KR20200098991A - Method for Extracting Folic acid from Mushroom - Google Patents

Abstract

The present invention relates to a method for extracting high concentration folic acid with a high yield using mushrooms. By using an extraction solvent containing organic acid, the organic acid stabilizes a structure of folic acid to prevent the destruction of folic acid, and the extraction yield of folic acid is increased, thereby obtaining high concentration folic acid in the high yield.

Description

Folic acid extraction method using mushrooms{Method for Extracting Folic acid from Mushroom}

The present invention relates to a method for extracting a high concentration of folic acid with a high yield using mushrooms.

Mushrooms are divided into mycelium, which is a nutritional organ, and fruiting body with spores, which are reproductive organs, mainly growing while feeding nutrition by spreading mycelium on fallen leaves buried on or in the ground, dry grass, and tree branches in mountains, or parasitic on the trunk or root of a dead tree. And grow. Recently, it has been reported that mushrooms contain various functional ingredients and physiologically active substances, and as many modern people are interested in healthy foods, the demand for edible and medicinal mushrooms increases. It is difficult to supply by collection and is cultivated by artificial methods. The composition of mushrooms is 70-95% moisture and 5-30% organic and inorganic components. Dried mushrooms contain 15 to 30% protein, 2 to 10% lipid, 50% sugar, crude fiber and 5 to 10% of minerals such as potassium, calcium, phosphorus and vitamins. These mushrooms are used not only as general food ingredients, but also as raw materials in various fields such as health functional foods, cosmetics, and pharmaceuticals.

Folic acid (folic acid) is one of the vitamin B complex, widely distributed in nature, especially fruits, vegetables, legumes, it is contained in a lot of animal liver. Folic acid is essential for synthesizing nucleic acids and amino acids necessary for cell division and growth in the body, and is used for growth development and red blood cell production by binding with vitamin B12. It not only promotes the secretion of noradrenaline, a neurotransmitter in the brain, but also blood vessels. Contributes to lowering the risk of high blood pressure by relaxing. Therefore, if adults continue to consume folic acid, it prevents anemia and helps blood vessel health and brain health.In particular, for pregnant women, folic acid supplements are prescribed because it can prevent premature birth or stillbirth of the fetus, low birth weight, and birth of neural tube defects. do. Folic acid is used for a variety of purposes, such as food additives added to supplement nutrients insufficient in processing foods such as infant food and health functional foods, and nutritional supplements taken to promote health or prevent nutritional deficiencies. At this time, folic acid is mainly used in a chemically synthesized form to reduce the production cost of the product. Recently, as consumers interested in health increase, preference for substances extracted from natural materials rather than chemical synthesis is increasing.

Therefore, the present inventors have explored various methods for extracting folic acid from natural ingredients in accordance with the market trend, and in the present invention, high-concentration folic acid is used in high yield so that folic acid is not destroyed or lost by using mushrooms rich in nutrients such as vitamins. The extraction method was completed.

Korean Patent Registration No. 10-1906839 Korean Patent Registration No. 10-1881638

In order to solve the above problems, the present invention (a) drying the mushrooms; (b) adding the mushrooms and organic acid dried in step (a) to the extraction solvent and heating to obtain an extract; (c) concentrating the extract to obtain a concentrate; And (d) drying the concentrate to obtain a dried product, wherein the organic acid is used in an amount of 3 to 10 parts by weight based on 100 parts by weight of the extraction solvent, and an object thereof is to provide a method for extracting folic acid using mushrooms. .

Here, the mushroom of the step (a) may be one or more selected from the group consisting of oyster mushrooms, shiitake mushrooms, enoki mushrooms, king oyster mushrooms, mushroom mushrooms, and matsutake mushrooms.

In addition, step (a) may be hot air drying the mushrooms at 40 to 90°C for 2 to 10 hours.

In addition, the organic acid in step (b) may be at least one selected from the group consisting of citric acid, acetic acid, tartaric acid, malic acid, succinic acid, acetic acid, formic acid, and lactic acid.

In addition, the step (b) is to extract the dried mushrooms and organic acid in water and heat for 2 to 10 hours at 60 to 90 ℃, the water is used 15 to 25 times the total weight of the dried mushrooms I can.

