KR101230388B1 - Method for extracting essential oil from pine, and essential oil produced thereby - Google Patents

Abstract

PURPOSE: A method for extracting essential oil from pine trees is provided to extract essential oil from the pine trees by a simple control without the loss or decomposition of volatile components in the essential oil. CONSTITUTION: A method for extracting essential oil from pine trees comprises: a step of cutting or crushing pine leaves and pine branches; a step of manufacturing a leaf-branch mixture by mixing the pine leaves and pine branches; a step of adding water into the leaf-branch mixture, and heating the mixture in a sealed state to manufacture a hot water extract; a step of cooling the hot water extract, removing the solid portions of the pine leaves and pine branches, and collecting rosin from the water; and a step of distilling the hot water extract in which the solid portions and the rosin are removed to obtain the essential oil.

Description

Method for extracting essential oil from pine, and essential oil produced thereby

The present invention relates to a method for producing pine essential oil by distilling and then distilling the leaves and stems of pine, and a pine essential oil produced by the method.

Pine tree is an evergreen conifer tree of the cultivar of Aspen, and contains a large amount of chlorophyll, protein, crude fat, phosphorus, iron, enzymes, essential oils, minerals, vitamin A and vitamin C.

Looking at the composition of each pine tree, pine needles contain estole which is composed mainly of ascorbic acid, carotene, vitamin K, vitamin B, high taste substance, flavonoids, anthocyanin, resin, tannin, carbohydrate p-nonacoic acid and uniper acid. It contains lead-type lead, kinasan, shikimic acid, chlorophyll and essential oils, and the bark contains tannin, anthocyanin, fimaric acid, β-sitosterol, dihydro-β-sitosterol, glucotanin, eicozanol and tetracozanole. .

In the neck, there are terpene hydrat, pinosylbin, pinosylbin monomethyl ester, dihydropinosylbin monomethyl ester, pinosembrine, pinobank, propionaldehyde, serotonic acid, unferric acid, terebin oil, tar, and young branches and The oil in the bark contains canipol, abienic acid and essential oils.

Raw pine extracts from pines are 70% essential oils and 25% resins by weight, and they contain myrogenic, terphenol, α-β-karenne, α-β-pinene and sesquiterpenes, Rongipolene. Rosin is 18-22% by weight, 70-75% resin, and α-β-pinene, camphor, fenlandene, terpenal alcohol, densifimaric acid and palustic acid. Pollen contains adenine, histidine, choline, Isoramnetine, quercetin, and seeds contain shikimic acid.

The components of the pine are known to be beneficial to the human body, the bactericidal effect, antioxidant effect, inhibiting the formation of harmful substances, strengthening immunity, wound healing, pore contraction, washing effect, cell regeneration, epidermal formation, skin whitening, skin vitality, Hemostasis, haemostasis, blood circulation, detoxification, digestive aid, metabolism promotion, cardiac peripheral vasodilation, anti-allergic action, etc. have been reported in the academic community.

In particular, essential oils, which are highly volatile oil components, are useful substances that can be used for various purposes, and may be applied to the skin, taken, or used to prepare perfume as a unique flavor or add flavor to food.

In oriental medicine, taking pine essential oils strengthens the heart and improves blood circulation (血 行), relieves pain such as shoulder aches, and is effective in stroke and high blood pressure. It is reported to be effective in atopic dermatitis and itching.

In addition, folk remedies were used for the treatment of arthritis and neuralgia, and the pine needles were used to put pine needles in order to slow down the rate at which the songpyun rests, and wild animals such as pigs and bears were traumatized. There is a myth that the wound healed by rubbing the trauma on pine trees.

The essential oil of pine, or pine oil, varies depending on the pine area.There are 0.1-1.3% by weight in pine needles, 0.36% in shoots, and 0.2-0.9% in annual branches. exist.

The essential oils of pine needles are α-pinene, β-pinene, camphor, fenlandene, limonene, cardinene, bornole, bornyl acetate, and silvestren. Acetat, α-β-VII-pinene, limonene, free alcohol, dipentene, camphor, fenlandrene, β-myrcene, terpineol, acetone, karen.

As the efficacy of various components contained in the essential oil of pine is known, studies are actively underway to utilize them in daily life. For example, Korean Patent Publication No. 1996-0029447 discloses pine needle essential oil and pine needle extract. The present invention relates to a human cleanser composition containing a pine needle extract complex, wherein the pine needle essential oil obtained by steam distillation of pine needles and soft branches at high temperature, and the pine needles are immersed in 1,3-butylene glycol and ethanol, followed by compression filtration. The obtained pine needle extract or pine needles were dried, extracted with an ethanol aqueous solution, filtered, and then mixed with polyquaternium-7, a cationic polymer of a surfactant, stirred and filtered, followed by evaporation to dryness in a vacuum to obtain a pine needle extract composite. The invention is added as an additive.

