JP2000239301A - Extraction of fucoidan - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an extraction method that gives fucoidan of a desired average molecular weight in high yield with no problem of corrosion of the facility and the like in the production installation. SOLUTION: In this extraction process, fucoidan is extracted from the seaweed, Cladoiphon okamuranus, with pressurized hot water in an autoclave. The extraction temperature is set to 100-120 deg.C, the extraction pressure is set to 1.0-2.0 atmospheric pressure and the extraction is continued for 0.2-16 hours.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a method for extracting fucoidan from Okinawa mozuku using hot pressurized water. More specifically, the present invention relates to a method for extracting fucoidan using hot pressurized water, which can efficiently obtain fucoidan having an average molecular weight within a desired range without causing problems such as corrosion in manufacturing equipment.

[0002]

2. Description of the Related Art Conventionally, fucoidan contained in Okinawa mozuku has an excellent anticholesterol effect, blood clarification effect,
Since it has pharmacological effects such as an anticoagulant effect, an anticancer effect, an anti-AIDS virus effect, and an antigastric ulcer effect, it has been desired to extract it efficiently.

[0003] Therefore, Japanese Patent Application Laid-Open No. 10-70970 discloses that from Mozuku, hot water of 60 to 100 ° C is used and the weight molecular weight is 50,000 to 50 for 30 minutes to 3 hours.
000, neutral sugar content of 50-90%,
A method is disclosed for extracting a hot water extract having a sulfur content in the range of 3-17%, such as a hot water extract containing fucoidan.

[0004] Further, Japanese Patent Application Laid-Open No. 10-165114, and published publication, Applied Glycoscience, Vol. 43, No. 2, p.
143-148, (1996) (published on June 30, 1996) using an inorganic acid (concentration: 0.2 N) such as hydrochloric acid or sulfuric acid as an extractant from cultured Okinawa mozuku, at room temperature for 24 hours. A method of extracting fucoidan over a period of time is disclosed.

Further, Japanese Patent Application Laid-Open Nos. 61-57519 and 61-5752019 disclose that a highly viscous fucoidan-containing solution extracted from seaweed using water, warm water or hydrochloric acid is used as a solution. -1,3-glucanase or protease is dissolved to decompose the high-viscosity-imparting substance contained in the fucoidan-containing solution to produce a low-viscosity fucoidan-containing solution, or fucoidan is further purified using an ultrafiltration membrane. A method of making is disclosed.

[0006]

However, according to the production method disclosed in JP-A-10-70970, the yield of fucoidan is as low as less than 1% based on the raw material used, and
In addition, there was a problem that the content of fucose (uronic acid) contained in fucoidan was small.

Further, in the production method disclosed in Japanese Patent Application Laid-Open No. H10-165114, etc., since a highly corrosive strong acid is used as an extractant, there is a problem that the production equipment is easily corroded. Of course, by using an inorganic material having high corrosion resistance, corrosion of manufacturing equipment can be prevented to some extent, but an inorganic material having high corrosion resistance is extremely expensive or poor in workability. And so on, which was economically disadvantageous. Further, fucoidan obtained by the production method disclosed in the same publication and the like has a molecular weight that is too high, and a desired molecular weight, for example, 10,000 to 500,0.
It was not easy to set the value within the range of 00. In addition,
For example, to typically show anti-AIDS virus activity, the average molecular weight of fucoidan is 100,000-200,0
It is known that a value within the range of 00 is preferable, and similarly, it is preferable to set the average molecular weight of fucoidan to a value of about 200,000 in order to typically exhibit an anti-gastric ulcer effect. Are known. Furthermore, when a strong acid is used as an extractant, it is necessary to finally neutralize the obtained fucoidan with a strong base, which causes a problem that the number of production steps increases and the amount of impurities contained increases. Was.

In the production methods disclosed in JP-A-61-575519 and JP-A-61-5752019, when hydrochloric acid, which is a strong acid, is used as an extractant, JP-A-10-165114 is used. In the case where water or warm water (40 ° C., 14 hours) is used as an extractant, there are problems such as corrosiveness and molecular weight similar to those described in
There was a problem that the extraction efficiency was extremely low as in the case of Japanese Patent Application Publication No. 0-70970.