In addition, the step (c) may be to obtain a concentrated solution having a solid content of 25 to 55 brix by concentrating the extract under reduced pressure at 40 to 60°C for 6 to 10 hours.

In addition, the drying in step (d) may be freeze drying or vacuum drying.

In addition, after the step (d), it may further include the step of pulverizing the dried product.

A method for extracting folic acid using mushrooms according to an embodiment of the present invention includes the steps of: (a) drying the mushrooms; (b) adding the mushrooms and organic acid dried in step (a) to the extraction solvent and heating to obtain an extract; (c) concentrating the extract to obtain a concentrate; And (d) drying the concentrate to obtain a dried product, and the organic acid may be used in an amount of 3 to 10 parts by weight based on 100 parts by weight of the extraction solvent.

Looking specifically at the steps (a) to (d) are as follows.

(a) drying the mushrooms

As the mushrooms, the types of mushrooms that can be used for edible or medicinal purposes can be used without limitation, for example, oyster mushrooms, shiitake mushrooms, enoki mushrooms, oyster mushrooms (big oyster mushrooms), mushrooms, matsutake mushrooms, chaga mushrooms, blossom mushrooms , Pseudomonas mushrooms, roe deer mushrooms, reishi mushrooms, neungi mushrooms, lean mushrooms, maitake mushrooms, manga beech mushrooms, salicornia mushrooms, cloud mushrooms, and white agaric mushrooms (Agaricus mushrooms). In the present invention, it is preferable to use mushrooms that are readily available in the vicinity, and may be one or more selected from the group consisting of oyster mushrooms, shiitake mushrooms, enoki mushrooms, oyster mushrooms, mushrooms, and matsutake mushrooms. In particular, it is more preferable to use oyster mushrooms having a high folic acid content. These mushrooms can be used after washing or cutting before drying. First, the mushrooms are cleaned to remove foreign substances, and if the size of the mushrooms is large, they can be cut into suitable sizes for drying.

When the mushrooms are dried and used, the folic acid contained in the mushrooms is concentrated, and a higher concentration of folic acid can be obtained than when the undried mushrooms are used. As a method of drying the mushrooms, a drying method known in the art may be used without limitation, and it is preferable to dry the mushrooms with hot air at 40 to 90° C. for 2 to 10 hours so that the folic acid contained in the mushrooms is not destroyed. At this time, if dried at less than 40℃ or less than 2 hours, the moisture content in the mushrooms is high, so the extraction yield of folic acid is low, and if dried at more than 90℃ or more than 10 hours, not only moisture but also folic acid is lost due to heat. Can be. In order to extract folic acid more efficiently, it is more preferable to perform hot air drying at 70° C. or higher for 8 hours or longer.

(b) adding dried mushrooms and organic acid to the extraction solvent and heating to obtain an extract

As the extraction solvent, an extraction solvent known in the art may be used without limitation, for example distilled water, alcohol of C ₁ ~ C ₄ , dimethyl formamide, dimethyl sulfoxide (DMSO), acetone, Acetonitrile, ethyl acetate, methyl acetate, pentane, hexane, chloroform, diethyl ether, carbon tetrachloride, tetrahydrofuran (THF), and the like. In the present invention, it is suitable to extract folic acid, which is a water-soluble vitamin, and in order to prevent chemical substances from remaining in the final product or unnecessary substances to be generated in the extraction process, it is preferable to use distilled water as a solvent.

In order to effectively extract folic acid from mushrooms, an organic acid may be further added to the extraction solvent. The organic acid stabilizes the structure of folic acid during extraction to prevent the destruction of folic acid by heat, and may increase the extraction yield of folic acid. As such an organic acid, it is preferable to use one selected from the group consisting of citric acid, acetic acid, tartaric acid, malic acid, succinic acid, acetic acid, formic acid and lactic acid, and it is more preferable to use citric acid that has weak acidity and can be safely used as a food additive. Do. At this time, in order to increase the extraction yield of folic acid, it is preferable to use the organic acid in an amount of 3 to 10 parts by weight based on 100 parts by weight of the extraction solvent. If the amount of the organic acid is less than 3 parts by weight, the effect of increasing the yield by the organic acid cannot be expected, and if it exceeds 10 parts by weight, the acidity of the solvent becomes strong, and folic acid may be destroyed. In order to more efficiently extract folic acid, it is more preferable to use the organic acid in an amount of 5 to 7 parts by weight based on 100 parts by weight of the extraction solvent.