In addition, Korean Patent Application Publication No. 2010-0098080 discloses a skin moisturizing cosmetic composition containing a rosin extract, a red pine leaf extract and a red pine root extract, which crystallizes the rosin and recovers the produced material, and then liquefies it. Distillation / collection was performed to collect the portions except the up and down parts, followed by two purifications, followed by hydrogenation, and then purified again and distilled to obtain a rosin extract, and the lyophilized red pine leaf was extracted with cold at room temperature. Next, the ethanol is evaporated and concentrated to obtain a red pine leaf extract, and the root of red pine is extracted with water or an organic solvent to obtain a red pine root extract to use as an additive for skin moisturizing cosmetics.

In addition, Korean Patent Publication No. 2010-0025992 discloses pine tree by subcritical extraction for 100 to 250 minutes at 50 to 170 ° C. using a subcritical fluid of 50 to 70 kgf / cm 2 using pine as a material. An antioxidant extracting method for preparing an subcritical extract of and then extracting the antioxidant from pine tree by extracting hot water is disclosed, and is used in the field of health functional food, medicine or cosmetics.

However, the above methods are carried out under high temperature or high pressure conditions or by adding organic solvents or chemicals to obtain pine essential oils or extracts. Under high temperature and high pressure conditions, volatile essential oil components may be lost or decomposed and deteriorated. If the extraction is performed by adding organic and chemical substances, it is necessary to remove them again, which causes a complicated manufacturing process and increases manufacturing costs.

In addition, the fragrance components of the manufactured pine essential oil have a disadvantage that the long-term storage is difficult due to the weak volatile persistence of the fragrance, there is a problem that must be used quickly after manufacture.

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for extracting essential oils from pine trees in a method of extracting essential oils from pine trees, with a simple operation, while preventing volatile components of the essential oils from being lost or decomposed.

In addition, even if the essential oil is stored for a long time to provide a way to maintain the unique flavor of pine.

In order to solve the above problems, the present invention is to collect and wash pine needles and pine branches and then cut or shred to 1 ~ 5 cm in length; Preparing a leaf branch mixture by mixing the cut or crushed pine needles and pine branches in a ratio of 3: 7 to 5: 5 by weight; Preparing a hot water extract by putting the leaf branch mixture in a heating container, adding 8-12 times water by weight, and then heating the mixture at a temperature of 80-90 ° C. for 18-22 hours in a sealed state; Cooling the hot water extract and then removing solids of pine needles and pine branches and collecting rosin spilled into the water; It provides a method for extracting essential oil from pine trees, including; and distilling the hot water extract from which the solids and rosin are removed to obtain pine essential oil for 18 to 22 hours at a temperature of 80 to 90 ° C.

At this time, the pine needles and pine branches are preferably taken from the tree of the genus pine including pine genus and pine genus.

In addition, the collected rosin is steam distilled to extract terebin oil, and then the extracted terebin oil is preferably mixed with the pine essential oil, extracting the terebin oil from the rosin and drying the remaining rosin is added to the pine essential oil More preferred.

The present invention also provides a pine essential oil extracted by the above method.

Pine essential oil extracted by the method according to the present invention is extracted at low temperatures, the volatile content is not lost or decomposed, the extraction yield is high, and the extraction process is simple, so the extraction cost is low.

In addition, the fragrance component of rosin is added to increase the fragrance component content of the essential oil of pine, and the fragrance of pine is maintained for a long time can be stored.

Hereinafter, a method for extracting pine essential oil according to the present invention will be described in detail.

First, pine is prepared. In the present invention, pine essential oil is extracted using pine needles and pine branches as materials.

Essential oil components of pine are distributed in pine needles, branches, roots and rosin, the present invention extracts essential oils from pine needles and branches for convenience of harvesting.

Pine described in the present invention is a category belonging to the genus Pine ( Pinus ), the pine genus pine, Gom brush, jungmong brush, Manchu Gom brush, white pine, Rigida pine, Taida pine, Banx pine, Fungens pine, Rezinosa pine, Scots pine, include pine subgenus (Haploxylon), such as pine subgenus (Diploxylon) and pine, Pinus pumila, Pinus parviflora, Pinus strobus, such as Pinus thunbergii nine weeks.