Therefore, the inventors of the present invention diligently studied the above problem, and found that the production equipment was corroded by using pressurized hot water as an extractant in an autoclave and limiting the extraction time to a certain range. The present invention has been found that a high extraction rate can be obtained without excessively decomposing fucoidan or excessively decomposing fucoidan. That is, the present invention has no problems such as corrosion in the manufacturing equipment,
An object of the present invention is to provide a method for extracting fucoidan from which fucoidan having an average molecular weight within a desired range can be efficiently obtained.

[0010]

SUMMARY OF THE INVENTION The present invention relates to a method for extracting fucoidan from Okinawa mozuku using an autoclave with hot pressurized water.
C. (excluding 100 ° C.), and the extraction pressure is a value within a range of 1.0 to 2.0 atm.
In addition, the extraction time is set to a value within a range of 0.2 to 16 hours. By using pressurized hot water in the autoclave in this manner, there is no problem of corrosiveness to the production equipment or the molecular weight of fucoidan, and further, there is no need to neutralize it. In addition, since the extraction temperature and the extraction time in the extraction step are limited to predetermined ranges, excellent extraction efficiency can be obtained, and production control is also improved.

In carrying out the extraction method of the present invention, the amount of hot pressurized water added to the autoclave per 100 g of Okinawa mozuku is preferably in the range of 50 to 500 g. By thus limiting the amount of pressurized hot water used, excellent extraction efficiency of fucoidan can be obtained, and the amount of impurities contained can be reduced.

Further, in carrying out the extraction method of the present invention, it is preferable that the length of the okinawa mozuku be a value within the range of 0.1 to 50 mm. By limiting the length of the Okinawa mozuku in this way, the contact area between fucoidan and hot pressurized water is significantly increased, and excellent extraction efficiency of fucoidan can be obtained.

In carrying out the extraction method of the present invention, it is preferable that the Okinawa mozuku has been treated with an organic acid salt. By pretreating the Okinawa mozuku in this way, the Okinawa mozuku can be swollen,
Excellent extraction efficiency is obtained for fucoidan.

In carrying out the extraction method of the present invention, the organic acid salt is citric acid, acetic acid, propionic acid, butyric acid, valeric acid, stearic acid, malonic acid, succinic acid, glutaric acid, adipic acid, maleic acid It is preferably a salt of at least one organic acid selected from the group consisting of fumaric acid, phthalic acid, glycolic acid, and benzoic acid. By using such kind of organic acid salt, excellent extraction efficiency can be obtained, and there is no problem of corrosiveness to production equipment and molecular weight of fucoidan.

Further, in carrying out the extraction method of the present invention, the hot pressurized water contains an organic acid and / or an inorganic acid or an acid compound of either one, and the pH of the hot pressurized water is 2 to 2.
It is preferably set to a value within the range of 6. By including the acid in this way, the extraction efficiency of fucoidan can be improved. At the same time, since the pH of the pressurized hot water is limited to a value within a predetermined range, there is no problem of corrosiveness to manufacturing equipment and molecular weight of fucoidan.

In carrying out the extraction method of the present invention, the average molecular weight of fucoidan is adjusted to 10,000 to 50.
Preferably, the value is in the range of 000. By limiting the average molecular weight of fucoidan in this way, for example, excellent anti-AIDS virus action and anti-gastric ulcer action can be exhibited.

[0017]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be specifically described below. It should be noted that the following description is merely an outline to the extent that the extraction method of the present invention can be understood. Therefore, the present invention is not limited only to the following description.

[First Embodiment] The first embodiment is a method for extracting fucoidan which sequentially includes the following steps (1) to (3). (1) Pretreatment process of Okinawa mozuku (2) Extraction process of fucoidan (3) Post-treatment process of fucoidan

(1) Step of Pretreatment of Okinawa Mozuku In extracting fucoidan from Okinawa mozuku,
In order to improve the extraction efficiency and reduce the amount of impurities, it is preferable to perform pretreatment (thawing, desalting, and crushing).

Thawing and desalting okinawa mozuku (cultured and natural okinawa mozuku)
After harvesting, it is often salted or refrigerated in order to improve the storage stability. Therefore, it is generally preferable to desalt or thaw in the pretreatment step. Specifically, after flushing the surface water with tap water, for example, 10
It is preferable to immerse the okinawa mozuku in a 00 liter container at a rate of 250 kg while flowing water for 0.5 to 5 hours.

