light components were collected to obtain spearmint essential oil. 0.1 g of spearmint essential oil was weighed and diluted 100 times with 95% ethanol to prepare a 1% spearmint essential oil solution. This solution was then injected into blank cigarettes using a cigarette flavoring injection machine, with 1 μL injected into each cigarette. The flavored sample cigarettes and blank cigarettes were placed in a constant temperature and humidity chamber at (22 ± 2)℃ and (60 ± 5)% relative humidity for 48 h for equilibration before evaluation. The evaluation results showed that the spearmint essential oil prepared by this method can impart a cool, minty aroma to cigarettes, increase aroma richness, reduce irritation, mask off-flavors, and improve the aftertaste.

[0029] The specific embodiments described above are merely illustrative or explanatory of the principles of the present invention and do not constitute a limitation thereof. Therefore, any modifications, equivalent substitutions, improvements, etc., made without departing from the spirit and scope of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for subcritical extraction of spearmint essential oil, characterized in that, The following steps are adopted: S1. Take the whole spearmint herb, dry it, and then grind it into 20-40 mesh; S2. Add spearmint whole herb powder to a subcritical extraction tank, use propane as the extractant, and circulate the extraction 3-5 times. Collect and combine the subcritical extraction fluids. S3. Add the subcritical extract fluid collected and combined in step S2 to an evaporator, evaporate under reduced pressure, recover propane and obtain spearmint extract. S4. Molecular distillation is performed on the spearmint extract obtained in step S3 to collect the light components, thus obtaining spearmint essential oil.

2. The method for subcritical extraction of spearmint essential oil according to claim 1, characterized in that, In step S2, the ratio of spearmint whole herb powder to propane is 1:(15-20).

3. The method for subcritical extraction of spearmint essential oil according to claim 2, characterized in that, The extraction temperature was 45-50℃, the extraction pressure was 2.8-3.2MPa, and each extraction lasted 30 minutes.

4. The method for subcritical extraction of spearmint essential oil according to claim 1, characterized in that, In step S3, the pressure for reduced pressure evaporation is set to -0.08 to -0.1 MPa.

5. The method for subcritical extraction of spearmint essential oil according to claim 1, characterized in that, The specific steps of molecular distillation in step S4 are as follows: set the vacuum degree to -0.06 ~ -0.08 MPa, the scraper rotation speed to 100 ~ 120 r / min, the feed evaporator temperature to 45 ~ 50℃, the feed rate to 1 ~ 2 mL / min, and the evaporator temperature to 80 ~ 100℃.

6. An application characterized in that, The use of spearmint essential oil prepared according to any one of claims 1 to 5 in cigarettes.

7. The application according to claim 6, characterized in that, Prepare a 1% spearmint essential oil ethanol solution and add it to cigarettes.

8. The application according to claim 7, characterized in that, The amount added to each cigarette is 1 uL.