Pine needles and pine branches are collected, washed, and cut or crushed into 1-5 cm lengths so that essential oils can be extracted more easily from pines.

Since the eggplants have fewer growth years, they contain more essential oil components. Therefore, it is preferable to collect eggplants with as few growth years as possible.

Next, the cut or crushed pine needles and pine branches are mixed in a ratio of 3: 7 to 5: 5 by weight to prepare a leaf branch mixture, and for convenience of work, the branches with pine needles are attached to pine needles: pine branches = 3: 7 to 5: 5 It may be used by cutting and crushing with 1 to 5 cm in length after collecting and washing with pine needles to the weight ratio.

The mixing ratio of pine needles and branches maximizes the extraction amount of essential oils and ensures a balanced distribution of the constituents of the mixed essential oils in which the essential oils of pine needles and essential oils of pine branches are mixed. The amount of rosin flowing from pine needles and pine branches can be obtained in an appropriate ratio with the amount of the essential oil.

Next, put the mixture of leaf branch in a heating container and add 8 to 12 times the water by weight, and then heated to a temperature of 80 ~ 90 ℃ 18 to 22 hours in a sealed state to prepare a hot water extract.

During heating, various components contained in pine needles and pine branches are eluted in water. By heating at a low temperature, the components eluted in water are minimized from decomposition by high temperature heat. It is prevented from being vaporized and lost to the outside.

Since operating at a temperature of less than 100 ℃ lower than the boiling point of water to minimize the increase in the internal pressure of the heating vessel is possible to operate in a sealed state, it is preferable to install a pressure automatic discharge device in the heating vessel in terms of safe operation.

The rosin contained in pine needles and pine branches also flows out into the water during the heating. The rosin contains turpentine, an essential oil component, and rosin, a resin component, and rosin is not dissolved in water. In free state with water.

Since cooling the hot water extract can separate the rosin from the water, the hot water extract is cooled to room temperature to remove solids of pine needles and pine branches, and the rosin spilled into the water is collected, and then the hot water extract is 80-90 ° C. Distilled at the temperature of 18-22 hours to obtain pine essential oil.

The distillation apparatus for performing the distillation is composed of a main body containing the pine hot water extract, the heating means of the lower part of the main body and a cover which is sealed by sealing with the upper end of the main body, the other end of the pipe is connected to the collecting vessel one end The cover and the collection container are connected to each other so as to be able to flow to each other through the pipe, and cooling means are provided in the middle of the pipe.

Preferably, the pipe is made of a material having a high thermal conductivity such that steam flowing from the cover is efficiently cooled and condensed in the cooling means, and the cooling means is installed at a capacity capable of sufficiently condensing the incoming steam.

The hot water extract steam generated in the main body is discharged to the collecting container through a pipe connected to the upper cover, and condensed while passing through the cooling means installed on the way, and collected in the collecting container to produce pine essential oil.

Since the distillation temperature is lower than 100 ℃, the steam contains only the volatile fragrance components of the pine, pine essential oil condensed the pine hot water extract steam is pine compared to the pine extract produced by simply concentrating the pine hot water extract It has a distinctive scent and is clear and transparent with no impurities.

In addition, the present invention can be mixed with the pine essential oil prepared above by extracting terebin oil having a colorless unique flavor from the rosin collected from the hot water extract.

Terebin oil contains a lot of unsaturated fatty acids, which prevents the accumulation of cholesterol, prevents arteriosclerosis, expands peripheral blood vessels, promotes blood circulation, improves brain cell function, sterilization and anti-inflammatory action, blood pressure, diabetes, heart disease. It is known to be effective in stroke, drug, nicotine detoxification and removal of harmful oxygen waste.

Terebin oil is not eluted from the rosin in water at the temperature of 80 ~ 90 ℃ at the time of the hot water extract production, steam distillation of the collected rosin to obtain terebin oil.

Since the steam distillation can be carried out using a known steam distillation method, a detailed description thereof is omitted in the present invention.

Extracting terebin oil from rosin leaves rosin. The main component of rosin is abietic acid, which is a dry white crystal with an absorption capacity of around 170 with an iodine value.

Pine oil refinery has a high volatility, each time the container containing the pine essential oil leaks volatiles, there is a problem that the fragrance of pine essential oil gradually disappears.

In order to solve this problem, it is desirable to sufficiently dry the absorbent rosin and soak it in the manufactured pine essential oil. The rosin retains the volatile flavor component of the pine essential oil for a long time, so that the pine flavor can last for a long time, and the rosin is crushed. The larger the surface area, the better the effect.

