JPS60120957A - Preparation of essence of beefsteak plant - Google Patents

Abstract

PURPOSE:To prepare an essence of a beefsteak plant containing sufficiently a fragrance or flavor of beefsteak plant of its own, by extracting essence of beefsteak plant with a carbon dioxide in a liquid range from beefsteak plant. CONSTITUTION:Leaves, flowers, fruits or stalks are used as beefsteak plant for starting raw material of extraction, the beefsteak plants are in a state immediately after harvesting, or in a state having the same water content as that at harvesting, or in a insufficiently dried state and used. In extractive operating, the raw material beefsteak plants are put in the extractor 1, the system is hermetically sealed, liquid carbon dioxide is fed from the storage tank 5 to it by the pump 6, and essence of beefsteak plant is extracted. In the operation, a feed ratio of liquid carbon dioxide as an extractant to the raw material beefsteak plant is 3-60 by weight, and the extraction temperature is 0-30 deg.C. Consequently, essence containing sufficiently fragrance or flavor of beefsteak plant of its own can be extracted.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a perilla extract using a perilla plant as a raw material, which contains the perilla-specific aroma or flavor of the raw material without impairing it.

Perilla plants grow wild or are cultivated all over Japan, and the Japanese people like them for their unique aroma, so they are used as a condiment for sashimi, soup, noodle sauce, etc., or as a coloring agent for pickled plums, pickles, etc. Widely used, mainly in food.

Also, after the Second War on Dogs, it began to be collected as an essential oil, and its use expanded to include flavoring agents, and now it is widely used as a natural flavoring agent.

The characteristic aroma and flavor of perilla plants is thought to be provided by many aromatic components, the main component of which is perilla aldehyde. It is generally said that many aromatic components are unstable to heat or are easily oxidized and decomposed. Therefore, in the manufacturing process of perfumes containing such aromatic ingredients as constituent substances, it is necessary to adopt a method that reduces the heat load as much as possible.

Most essential oils from perilla plants are currently produced by steam distillation. In the case of steam distillation, the starting material, perilla plants (hereinafter referred to as perilla), is brought into contact with steam and the essential oil is distilled out. Aromatic components that are unstable to heat or that are easily decomposed by acid or arsenic have the disadvantage that their aromas change as they are decomposed by water vapor.

The technology of extracting the aromatic components of plants using liquid carbon dioxide has been known for a long time, and has been used to extract aromatic components from plants such as coffee, hops,
Extraction examples of many plants such as fruits have been reported.
Chri-stopher Grimmett.

Cheinistry and Industry,
16' May, p, 359-362.

1981'). Many patents have also been filed.
For example, U.S. Pat. No. 3,477.856 or Japanese Patent Publication No. 48-44864). However, in the extraction examples found in these published publications, there is no method of extracting perilla with carbon dioxide to obtain a perilla extract containing aromatic components unique to perilla.

It is thought that perilla is mainly composed of perilla aldehyde, and many other aromatic components such as limonene and pinene are mixed together to give perilla its unique aroma and flavor. It volatilizes and dissipates in large quantities due to over-cooking. For example, according to tests conducted by the present inventors, even by freeze-drying, which is known as a drying method with high aroma retention properties because almost no heat load is applied, perillaldehyde, the main component, was reduced by more than 80% compared to fresh leaves. With irimonene, which has a lower boiling point than perillaldehyde, a reduction of around 90% was observed. This means that the aromatic components of perilla, which contain many low-boiling point substances, are easily transmuted by decomposition or volatilization, and it is extremely difficult to extract these components while preserving the aroma and flavor of raw perilla. This shows that the situation is difficult.

An object of the present invention is to obtain perilla essential oil (hereinafter referred to as perilla extract) that contains all the aromatic components of perilla, which is a starting material, without alteration. That is, the gist of this method is to produce an extract that obediently and sufficiently contains the aroma or flavor peculiar to perilla according to the state of the perilla, which is the starting material, by extraction from perilla using carbon dioxide in the liquid region.

