KR102496820B1 - Method for producing Gastrodia elata with reduced unpleasant odor - Google Patents

Abstract

The present invention comprises the steps of extracting an extract from Chunma; And it relates to a method for producing a cinnamon extract from which the unpleasant odor is removed, comprising the step of passing the cinnamon extract through a porous synthetic adsorbent to remove the unpleasant odor. In more detail, when the unpleasant odor of Cheonma is removed using the porous synthetic adsorbent of the present invention, ρ -cresol, which is the cause of the unpleasant odor, is effectively removed, and the functional components of Cheonma are not removed, thereby eliminating the unpleasant odor without loss of functional components. can be effectively removed.

Description

Manufacturing method of Chunma with reduced unpleasant odor {Method for producing Gastrodia elata with reduced unpleasant odor}

The present invention relates to a method for producing a Chunma extract with reduced unpleasant odor.

Gastrodia elata Blume is a perennial herbaceous plant belonging to the Orchidaceae family that grows wild in Korea, Japan, and China. It does not have chlorophyll and cannot assimilate carbon, so it grows in symbiosis with Armilla mellea, a basidiomycete. . The clinical efficacy of Chunma is widely recorded in various ancient documents including Herbal Medicine and Donguibogam. Even the private sector has been using Cheonma since early times.

However, Cheonma could not be developed as a functional food because it was bound by the Food and Drug Administration's regulations on items that cannot be used as food ingredients. development became possible.

Looking at the current status of research on Cheonma in Korea, the content mainly consists of cultivation of Cheonma and analysis of general components, and some studies on the efficacy of Cheonma such as platelet aggregation, anti-anxiety, and anti-convulsion have been reported. In the 2000s, the cultivation area of Cheonma increased and it became possible to use it as a food of Cheonma. After that, Cheonma's ingredient characteristics and functional beverage production, GABAergic neurotransmission control action of Cheonma's active ingredients and derivatives, and Cheonma extracts A study on the efficacy in various fields, such as the effect on local coronary circulation function, the melanin production inhibitory action of phenolic substances isolated from Chunma, the hangover removal effect by ethanol intake of the mixture of Hovenia japonica and Chunma, and the effect on learning and memory is being reported.

In this way, Cheonma, which has been traditionally used as an important medicinal material in oriental medicine, has recently received new attention as a food material, and some reports related to the physiologically active components of Cheonma have been presented. There are not many systematic studies as a food material. Therefore, more specific studies on the physiological activity of Chunma, which is effective in lowering blood pressure, lowering cholesterol, and nervous system diseases, and research as a food material based on this are needed.

Due to these functionalities, Cheonma has been developed as a processed food since it was registered as a food ingredient in 2000, but there are restrictions on its use due to its unique bitter taste, fishy taste, and unpleasant odor. In particular, the bitter and fishy taste of Chunma can be eliminated through drying, but the unpleasant odor does not disappear even after drying.

It is known that the unpleasant odor from Chunma is similar to that of pig feces, and the causative component is p-cresol. To remove p-cresol, a method of steaming and drying repeatedly several times or drying at a very high temperature has been used, but it is difficult to completely remove the unpleasant odor with this method. A problem with the above method is that p-cresol has a very high boiling point of 201.8 ° C and a melting point of 35.5 ° C, so it can exist as a solid at room temperature. In addition, even at a very low concentration, it exhibits a strong irritating odor for a long time, so an unpleasant odor may be felt strongly even if part of it is removed.

Accordingly, the present inventors have tried to effectively reduce the unpleasant odor of Cheonma. After preparing the extract by extracting Chunma with hot water, a high porous type synthetic adsorbent made of a copolymer of styren and divinyl benzene is used to selectively adsorb p-cresol. Thus, the present invention was completed by developing a method for removing unpleasant odor components.

The inventors of the present invention have tried to find a method for selectively removing p-cresol, a component that causes unpleasant odor in cheonma, without loss of functional components of cheonma, using a synthetic adsorbent, and have completed the present invention.

Accordingly, an object of the present invention is to provide a Chunma extract from which unpleasant odor is removed by using a porous non-polar synthetic adsorbent.

Another object of the present invention is to provide a method for preparing a Chunma extract from which unpleasant odor is removed using a porous, non-polar synthetic adsorbent.

Another object of the present invention is to provide a health food composition containing the Chunma extract with reduced unpleasant odor.