As a method of obtaining an extract containing folic acid from mushrooms, extraction methods known in the art can be used without limitation, and examples include cold needle extraction, ultrasonic extraction, reflux cooling extraction, hot water extraction, pressure extraction, and solvent extraction. . In the present invention, in order to extract high-concentration folic acid in a high yield, the dried mushrooms and organic acids are added to water and extracted by heating at 60 to 90°C for 2 to 10 hours, and water is extracted from 15 to the total weight of the dried mushrooms. It is desirable to use 25 times. At this time, when heated at less than 60°C or less than 2 hours, the concentration of folic acid in the extract is low, and when heated for more than 90°C or 9 hours, folic acid may be destroyed by heat. In order to extract folic acid more efficiently, it is more preferable to heat it at 70° C. or higher for 4 hours or longer. In addition, if the amount of water used is less than 15 times, the solvent is insufficient and folic acid cannot be sufficiently extracted. If it exceeds 25 times, the extracted folic acid is diluted in the solvent and the concentration of folic acid in the extract is rather low. Concentration can take a long time.

When solids such as mushroom residue and impurities are contained in the extract obtained by this method, precipitates may form over time or negatively affect the quality of the final product. Therefore, in order to remove the solids contained in the extract, a filtration method known in the art may be used without limitation, and for example, it may be filtered using a filter press, a centrifuge, or a filter paper. In order to completely remove the solids, the filtration process may be repeated one or more times.

(c) concentrating the extract to obtain a concentrate

The extract is a liquid extract containing folic acid extracted from the mushroom obtained through step (b), and it can be concentrated to obtain a high concentration of folic acid.

As a method of concentrating the extract, a concentration method known in the art may be used without limitation, and examples include heat concentration, vacuum heating concentration, freeze concentration, evaporation concentration, vacuum low temperature concentration, and the like. In the present invention, in order to efficiently concentrate, the extract is concentrated under reduced pressure at a temperature of 40 to 60° C. at a pressure of 0.05 to 0.1 Mpa for 6 to 10 hours to obtain a concentrate having a solid content of 25 to 55 brix. desirable. At this time, if the concentration is less than 40℃ or less than 6 hours, it takes a lot of time and cost to concentrate the extract, and if it is concentrated more than 70℃ or more than 10 hours, folic acid is destroyed by heat or the solid content in the concentrate is destroyed. It can be agglomerated and difficult to dry in a later step.

(d) drying the concentrated solution to obtain a dried product

The concentrate is obtained by concentrating the extract containing folic acid obtained through step (c), and can be dried for easy storage and use.

As a method of drying the concentrate, any drying method known in the art can be used without limitation. For example, freeze drying, vacuum drying, aeration drying, blowing drying, hot air drying, flow drying, spray drying, infrared drying, high frequency drying, etc. Can be lifted. In the present invention, it is preferable to freeze drying or vacuum drying so that folic acid is not destroyed without using an excipient or the like in the concentrate during drying. The freeze-drying is a method of drying the concentrate at a low temperature of -10 to -30°C. It is easy to store at room temperature for a long period of time, and a dried product having excellent resolubility in water can be obtained. The vacuum drying is a method of drying by evaporating water while lowering the pressure, and at this time, heat of 40 to 60° C. may be supplied to accelerate the rate of water evaporation.

The dried product obtained through such a concentration process may be further subjected to a pulverization process, and the particles are fine, so that it is easy to mix with other materials and can be prepared into a powder in a form that is well soluble in water.

As a method of pulverizing the dry matter, any pulverization method known in the art can be used without limitation. For example, a ball mill, hammer mill, rod mill, vibration mill, roll crusher, centrifugal impact mill, vertical bead mill, wear mill, vibration mill , A pin mill, a hammer mill, a pulverizer, a crusher, a knife cutter, and the like. The size of the powder subjected to this pulverization process may be 100 mesh.

In the method for extracting folic acid using mushrooms according to the present invention, the organic acid stabilizes the structure of the folic acid by using an extraction solvent containing the organic acid, thereby preventing the destruction of folic acid by heat, and increasing the extraction yield of folic acid to obtain a high concentration of folic acid. It can be obtained in high yield.