Pine essential oils prepared as described above contain various components beneficial to the human body, so that they can be applied to the skin, or can be formulated using fragrance, for example, cosmetics using effects such as washing, skin whitening, and skin vitality. Composition, medicine additives using effects such as prevention of atopic dermatitis and itching, blood circulation, metabolism promotion, immunity enhancement, wound healing, fragrances for adding scent to foods such as steaming puffs, It can be used in food additives, various fragrances (등에 香 하는) and the like added to the food so that the useful component of pine essential oil is contained in the food.

Hereinafter, the present invention will be described in more detail with reference to the following examples, comparative examples and test examples.

It should be noted, however, that the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The present invention is not limited to the following examples. Will be apparent to those skilled in the art to which the present invention pertains.

≪ Example 1 >

Pine needles and pine branches were collected and selected from the coast of Gangwon-do, washed, and cut into 3 cm.

2 kg of the cut pine needles, 3 kg of cut pine branches and 50 L of purified water were sealed in a heating container, and then sealed, and heated at a temperature of 85 ° C. for 20 hours to obtain a hot water extract.

The hot water extract was cooled to room temperature and then filtered to remove pine needles and pine branches. The pine leaves from pine needles and pine branches were collected, and the remaining hot water extracts were put in a distillation apparatus and distilled at a temperature of 85 ° C. for 20 hours to refine the pine oil. Was prepared.

The distillation apparatus is provided with a heating means in the lower part of the main body containing the contents, the cover is tightly fastened to the upper body, one end of the copper pipe of 1.5 cm diameter is connected to the cover and the other end of the copper pipe It is connected to the collection vessel, the cover and the collection vessel is connected to each other through the pipe so as to distribute.

The copper pipe was 10 m in length and was installed so as to be submerged in a cooling water tank through which cold water flows, and the copper pipe was allowed to flow downward from the lid toward the collection vessel.

When the main body is heated by a heating means, steam generated therein is introduced into the copper pipe and condensed while passing through the cooling water container, and is naturally collected in a collecting container by gravity to obtain pine oil.

<Example 2>

In Example 1, the collected rosin was steam distilled to obtain 50 g of terebin oil.

A pine essential oil was prepared in the same manner as in Example 1 except for mixing terebin oil with the pine essential oil prepared in Example 1.

<Example 3>

In Example 2, a pine essential oil was prepared in the same manner as in Example 2, except that the rosin from which the terebin oil was removed from the rosin was crushed and dried and added to the pine essential oil containing the terevin oil.

&Lt; Comparative Example 1 &

In Example 1, a pine essential oil was prepared in the same manner as in Example 1, except that the heating temperature of the step of obtaining the hot water extract and the boiling temperature of the distillation step was the boiling point of water.

At this time, the internal steam was intermittently discharged through the pressure automatic discharge device installed on the heating vessel due to the increase in the internal pressure of the heating vessel during manufacture of the hot water extract.

Comparative Example 2

In Example 1, the hot water extraction process was omitted, except that the cut pine needles 2 kg, the cut pine branches 3 kg and 50 L of purified water were put in a distillation apparatus and distilled at a temperature of 85 ° C. for 20 hours to obtain pine oil. In the same manner as in Example 1 to prepare a pine essential oil.

&Lt; Comparative Example 3 &

Except for Example 1, except that 3 kg of pine needles cut in a heating container, 2 kg of cut pine branches and 50 L of purified water were sealed and heated at a temperature of 85 ° C. for 20 hours when the hot water extract was prepared. Pine essential oil was prepared in the same manner as 1.

<Test Example> Analysis of Flavor Components

In order to analyze the fragrance components of the pine essential oils prepared in Examples and Comparative Examples and to confirm the change over time, the fragrance components of each group were analyzed after 10 days in the open environment immediately after the manufacture and after the preparation. .

The analysis was performed using gas chromatography (series 5890 II Plus, manufactured by Hewlett-Packard, USA) and MSD (mass selective detector, series 5972, manufactured by Hewlett-Packard, USA), and the analysis conditions are shown in Tables 1 and 2 below. Same as

Gas Chromatography Analysis Conditions Item Analysis condition Column HP-5 (30 m × 0.32 mm × 0.25 μm) Carrier gas He (1.0 mL / min) Make up gas N ₂ (30 ml / min) Temp. program 30 ° C (5 min) -3 ° C / min-200 ° C (10 min) Detector temp. 300 ℃ Injector temp. 250 ℃

MSD Analysis Condition Item Analysis condition Ion source and interface temp. 280 ℃ Ionization voltage 70 eV Mass scan range 20 ~ 300 a.m.u scanning rate 1.0 scan / sec electron multiplier voltage 1670 V

Confirmation of the analyzed component was confirmed by comparing with the mass reference data of NBS 75K.L (NIST / EPA / MSDC), the analysis results are shown in Table 3 below.