First, the method for producing perilla extract according to the present invention will be explained in detail according to the flow of the extraction device. FIG. 1 shows an example of an extraction device for carrying out the method of the invention. First, perilla leaves, flowers,
Perilla extract is obtained by placing the fruits or stems in their original form, cutting or crushing them into an extractor (1), which is a high-pressure container, using a commonly used method and extracting with a diacid "arsenic" in the liquid range. Types of perilla used as raw materials include Perilla perilla, Chilimen aka perilla, Chilimen aka perilla, and Katamen jiso.The leaves, flowers, fruits, or stems that contain the unique aroma or flavor of these perilla are cut using a cutting machine or Width 3 mm using a coarse crusher
Cut or coarsely crush into pieces of 10mm or 3 to 1Qfill+ in diameter. In addition, leaves, flowers, or fruits may be left in their original form without being cut or crushed. It is also possible to select a shape depending on the use of the extraction residue. Perilla used as a starting material is used in a fresh state, that is, with a moisture content of approximately the same level as when harvested, that is, approximately 700% (based on dry matter), and in a half-dried state, that is, with a moisture content of approximately 100% (based on dry matter). However, it is preferable to use the freshest possible ingredients.

In the extraction operation, the raw material Shin is loaded into the extractor (1), the system is sealed, and then liquid carbon dioxide is injected from the storage tank (5) using the pump (6). The extraction method may be either a batch method or a once-through method.

The extraction operation is performed by filling liquid carbon dioxide, which is an extracting agent, into the extractor (1) containing perilla, which is an extraction raw material, to a predetermined ratio of extracting agent, and when the extraction is completed, the extract is transferred to the extractor (1). (
1) to the separator (2). In the separator, the extract is separated into extract and carbon dioxide. That is, the separator (2
) The carbon dioxide vaporized in the separator (2) is compressed by the compressor (3), further cooled by the heat exchanger (4), liquefied again, and recovered in the storage tank (5). Therefore, only the perilla extract remains in the separator (2) in the form of an oil, so it cannot be properly removed from the bottom of the separator (2). The extracting agent ratio, ie, the injection ratio of liquid carbon dioxide, which is an extracting agent, to perilla, which is an extraction raw material, is preferably 3 to 60, particularly 5 l/)20 in terms of weight ratio. Extraction temperature is 0
Preference is given to operating at temperatures between .degree. C. and 30.degree. C., in particular between .gamma.C4r and 15.degree. In this case, the pressure inside the extractor (1) indicates the value of the pressure on the saturated liquid line at each extraction temperature. For example, when the extraction humidity is between 0°C and 30°C, the pressure inside the extractor is 35 K9/cr/I to 73 h/cJ, respectively.The extraction temperature can be adjusted using the extractor (1).
This is done by circulating water or brine at a constant temperature through a jacket attached to the extractor, but it is better to heat the liquid carbon dioxide injected into the extractor (1) to near the extraction temperature using the heat exchanger (8) in advance. Effective.

The extraction time t' varies depending on the form of the extraction raw material, but it is more preferable to complete the extraction operation within 15 minutes to 5 hours, especially 1 to 2 hours after filling the extractor (1) with liquid carbon dioxide. When the extraction is completed, the raffinate is kept in the extractor (1) and only the extract is transferred to the separator (2). In this case, the temperature of the separator (2) is 5°C to 1°C lower than the extraction temperature.
It is preferable to lower the temperature by 0°C from the viewpoint of transfer efficiency.

When extraction is performed using the once-through method, liquid carbon dioxide is passed from a storage tank (5) into an extractor (1) containing perilla, which is an extraction raw material, by a pump (6).
7) and preheated in a heat exchanger (8) before entering the extractor (1).

The amount of liquid to be passed is 0.6 to 9 kg/hour for liquid carbon dioxide per K9, especially 5 to 9 kg/hour.
Preferably, it is carried out at a rate of 20Kp/hour. extraction f
The average residence time for the flow of liquid carbon dioxide through F&(1) is preferably from 0.5 to 6 hours, in particular from 1 to 3 hours. Extraction temperature is OC to 30℃,
In particular, it is preferred to operate at 72°C to 15°C. The extraction pressure is ``K9/lJ to 100 to 9/crl, especially 40 Ky/ca to 60 Kg/cr! It is preferable to operate with Liquid carbon dioxide in which aromatic components of perilla are dissolved in the extractor (1), ie, an extract, is continuously transferred from the extractor (1) to the separator (2).

In the separator (2) the liquid carbon dioxide is vaporized and separated from the oily extract of perilla. The gaseous carbon dioxide discharged from the separator (2) is liquefied again in the heat exchanger (4) and collected in the storage tank (5), where it is returned to the tank (5).

It is sent to the extractor (1) by the pump (6) and is recycled and used as an extraction agent. The perilla extract remaining in the separator (2) is taken out of the system by appropriately opening and closing a valve in the lower piping of the separator (2).