1 is a flow chart of a method for extracting folic acid using mushrooms according to an embodiment of the present invention.

Hereinafter, a method for extracting folic acid using mushrooms according to the present invention will be described in more detail with reference to the accompanying drawings. However, these descriptions are provided by way of example only to aid understanding of the present invention, and the scope of the present invention is not limited by these exemplary descriptions.

Experimental Example 1. Measurement of folic acid content of oyster mushroom

The oyster mushrooms were washed to remove foreign substances and then dried.

From the prepared oyster mushrooms, 10 g of each of samples 1 to 4 were collected and placed in a 50 ml flask, and 20 ml of a 5 mM sodium hexanesulfonate/0.1% acetic acid solution was added. After crushing the oyster mushrooms using ultrasonic waves for 30 minutes, 5 mM Sodium hexanesulfonate/0.1% acetic acid solution was added to adjust the final volume to 50 ml. Thereafter, centrifugation was performed at 35,000 xg for 10 minutes, and the supernatant was taken and filtered through a 0.2 μm filter paper (membrane filter) to prepare a test solution. Using each test solution, the folic acid content was measured by HPLC under the conditions shown in Table 1 below, and the results are shown in Table 2 below.

Item Condition Instrument Agilent Technologies 1200 Series Column Agilent XDB-C18 (4.6*250 mm. 5 μm) Solvent Solution A 5 mM sodium hexanesulfonate/0.1% acetic acid solution B solution Methanol:DW = 70: 30 Column Temp. 30℃ Wavelength UV 280 nm Flow rate 1.0 ml/min Injecton volumn 20 μl

Sample 1 Sample 2 Sample 3 Sample 4 Folic acid (㎍/100g) 56.3 54.1 55.8 57.2

As shown in Table 2, samples 1 to 4 of oyster mushrooms were found to contain folic acid 56.3, 54.1, 55.8, and 57.2 μg/100g, respectively.

Experimental Example 2. Measurement of moisture and folic acid content of oyster mushroom according to drying conditions

The moisture and folic acid content of oyster mushrooms were measured according to the drying conditions.

The oyster mushrooms were washed to remove foreign substances and then dried.

Prepared 1 kg of oyster mushrooms were dried with hot air at 40, 50, 60, 70, 80, 90°C for 2, 4, 6, 8, 10 hours, and then the moisture and folic acid content were measured, and the results are shown in Tables 3 and 4 below. same.

Moisture content was measured using an infrared moisture meter for measuring the transmitted light and reflected light by irradiating infrared rays to the sample, and the folic acid content was measured in the same manner as in Experimental Example 1.

Moisture content
(%) Drying time 2 hours 4 hours 6 hours 8 hours 10 hours Drying temperature 40℃ 87.5 65.2 40.5 32.4 12.4 50℃ 85.1 60.3 32.1 28.1 11.2 60℃ 85.2 58.3 30.5 17.4 10.6 70℃ 82.3 50.1 25.6 17.8 9.4 80℃ 80.3 45.3 20.2 12.5 8.6 90℃ 78.1 40.1 18.1 10.5 8.1 * If the moisture content is 10-15%, it is judged to be completely dried

Folic acid content
(㎍/100g) Drying time 2 hours 4 hours 6 hours 8 hours 10 hours Drying temperature 40℃ 54.5 75.6 80.6 101.2 258.1 50℃ 63.1 70.5 92.1 213.5 366.9 60℃ 57.6 85.3 120.3 410.6 430.1 70℃ 55.3 80.1 190.5 400.3 515.5 80℃ 43.8 95.8 213.9 480.1 500.1 90℃ 40.8 90.1 200.1 350.5 456.3

As shown in Tables 3 and 4, when the oyster mushrooms were dried under conditions of 60° C. or more and 8 hours or more, the moisture in the oyster mushrooms was removed, and the folic acid content was found to increase.

Experimental Example 3. Setting Conditions for Extracting Folic Acid from Oyster Mushrooms

In order to establish standardized process conditions for efficient folic acid extraction from oyster mushrooms, folic acid content was measured according to hot water extraction conditions of oyster mushrooms.