In order to achieve the above object, the present invention provides a Chunma extract from which unpleasant odor is removed by using a porous non-polar synthetic adsorbent.

In addition, the present invention provides a method for producing a Chunma extract from which unpleasant odor is removed using a porous, non-polar synthetic adsorbent.

In addition, the present invention provides a health food composition containing the Chunma extract with reduced unpleasant odor.

The manufacturing method of Cheonma from which unpleasant odor is removed according to the present invention has an effect of selectively removing p-cresol, a component that causes unpleasant odor unique to Cheonma, without removing the phenol component, which is a functional component of Cheonma.

1 is a diagram showing the results of measuring the ρ-cresol content in the Cheonma fraction from which the unpleasant odor was removed.
Figure 2 is a diagram showing the results of measuring the ρ-cresol content in the fractions fractionated 11 to 14 times among the Cheonma fractions from which the unpleasant odor was removed.
3 is a diagram showing the results of analyzing the contents of gastrodin and 4-HBA in the Chunma fraction from which the unpleasant odor was removed.
4 is a diagram showing the results of analyzing the contents of gastrodin and 4-HBA in fractions fractionated 3 to 10 times among the fractions of Cheonma from which the unpleasant odor was removed.
Figure 5 is a diagram showing the results of measuring the total phenolic component content in the Chunma fraction from which the unpleasant odor was removed.

Hereinafter, the present invention will be described in detail as an embodiment of the present invention with reference to the accompanying drawings. However, the following embodiments are presented as examples of the present invention, and if it is determined that detailed descriptions of well-known techniques or configurations may unnecessarily obscure the gist of the present invention, the detailed descriptions may be omitted. , the present invention is not limited thereby. Various modifications and applications of the present invention are possible within the scope of the claims described below and equivalents interpreted therefrom.

In addition, the terminology used in the present invention is a term used to appropriately express a preferred embodiment of the present invention, which may vary according to the intention of a user or operator or customs in the field to which the present invention belongs. Therefore, definitions of these terms will have to be made based on the content throughout this specification. Throughout the specification, when a certain component is said to "include", it means that it may further include other components without excluding other components unless otherwise stated.

All technical terms used in the present invention, unless defined otherwise, are used in the same meaning as commonly understood by one of ordinary skill in the art related to the present invention. In addition, although preferred methods or samples are described in this specification, those similar or equivalent thereto are also included in the scope of the present invention. The contents of all publications incorporated herein by reference are incorporated herein by reference.

The present invention provides a Chunma extract from which unpleasant odor is removed using a porous, non-polar synthetic adsorbent.

The term "extract" used in the present invention refers to a preparation obtained by extracting Chunma with an appropriate extraction solvent and evaporating the solvent to concentrate, but is not limited thereto, an extract obtained by extraction, a diluted solution of the extract, or It may be a dried product obtained by drying a concentrate or an extract, or a crude or purified product thereof. The Chunma extract can be prepared using general extraction methods, separation and purification methods known in the art. The extraction method is not limited thereto, but preferably, methods such as hot water extraction, hot water extraction, cold needle extraction, reflux cooling extraction, or ultrasonic extraction may be used.

In one embodiment of the present invention, the Cheonma extract is extracted with a solvent selected from the group consisting of water, methanol, alcohol, organic solvents and mixtures thereof, preferably water or fermented alcohol, but to effectively extract Cheonma For the purpose, it is not limited to this.

The present invention provides a method for preparing a Chunma extract from which unpleasant odor is removed using a porous, non-polar synthetic adsorbent.

As an embodiment of the present invention, the adsorbent for removing an unpleasant odor is for effectively removing an unpleasant odor, and is not limited thereto, and a porous adsorbent may be used, preferably a hydrophobic gel such as styrene and Copolymers of divinylbenzene may be used.

As an embodiment of the present invention, the copolymer of styrene and divinylbenzene has a particle size of 0.250-850 μm and a pore radius of 38-600 Å, and the filler is DIAION HP-20, MCI GEL CHP20P or Sepabeads SP850 or the like may be used, and most preferably, the filler is DIAION HP-20.

The DIAION HP-20 is a porous synthetic adsorbent that is a copolymer of styrene and divinylbenzene, and has a particle size of 0.250-850 ㎛ and a pore radius of 200-300 Å. DIAION HP-20 has a large number of pores and excellent adsorption capacity due to its high specific surface area. Because of its relatively large pores, it is suitable for adsorption of large molecules (MW 1,500 or more) and has the characteristics of easy elution of adsorbed materials. In addition, DIAION HP-20 has a hydrophobic particle surface, so when an organic substance is adsorbed to a synthetic adsorbent, the hydrophobic group in the organic molecule can be adsorbed.