Analysis result (Unit:%) α-pinene β-pinene β-myrcene limonene Immediately after manufacture Example 1 9.8 17.0 2.2 9.6 Example 2 10.3 18.2 2.0 9.9 Example 3 9.6 16.4 1.8 9.3 Comparative Example 1 7.2 12.4 1.5 7.7 Comparative Example 2 7.5 13.6 1.7 8.2 Comparative Example 3 8.3 16.2 1.8 7.1 10 days after manufacture Example 1 7.3 13.5 1.3 6.2 Example 2 8.8 14.1 1.4 7.3 Example 3 9.0 14.7 1.5 8.4 Comparative Example 1 5.2 9.4 0.8 5.3 Comparative Example 2 5.5 10.6 1.0 6.0 Comparative Example 3 6.5 11.8 1.1 5.8

Referring to the results of Table 3, the composition is contained in the order of β-pinene (β-pinene)> α-pinene (α-pinene)> limonene> β-myrcene (β-myrcene), The β-pinene and α-pinene stimulates the cerebral cortex, increases concentration and exercise power, has antioxidant and anti-aging functions, and limonene has a strong lemon scent and insect repellent effect, and β-myrcene protects blood and lowers heat. And it is known to prevent bacteria propagation.

The aroma content of each group was about 2 times after mixing the turpentine oil obtained from rosin immediately after preparation. Example 1> Example 1 distilled after hot water extraction. Example 3 when rosin was added to essential oil mixed with turpentine. Comparative Example 3 with a high ratio> Comparative Example 2, which omitted the hot water extraction process, appeared in the order of Comparative Example 1 heated to the boiling point of water in the hot water extraction process and distillation process.

On the other hand, after 10 days of manufacture, the content of the fragrance component of Example 3 was measured highest.

Analyzing the results, the aroma content of pine essential oil is increased by mixing turpentine oil from pine oil obtained through hot water extraction process and distillation process, and rosin is added to pine essential oil so that the fragrance is affected even in the open and open environment. It can be seen that it stays long.

On the other hand, if the heating temperature is increased during hot water extraction and distillation, the content of fragrance component is the lowest. can do.

In addition, the distillation after hot water extraction from the results of Comparative Example 2 and Comparative Example 3, it can be seen that the mixing of more pine branches than pine needles during hot water extraction is preferable to increase the content of aroma component of pine essential oil.

As described above, the pine essential oil extracted by the method according to the present invention is extracted at a low temperature, so that volatiles are not lost or decomposed, so that the extraction yield is high and the extraction process is simple. As the fragrance ingredient is added, the fragrance ingredient content of pine essential oil increases and the fragrance of pine tree is maintained for a long time.

Claims (6)

Collecting and washing pine needles and pine branches and cutting or crushing them into 1-5 cm long;
Preparing a leaf branch mixture by mixing the cut or crushed pine needles and pine branches in a ratio of 3: 7 to 5: 5 by weight;
Preparing a hot water extract by putting the leaf branch mixture in a heating container, adding 8-12 times water by weight, and then heating the mixture at a temperature of 80-90 ° C. for 18-22 hours in a sealed state;
Cooling the hot water extract and then removing solids of pine needles and pine branches and collecting rosin spilled into the water; And
Distilling the hot water extract from which the solids and the rosin are removed to obtain pine essential oil by distilling at a temperature of 80 to 90 ° C. for 18 to 22 hours. The method according to claim 1,
The pine needles and pine branches extract essential oil from the pine tree, characterized in that it is taken from the tree of the genus pine including pine and pine. The method according to claim 1,
Steam distilling the collected rosin to extract terebin oil and then the extracted terebin oil is mixed with the pine essential oil. The method according to claim 3,
Extracting terebin oil from the rosin and drying the remaining rosin and then added to the pine essential oil method for extracting essential oil from pine. Pine essential oil extracted by the method of any one of Claims 1-4. The method according to claim 5,
Pine essential oil, characterized in that the pine essential oil is used as a cosmetic composition, pharmaceutical additives, flavoring agents, food additives or fragrances.