Oyster mushrooms were washed to remove foreign substances and then dried to prepare them, and dried at 70° C. for 10 hours. After heating at 60, 70, 80, 90℃ for 2, 4, 6, 8 hours using 15, 20, 25, 30 ℓ of water in 1 kg of dried oyster mushroom, folic acid and solid content in the extract Was measured, and the results are shown in Tables 5 to 7.

The solid content was measured using a digital sugar content meter that measures the solid content by changing the refractive index through which light is transmitted according to the molecular content in the liquid, and the folic acid content was measured in the same manner as in Experimental Example 1.

Extraction conditions Extract Water quantity
(ℓ) Heating time
(time) Heating temperature
(℃) Final quantity
(ℓ) Solid content
(brix) Theoretical yield
(kg) Folic acid content
(㎍/100g) 15 10 90 5.5 2.8 0.154 42.6 20 10 90 12.0 2.5 0.300 45.5 25 10 90 16.5 1.9 0.310 44.0 30 10 90 22.0 1.2 0.264 41.2

As shown in Table 5, as a result of measuring the content of folic acid in the extract according to the amount of water, it was found that the content of folic acid was highest when the amount of water was 20 ℓ.

Extraction conditions Extract Water quantity
(ℓ) Heating time
(time) Heating temperature
(℃) Final quantity
(ℓ) Solid content
(brix) Theoretical yield
(kg) Folic acid content
(㎍/100g) 20 2 90 12.5 1.2 0.150 35.4 20 4 90 12.5 1.8 0.225 40.5 20 6 90 12.5 2.1 0.262 41.8 20 8 90 12.5 2.5 0.312 45.8

As a result of measuring the folic acid content in the extract according to the heating time as shown in Table 6, it was found that the folic acid content was the highest when heated for 8 hours.

Extraction conditions Extract Water quantity
(ℓ) Heating time
(time) Heating temperature
(℃) Final quantity
(ℓ) Solid content
(brix) Theoretical yield
(kg) Folic acid content
(㎍/100g) 20 8 60 12.5 2.4 0.150 36.4 20 8 70 12.5 2.5 0.225 45.0 20 8 80 12.5 2.5 0.262 44.9 20 8 90 12.5 2.6 0.312 45.8

As a result of measuring the folic acid content in the extract according to the heating temperature as shown in Table 7, it was found that the folic acid content was high when heated at 70°C or higher.

Experimental Example 4. Confirmation of Conditions for Extracting Folic Acid from Oyster Mushrooms

By applying the heating time and temperature conditions identified in Experimental Example 3, the folic acid content of the extract extracted from oyster mushroom in a large amount was measured.

In a medium-sized extractor (volume 200 kg), 10 kg of oyster mushrooms dried in the same manner as in Experimental Example 3, 200 ℓ of water (20 times the amount of water used in oyster mushrooms) was added, and for 2, 4, 6, 8, 10 hours After heating at 70, 80, and 90°C to obtain an extract, the folic acid content in the extract was measured, and the results are shown in Table 8 below.

The folic acid content was measured in the same manner as in Experimental Example 1.

Folic acid content
(㎍/100g) Heating time 2 hours 4 hours 6 hours 8 hours 10 hours Heating temperature 70℃ 12.3 23.5 30.9 45.5 46.0 80℃ 10.6 20.7 25.6 40.1 39.2 90℃ 9.5 18.5 20.7 35.4 36.5

As shown in Table 8, when the oyster mushroom is heated at 70° C., the content of folic acid in the extract is higher than when heated at 80 and 90° C., and the extracted folic acid also increases as the heating time increases.

Experimental Example 5. Addition of citric acid to improve the extraction efficiency of folic acid

By applying the conditions identified in Experimental Example 4, the folic acid content according to the amount of citric acid was measured in order to improve the folic acid extraction efficiency of oyster mushroom.

In a medium-sized extractor, 10 kg of oyster mushrooms dried in the same manner as in Experimental Example 3, 200 ℓ of water, and citric acid (3, 5, 7, 10% added to the amount of water used) were added, and the extract was heated at 70° C. for 8 hours. After obtaining, the folic acid content was measured, and the results are shown in Table 9 below.

The folic acid content was measured in the same manner as in Experimental Example 1.