The MCI GEL CHP20P is a porous synthetic adsorbent that is a copolymer of styrene and divinylbenzene, and has a particle size of 75-150 μm and a pore radius of 400-600 Å.

The Sepabeads SP850 is also a porous synthetic adsorbent that is a copolymer of styrene and divinylbenzene, and has a particle size of 250-850 μm and an average pore radius of 38 Å.

The present invention provides a health food composition or a health functional food composition containing the Chunma extract with reduced unpleasant odor.

In the case of using the Chunma extract with reduced unpleasant odor of the present invention as a health functional food and a health food composition, there is no particular limitation on the type of food. Examples of foods to which the Chunma extract with reduced unpleasant odor of the present invention can be added include drinks, meat, sausages, bread, biscuits, rice cakes, chocolates, candies, snacks, confectionery, pizza, ramen, other noodles, chewing gum, and ice cream. There are dairy products, various soups, beverages, alcoholic beverages and vitamin complexes, dairy products and milk-processed products, including, all of health functional foods and health food compositions in the conventional sense.

The health functional food and health food composition containing the extract of Chunma with reduced unpleasant odor according to the present invention may be added to food as it is or used together with other foods or food ingredients, and may be appropriately used according to conventional methods. The mixing amount of the Chunma extract with reduced unpleasant odor may be appropriately determined depending on the purpose of use (prevention or improvement). In general, the amount of the composition in the health functional food and health food composition may be added to 0.1 to 90 parts by weight of the total food weight. However, in the case of long-term intake for the purpose of health maintenance or health control, the amount may be less than the above range, and since there is no problem in terms of safety, the Chunma extract with reduced unpleasant odor can be used in an amount above the above range. can be used

The health functional food and health food composition of the present invention are not particularly limited in other components, except for containing the unpleasant odor-reduced cinnamon extract of the present invention as an essential component in the indicated ratio, and various flavors or natural Carbohydrates and the like may be contained as additional components. Examples of the aforementioned natural carbohydrates include monosaccharides such as glucose, fructose, and the like; disaccharides such as maltose, sucrose and the like; and polysaccharides such as conventional sugars such as dextrins, cyclodextrins, and the like, and sugar alcohols such as xylitol, sorbitol, and erythritol. As flavoring agents other than those mentioned above, natural flavoring agents (thaumatin, stevia extract (eg rebaudioside A, glycyrrhizin, etc.) and synthetic flavoring agents (saccharin, aspartame, etc.) can advantageously be used. The ratio of the natural carbohydrate is generally about 1 to 20 g, preferably about 5 to 12 g per 100 of the health functional food and health food composition of the present invention.

In addition to the above, the health functional food and health food composition containing the Chunma extract with reduced unpleasant odor of the present invention are various nutrients, vitamins, minerals (electrolytes), flavors such as synthetic flavors and natural flavors, colorants and enhancers (cheese, chocolate, etc.), pectic acid and its salts, alginic acid and its salts, organic acids, protective colloidal thickeners, pH adjusters, stabilizers, preservatives, glycerin, alcohol, carbonating agents used in carbonated beverages, etc. . In addition, the health functional food and health food composition of the present invention may contain natural fruit juice, fruit juice beverages, and fruit flesh for preparing vegetable beverages. These components may be used independently or in combination.

Hereinafter, the present invention will be described in more detail through the following examples. However, the following examples are only examples for easily explaining the content and scope of the technical idea of the present invention, and thereby the technical scope of the present invention is not limited or changed. In addition, based on these examples, it can be easily determined by those skilled in the art that various modifications and changes are possible within the scope of the technical spirit of the present invention.

Example 1. Preparation of Fractions of Cheonma Extract from which Unpleasant Odor is Removed Using a Synthetic Adsorbent

The hot water extract of Cheonma was purchased from a Chunma processing company located in Sangju, Gyeongsangbuk-do and used without any other raw materials other than Cheonma. Diaion HP-20 (HP-20, Supelco, Bellefonte, USA) was used as a porous non-polar synthetic adsorbent used in the following experiments, and fermented alcohol and distilled water were used as elution solvents. Gastrodin, 4-HBA, and ρ-cresol used in the analysis were purchased from Sigma-Aldrich (St. Louis, MO, USA).