The separation temperature is operated below the extraction temperature. The temperature of the heat exchanger (4) and the storage tank (5) are lower than the humidity of the separator (2), and by operating with a temperature difference of 2°C or more, the carbon dioxide in the separator (2) is reduced. Vaporization and heat exchanger (4
) can be carried out sequentially.

The present invention will be explained below by way of examples.

Actual example-1 Fresh leaves of Olamina japonica (moisture content 680% vs. dry matter) 30 (l
Use a cutter to cut the material into 0.5 cm width pieces, and insert into the extractor (1).
2.10 Of liquid carbon dioxide was injected into the solution, and extraction was carried out batchwise at an extraction temperature of 15° C. for 15 hours.

The pressure inside the extractor (1) at this time was 51 Kp/ca. After the extraction was completed, the K extract was transferred to a micrometer (2) kept at 2°C. Carbon dioxide was vaporized and separated and removed from the extract in the separator (2) to obtain 1.5 y of perilla extract as a perilla extract.

The obtained perilla extract is a golden yellow viscous oil.
It had a strong aroma and flavor that closely resembled fresh leaves of Aspera.

Example-2 Ear of perilla perilla (ear of perilla, flowers fall off and become fruit in the lower part, and flowers in the upper part. Moisture content 520% vs. dry matter)
2ooy in its original form was placed in extraction i (1), 3,000 f of liquid carbon dioxide was injected, and extraction was performed in a batch manner at 10°C for 15 hours. The pressure was U↓46 Ky/cIi.After the extraction was completed,
The extract is transferred to a separator (2) kept at 5°C, and carbon dioxide is separated and removed to produce perilla extract (1175't14J7'ic) as a panicle extract.

This perilla extract was a brownish-yellow, viscous oil5, and had a strong perilla aroma very similar to that of panicle perilla.

Example-3 Chilimen perilla stems (moisture content 330% vs. dry matter) 400
7 was cut into pieces of about 0.5 on, placed in the extractor (1), and 2,000 ml of liquid carbon dioxide was injected into the cut pieces. After several hours, perilla extract 0027 was obtained as an extract.

This perilla extract was in the form of a pale yellow paste, and had a perilla aroma containing a slightly raw wood-like aroma, very similar to the aroma of perilla stems.

Example-4 300 g of fresh leaves of Aspera oleracea (moisture content: 680% vs. dry matter) were put into a freeze dryer as whole leaves at a freezing temperature of -25°C and a freezing time of 5.
The leaves were frozen for an hour and dried at a drying temperature of 25°C for a drying time of 26 hours to obtain freeze-dried leaves (moisture content 4% vs. dry matter). Approximately 10 whole leaves of the same lot, 3002, are taken into one
The bundles were tied together, hung indoors, and dried in the shade for 5 days to obtain shade Chiba leaves (moisture content 12% to 2% dry matter). Freeze-dried leaves 401 (30 (equivalent to liter) as fresh leaves) subjected to the above drying process and shade Chika 43f (equivalent to 3001 as fresh leaves) Oagebi fresh leaves ao
Batch extraction of or was performed using liquid carbon dioxide 24009 under the same extraction conditions as in Example-1. Table 1 shows the amount of perilla extract obtained as an extract and the main components perilla aldehyde (boiling point 237°C) and limonene (boiling point 176°C) extracted from fresh leaves. It is expressed as a ratio to the amount of I. As is clear from Table 1, the aromatic components of perilla disappeared in large quantities during the drying process, and in particular, the volatilization of low-boiling components such as limonene increased.

Table 1 Note) This is an example of a ratio diagram of the amount of extraction to the amount of extraction from fresh leaves.

! (E): Extractor (To): Separator 4: Compressor Small: Heat exchanger evening ←→；Storage tank Pump: Pump Edict: Flowmeter 10, ll: Hair-7

Claims (1)

[Claims] ■) In a method for producing perilla extract from a perilla plant, the perilla extract is obtained from a perilla plant in a liquid range according to the condition of the perilla plant as a starting material, without impairing the characteristic scent or flavor of perilla. A method for producing perilla extract, characterized in that it is produced by extraction with carbon dioxide. 2) Leaves as perilla plant which is the starting material for extraction. The method according to claim 1, which uses flowers, fruits or stems. 3) The state of the perilla plant, which is the raw material for extraction, is immediately after harvesting, retains the same moisture content as at the time of harvest, or is in a half-dried state.Claim 1
2. The method according to any one of paragraphs 1 and 2. 4) The temperature of the liquid/zone carbon dioxide used for extraction is 0°C.
Claims 1 to 3 used in the range from 30°C to 30°C.
The method described in any of the paragraphs.