Citric acid 3% 5% 7% 10% Folic acid (㎍/100g) 52.8 60.5 60.3 55.4

As shown in Table 9, as a result of measuring the folic acid content in the extract according to the amount of citric acid used, it was found that the folic acid content was highest when 5 or 7% citric acid was used. From these results, it can be seen that citric acid prevents the destruction or loss of folic acid due to heat and increases the extraction efficiency of folic acid.

Experimental Example 6. Concentration condition setting of oyster mushroom extract

The folic acid content of the oyster mushroom concentrate according to the concentration conditions was measured.

10 kg of oyster mushrooms dried in the same manner as in Experimental Example 3, 200 ℓ of water, and 10 kg of citric acid were added to a medium-sized extractor, and heated at 70° C. for 8 hours to obtain an extract. The extract was concentrated under reduced pressure at 50° C. to 0.08 MPa, and the concentration was stopped when the solid content reached 30, 40, and 50 brix to measure the folic acid content in the concentrate, and the results are shown in Table 10 below.

The solid content was measured in the same manner as in Experimental Example 3, and the folic acid content was measured in the same manner as in Experimental Example 1.

Solid content (brix) 30 40 50 Folic acid (㎍/100g) 284.5 428.6 450.1

As shown in Table 10, it was found that as the solid content increased by concentrating the extract, the folic acid content in the concentrated solution also increased.

Experimental Example 7. Setting of drying conditions for oyster mushroom concentrate

The folic acid content of the dried oyster mushrooms according to the freezing conditions was measured.

10 kg of oyster mushrooms dried in the same manner as in Experimental Example 3, 200 ℓ of water, and 10 kg of citric acid were added to a medium-sized extractor, and heated at 70° C. for 8 hours to obtain an extract. The extract was concentrated under reduced pressure at 50° C. to 0.08 MPa, and concentration was stopped when solid content of 30, 40, and 50 brix was reached. Each concentrate was freeze-dried or vacuum-dried to obtain a dried product, and then powdered using a pin mill (100 mesh). The folic acid content in the powder was measured, and the results are shown in Table 11 below.

The folic acid content was measured in the same manner as in Experimental Example 1.

Folic acid
(㎍/100g) Solid content (brix) 30 40 50 Freeze drying 840.5 1020.1 820.5 Vacuum drying 820.4 1020.5 830.1

As shown in Table 11, when the concentrate was dried, the folic acid content increased by about two times compared to the case where it was not dried (see Table 10 in Experimental Example 6), and there was no difference in the folic acid content according to the drying method.

Based on these experiments, the method of extracting folic acid using mushrooms according to the present invention is to obtain an extract from oyster mushrooms dried using an extraction solvent containing citric acid, and concentrate and dry it to extract high-concentration folic acid in high yield. Confirmed that it can.

Claims (8)

(a) drying the mushrooms;
(b) adding the mushrooms and organic acid dried in step (a) to the extraction solvent and heating to obtain an extract;
(c) concentrating the extract to obtain a concentrate; And
(d) drying the concentrated solution to obtain a dried product
Including,
A method for extracting folic acid using mushrooms using the organic acid in an amount of 3 to 10 parts by weight based on 100 parts by weight of the extraction solvent.
The method of claim 1,
The mushroom of step (a) is one or more selected from the group consisting of oyster mushrooms, shiitake mushrooms, enoki mushrooms, king oyster mushrooms, mushrooms and matsutake mushrooms.
The method of claim 1,
The step (a) is a method of drying the mushrooms with hot air at 40 to 90°C for 2 to 10 hours.
The method of claim 1,
The organic acid in step (b) is at least one selected from the group consisting of citric acid, acetic acid, tartaric acid, malic acid, succinic acid, acetic acid, formic acid and lactic acid.
The method of claim 1,
In the step (b), the dried mushrooms and organic acids are added to water and extracted by heating at 60 to 90° C. for 2 to 10 hours, and the water is used in an amount of 15 to 25 times the total weight of the dried mushrooms. .
The method of claim 1,
In the step (c), the extract is concentrated under reduced pressure at 40 to 60° C. for 6 to 10 hours to obtain a concentrated solution having a solid content of 25 to 55 brix.
The method of claim 1,
The drying in step (d) is freeze drying or vacuum drying.
The method of claim 1,
After the step (d), the method further comprising the step of pulverizing the dried product.

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