In order to confirm the deodorizing effect of HP-20, a porous non-polar synthetic adsorbent, on the Chunma extract, fractions were prepared in a column filled with HP-20. The preparation of the fractions was performed by loading 50 ml of the Chunma extract into an open column filled with HP-20 with a diameter of 25 mm and a length of 100 mm, followed by distilled water (Fr. 1, Fr. 2, Fr. 3), 10% ethanol (Fr. 4, Fr. 5), 20% ethanol (Fr. 6, Fr. 7), 30% ethanol (Fr. 8, Fr. 9), 40% ethanol (Fr. 10, Fr. 11), 50% ethanol (Fr. 12, Fr. 13) and 95% ethanol (Fr. 14, Fr. 15) solutions were sequentially added for elution, and each fraction was aliquoted by 50 ml and used in the experiment.

Experimental Example 1. Measurement of ρ-cresol content of Chunma extracts and fractions

In order to confirm the deodorizing effect of Cheonma extract, the content of ρ -cresol, which is the biggest cause of unpleasant odor of Cheonma, was analyzed.

HPLC-UVD and Synergy fusion-RP18 columns were used for analysis. The mobile phase is acetonitrile (A) and water (B) under gradient conditions (0-5 min: 18-18% A, 5-20 min: 18-40% B, 20-25 min: 40-40% A, 25-45 min: 40-50% A), column temperature 30 ℃, flow rate 0.8 ㎖ / min, injection amount 10 ㎖, detection wavelength 280 ㎚ was analyzed, ρ -cresol was used as a standard.

As a result, as shown in FIGS. 1 and 2, the ρ -cresol content of the Chunma extract was 11.769±0.715 μg/ml. In particular, as shown in FIG. 2, among the fractions separated from the HP-20 resin, ρ -cresol was detected from fraction 12 (Fr. 12) and showed the highest content in fraction 14 (Fr. 14). The ρ -cresol contents of fractions 12 (Fr. 12), 13 (Fr. 13), 14 (Fr. 14), and fraction 15 (Fr. 15) were 1.898, 3.586, 6.047, and 0.391 μg/ml, respectively. 11.922 ± 0.609 μg / ml showed a content similar to that of the extract.

Experimental Example 2. Measurement of the content of gastrodin and 4-HBA in the extracts and fractions of Chunma

Gastrodin and 4-HBA contents were analyzed to confirm the loss of major functional components of Cheonma extract during the selective removal of ρ -cresol, an unpleasant odor component of Cheonma extract.

For the analysis of gastrodin and 4-HBA, HPLC-UVD (1200 series, Agilent Technologies, Santa Clara, CA, USA) and Synergy fusion-RP18 column (250 × 4.6 mm, 4 ㎛, Phenomenex, Torrance, CA, USA) were used. used The mobile phase is 0.1% acetic acid / acetonitrile (A) and 0.1% acetic acid / water (B) gradient conditions (0-5 min: 5-5% A, 5-15 min: 5-10% B, 15-16 min : 10-95% A, 16-24 min: 95-95% A, 24-25 min: 95-5% A, 25-30 min: 5-5% A), column temperature 30°C, flow rate 1.0 ml/ Min, injection amount 10 μl, detection wavelength 280 nm was analyzed. Gastrodin and 4-HBA were used as standards.

Gastrodin was distributed from 3 to 6 times because it has stronger hydrophilicity due to the sugar bonded to 4-HBA.

As a result, as shown in FIGS. 3 and 4, the gastrodin contents of fractions 3 (Fr. 3), 4 (Fr. 4), 5 (Fr. 5), and 6 (Fr. 6) were 37.934, 146.625, 209.475 and 12.420 μg/ml, and the total content was 406.454 ± 26.941 μg/ml, and it was confirmed that most of the gastrodin was recovered in an ethanol solution at a concentration of 20% or less compared to the Chunma extract (403.131 ± 17.424 μg/ml).

In addition, as a result of analyzing the content of 4-HBA, known as the main functional component of Chunma along with gastrodin, it was distributed between fraction 4 (Fr. 4) and fraction 10 (Fr. 10), and the content by fraction was 4 (Fr. 4), 5 (Fr. 5), 6 (Fr. 6), 7 (Fr. 7), 8 (Fr. 8), 9 (Fr. 9) and 10 (Fr. 10) fractions 5.741, respectively; 119.569, 173.563, 78.951, 9.207, 1.972, and 0.427 μg/ml were mostly eluted from fractions 5 (Fr. 5)-7 (Fr. 7), and were separated from 10% ethanol solution and recovered in 40% ethanol solution. It became. The total content of 4-HBA recovered was 389.430±13.981 μg/ml, which was more than 95% recovery compared to 408.154±14.575 μg/ml present in the extract.

