JPS61209567A - Method of extracting fragrant substance - Google Patents

Abstract

PURPOSE:To obtain a high-quality complex fragrant substance by one process, by extracting the fragrant subtance from a spice mixture by the use of a fluid in a subcritical or supercritical state as an extractant, and separating it. CONSTITUTION:In extracting and separating a fragrant substance from a spice mixture such as curry powder, a fluid in a subcritical or supercritical state is used as an extractant. Generally any liquid in the subcritical or supercritical state is usable, usually carbon dioxide is used as the extractant, because it has many merits such as improved separating ability of the fragrant component substance from the spice mixture, possibility of relatively low-temperature treatment, simple handling and operation, advantageous economic efficiency, etc. This extraction method requires operation at 50-500kg/cm<2>, preferably 60-300kg/cm<2> pressure in an extraction column at 25-150 deg.C, preferably 25-100 deg.C.

Description

DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Field of Industrial Application) The present invention relates to a method for extracting and separating flavor substances from a spice mixture (eg, curry powder).

More specifically, the present invention relates to a method for separating flavor substances from a spice mixture (for example, curry powder) using a fluid in a subcritical or supercritical state as an extraction agent.

Spices are aromatic or pungent substances used to season food, and most of them are the seeds of plants grown in the south.

Fruits, leaves of flowers, roots, skins, etc. are dried and used as companions.

These spices are sometimes treated with ethylene oxide or the like to sterilize processed foods, as processed foods may go bad due to bacterial contamination.

In recent years, the flavor components of these spices have been extracted and used in processed foods, which not only simplifies use but also avoids the harmful effects of bacterial contamination.

(Prior Art) When extracting flavor components from spices, there are examples of single spices, but there are no examples of methods for extracting flavor substances from composite spice mixtures.

It is very difficult to obtain complex flavor components using a single extraction agent and a single method using conventional extraction methods. The only way to do this is to prepare it, and conventional extraction methods include using various organic solvents or steam distillation.

In addition, in recent years, examples of extraction using supercritical fluid have become known, but all of these methods are intended only for single spices.

(Problems to be Solved by the Invention) An example of the mixed composition of a spice mixture such as curry powder is shown in Table 1 below.

Table 1 It is very complicated and impractical to extract each flavor component from these multi-component spices and prepare the extracted components using the conventional method. If possible, it would be extremely simple and advantageous, and the emergence of such a method has been desired. 5 In the conventional organic solvent extraction method, it is necessary to select the solvent depending on the target object, and there are also problems such as differences in flavor depending on the type of solvent used, loss of active ingredients during solvent recovery, residue of the used solvent, and flammability. There were many issues of concern, including the danger of injury and physical safety.

In addition, steam distillation is commonly used to extract essential oils, but
There is a concern that the effective flavor components may deteriorate or deteriorate due to moisture and heat.

Both of these methods require a large amount of energy consumption and are not economical.

[Structure of the invention]

(Means for solving the problem) In view of the above situation, the present inventors developed a spice mixture (
As a result of extensive research into a method for industrially advantageous obtaining flavor substances from (for example, curry powder), we found that if a subcritical reactor uses a supercritical fluid as an extractant, the drawbacks of the conventional method can be overcome. I realized that it was possible to obtain a high-quality complex flavor substance in one step by eliminating the above ingredients, and arrived at the present invention.

Furthermore, the present invention was completed by examining the extraction process, type of extractant, extraction and separation conditions, etc.

That is, the gist of the present invention is an extraction method characterized by using a fluid in a subcritical or supercritical state as an extractant when extracting and separating flavor substances from a spice mixture.

(Function) A method of separating an organic compound from a mixture containing it using a fluid in a supercritical state using a subcritical reactor is known, for example, as described in Japanese Patent Publication No. 10539/1983.
A method for extracting and separating flavor substances from a spice mixture is still completely unknown.0 A fluid in a supercritical state is a fluid in a state near or exceeding the critical temperature and pressure. For example, ethylene (9.9°C, 50 atm).

It is a fluid like carbon dioxide (31.0° C., '7L9 atm) that is near or above the critical state, and has a density close to that of a liquid and a large diffusion coefficient close to that of a gas.

Because of this characteristic, various compounds can be extracted rapidly and efficiently in large quantities, and the extractant can be easily separated. Another feature is that selective extraction can be performed because the ability to dissolve various compounds can be greatly changed by changing the pressure or temperature slightly.

In the present invention, generally any of the fluids in the subcritical or supercritical state can be used, but it is easy to handle because it has excellent separation ability between the spice mixture and flavor component substances and can be processed at a relatively low temperature. Carbon dioxide is usually used as the extraction agent because it has many advantages such as easy operation and economic advantage.

Embodiments of the present invention will be described below based on 70-sheets.

In FIG. 1, CO2 shilling-1 is compressed to a predetermined pressure using a compressor 2, and fcCO2 is brought to a predetermined extraction temperature through a heat exchange group 3, and brought into a subcritical or supercritical state into an extraction column 4. The extraction tower 4 is charged with a raw material spice mixture, and the CO2 phase containing the substances to be extracted is passed through a pressure reducing valve 5, cooled and liquefied in a sensor 7, and then transferred to a compressor 2t-
and then recycled.

In this process, an extract with a high content of light essential oil components is obtained as the initial extract, so first extract and separate a predetermined amount of this component, and then perform split extraction to obtain the heavy flavor components as an extract. It is also possible.

It can also be obtained by dividing it into components, such as the essential oil part and the oleoresin part.

In the above process, the pressure of CO2 in the extraction tower is 50~
500 Kg/cI/1. Preferably 60-300Kg
/cd.

It is necessary to maintain the temperature in the range of 25 to 150°C, preferably 25 to 100°C for extraction. If it is too low, not only will the accuracy of the separation become poor as it becomes liquefied CO2, but also energy is required to separate the extractant from the extract.On the other hand, if it is too high, the cost of the equipment will increase and there will be economic problems.

In addition to the above-mentioned pressure reduction method, the extraction agent and extract may be separated by a temperature change method, and it is also possible to perform semi-continuous operation using two extraction columns.

(Example) The following is an example of this F! 4t-More details will be explained in detail, but the present invention is not limited thereto.

Example 1 Commercially available (commercial use) curry extract-I Kf with a content of 5L
The mixture was packed into an extraction column, and extracted using CO2 at an extraction temperature of 40'' C9 pressure and 200 Kf/cd according to the process shown in Figure 1, and the extract was separated at room temperature and atmospheric pressure.
An extract of 0F and an extraction residue of 845F were obtained. After conducting a flavor test on the extract, we found that it was a curry extract similar to that obtained using conventional solvent extraction methods.

Example 2 Same force as used in Example 1 - 2KfK/d
Extraction was performed using CO2T-I, and the extracts obtained sequentially according to changes in extraction pressure were separated from the solvent at room temperature and atmospheric pressure. The obtained extracts were subjected to flavor tests at CI) 30F (extraction pressure 100-1301csf), (II) 60y (extraction pressure 150l50-180K), and (III) 150P (extraction pressure 200-250Krd). CI)K has a strong light essential oil flavor.
If) K had an overall well-balanced curry flavor, and (m) was confirmed to be an umami extract with a heavy flavor.

Furthermore, by appropriately mixing these CI) (II) and (III), it is possible to create extracts that are not only equivalent to conventional products, but also have a new flavor balance.

〔Effect of the invention〕

By the method of the present invention, high-quality flavor substances can be obtained, and the following superior effects can be achieved compared to conventional methods.

(1) High-grade flavor substances can be extracted directly and collectively from a multi-component complex spice (for example, curry bakda), which is convenient and advantageous.

(2) Since extraction is performed at a relatively low temperature and in an inert atmosphere, an extract can be obtained in high yield without deterioration.

(3) Depending on the extraction conditions, components such as the essential oil part and the oleoresin part can be obtained by dividing them. By optionally mixing them, preferred flavor substances are obtained.

(4) Various problems encountered in conventional extractions using organic solvents or steam distillation are avoided, and high-quality flavor substances can be obtained with high efficiency.

(5) Regarding the treatment of the extraction residue, there is no residual solvent used, so there is no danger when discarding it, it is easy to dispose of from a sanitary safety standpoint, and it can also be used separately.

[Brief explanation of the drawing]

FIG. 1 is a flow sheet showing an embodiment of the present invention. Applicant: Hiroshi Sasaki, Representative of Steel Manufacturing Chemical Industry Co., Ltd.

Claims (6)

[Claims] (1) An extraction method characterized by using a fluid in a subcritical or supercritical state as an extractant when extracting and separating flavor substances from a spice mixture. (2) The method according to claim (1), wherein the spice mixture is curry powder. (3) The method according to claim (1), wherein the fluid in a subcritical or supercritical state is carbon dioxide. (4) Subcritical or supercritical fluid has a pressure of 60 to 9
The method according to claim (2), wherein the carbon dioxide is carbon dioxide at a temperature of 25 to 100°C. (5) The conditions for separating the extract from the extraction phase are a pressure of 1 to 100 Kg/cm^2 and a temperature of 30 to 100°C.
The method according to claim (1), (3) or (4). (6) A patent claim characterized in that components such as essential oil parts and oleoresin parts are obtained by dividing them by performing stepwise extraction in the extraction process or by performing fractional separation in the separation process. The method described in ranges (1) to (4).