Therefore, it was confirmed that the loss of major functional components of cheonma hardly occurs even when the unpleasant odor is removed by the method of removing the unpleasant odor of cheonma of the present invention.

Experimental Example 3. Measurement of total phenol content of Chunma extracts and fractions

In addition to ρ -cresol, which is the cause of unpleasant odor, including gastrodin and 4-HBA, known as major functional components, in Chunma, there are various phenolic components, so the overall distribution of phenolic components according to the removal of unpleasant odor was confirmed.

In order to confirm the distribution of total phenol components in the Chunma fractions, the total phenol content in the fractions was measured (Dewanto et al., 2002). After adding 2 ml of 2% Na ₂ CO ₃ solution to 100 μl of each fraction, it was allowed to stand for 3 minutes, and then 100 μl of 1 N Folin-Ciocalteu reagent (Sigma-Aldrich) was added and mixed. After leaving the reaction solution at room temperature for 30 minutes, absorbance was measured at 750 nm. A calibration curve was prepared using gallic acid (Sigma-Aldrich) as a standard material, and the total phenol content was expressed as mg gallic acid in 1 ml of the sample.

As a result, as shown in FIG. 5, the total phenol content of the Cheonma extract from which the unpleasant odor was not removed was 2,476.087 μg/ml, and the total phenol content of the fraction from which the unpleasant odor was removed was 2,260.56 ± 140.057 μg/ml, showing a recovery rate of 91% or more. was

Judging from these results, except for fractions 12 (Fr. 12) to 15 (Fr. 15) where the unpleasant odor is distributed, the phenol content was 1,771.47 ± 62.563 ㎍/㎖, and even after removing the unpleasant odor, the total phenolic components It is estimated that 71% of this can be recovered.

Specifically, the results of confirming the correlation between the distributions of major components in the fractions are shown in Table 1 below.

Positive correlations were shown between gastrodin, 4-HBA, and total phenol contents, which are functional components present in the fractions, indicating that the distributions were similar. In particular, high correlation of 0.889 (p<0.01) between 4-HBA and total phenol contents. , it is estimated that the content of 4-HBA occupies a significant part of the total phenol content.

On the other hand, ρ -cresol, an unpleasant odor component, did not show a significant correlation with gastrodin, 4-HBA, and total phenol content, and showed a negative correlation, indicating that the distribution was different from that of functional components.

Therefore, when looking at the distribution of phenol components in the fractions from which the unpleasant odor was removed, the highest content was found in fractions 5 (Fr. 5) and 6 (Fr. 6), where gastrodin and 4-HBA were distributed in high concentrations. As shown, it is determined that a significant portion of the phenolic components present in fractions 5 (Fr. 5) and 6 (Fr. 6) among the fractions from which the unpleasant odor was removed are gastrodine and 4-HBA.

Claims (13)

Extracting an extract from Chunma; And removing the unpleasant odor by passing the cheonma extract through a copolymer of styrene and divinylbenzene;
In the step of removing the unpleasant odor, distilled water and ethanol are used as the elution solvent, but after fractionation using distilled water, fractionation is performed while increasing the concentration of ethanol with 10% ethanol, 20% ethanol, 30% ethanol, and 40% ethanol. It is characterized by recovering each fraction from which the unpleasant odor has been removed through the process,
The causative component of the unpleasant odor is ρ -cresol,
Manufacturing method of cheonma extract from which unpleasant odor is removed. delete delete According to claim 1,
The copolymer of styrene and divinylbenzene has a particle size of 0.250-850 μm and a pore radius of 38-600 Å. According to claim 1,
The extract is a method for producing a chunma extract from which an unpleasant odor is removed, characterized in that water is extracted as a solvent. delete delete delete delete According to claim 1,
The step of removing the unpleasant odor is followed by fractionation with distilled water three times, fractionation with 10% ethanol twice, 20% ethanol twice, 30% ethanol twice, and 40% ethanol twice. , manufacturing method. According to claim 1,
After the step of removing the unpleasant odor, further comprising the step of washing the synthetic adsorbent with a 50 to 100% ethanol solution. delete delete

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