Crushing In order to increase the extraction efficiency, it is preferable to crush Okinawa mozuku into small pieces. The size of the small piece is not particularly limited, but specifically, it is preferable to set the length (long side) to a value in the range of 0.1 to 50 mm using a cutter mixer or the like, The value is more preferably in the range of 0.5 to 30 mm, and even more preferably in the range of 1 to 20 mm.

Swelling treatment Before the extraction step, it is preferable to carry out an organic acid salt treatment for swelling the Okinawa mozuku in order to obtain excellent extraction efficiency. Preferred organic acid salts include citric acid, acetic acid,
Propionic acid, butyric acid, valeric acid, stearic acid, malonic acid, succinic acid, glutaric acid, adipic acid, maleic acid,
Examples thereof include a sodium salt, a potassium salt, and a calcium salt of at least one organic acid selected from the group consisting of fumaric acid, phthalic acid, glycolic acid, and benzoic acid. In particular, sodium citrate is preferable because it has an excellent swelling effect on Okinawa mozuku and excellent extraction efficiency can be obtained.

The conditions of the organic acid salt treatment are not particularly limited. For example, the treatment temperature is 25 to 90 ° C., the amount of the organic acid salt treatment is 0.1 to 20 parts by weight (Okinawa mozuku 10
The processing time is preferably in the range of 0.5 to 24, the processing temperature is 40 to 70 ° C., the organic acid salt processing amount is 1 to 15 parts by weight (per 100 parts by weight of Okinawa mozuku), More preferably, the treatment time is set to a value within the range of 1 to 12.

(2) Step of extracting fucoidan As conditions for determining the extraction efficiency and molecular weight of fucoidan,
The extraction conditions (extraction temperature, extraction pressure, extraction time, extraction pH value, stirring conditions, amount of pressurized hot water used) in the first embodiment will be described.

Extraction Temperature In carrying out the extraction method of the first embodiment,
It is preferable to set the extraction temperature to a value within the range of 100 to 130 ° C. The reason for this is that if the extraction temperature is lower than 100 ° C., the extraction efficiency may be significantly reduced,
On the other hand, if the extraction temperature exceeds 130 ° C., production control may be difficult, or fucoidan may be excessively decomposed. Therefore, since the balance between the extraction efficiency and the production control becomes better, the extraction temperature is set to 100 to
It is preferable that the value be in the range of 130 ° C.
More preferably, the value is in the range of 120 ° C.

Extraction time In carrying out the extraction method of the first embodiment,
It is preferable that the extraction time of the extraction step be a value within the range of 0.2 to 16 hours. The reason for this is that if the extraction time is less than 0.2 hours, the extraction efficiency may be significantly reduced. On the other hand, if the extraction time exceeds 16 hours, it becomes difficult to adjust the molecular weight, or economical. This is because it may be disadvantageous to Therefore, since the balance between the extraction efficiency and the molecular weight becomes better, the extraction time is reduced to 0.1.
Preferably, the value is in the range of 3 to 10 hours.
More preferably, the value is in the range of 5 to 3 hours.

Extraction pressure In carrying out the extraction method of the first embodiment,
The extraction pressure is preferably set to a value within the range of 1 to 2 atm. The reason for this is that if the extraction pressure is less than 2 atm, the extraction efficiency is significantly reduced.
If the pressure exceeds the atmospheric pressure, it becomes difficult to adjust the molecular weight, or the size of the extraction device (autoclave) becomes excessively large, which is economically disadvantageous. Therefore, the extraction pressure is preferably set to a value within the range of 1.1 to 2 atm, since the balance between the extraction efficiency and the molecular weight property becomes better.
More preferably, the value is in the range of 1.1 to 1.2 atm.

Extraction pH value In carrying out the extraction method of the first embodiment,
It is preferable that the pH value at the time of extraction be a value within the range of 2 to 8. The reason for this is that if the pH value is less than 2, the corrosiveness to the production equipment may be significantly increased,
On the other hand, if the pH value exceeds 8, the extraction efficiency may be significantly reduced. Therefore, since the balance between the corrosiveness to the production equipment and the extraction efficiency is better, the pH value at the time of extraction is preferably set to a value within the range of 3.5 to 8, preferably 4 to 7.0. More preferably, the value is within the range.

Stirring Conditions In carrying out the extraction method of the first embodiment,
It is preferable to stir in the extraction container. Specifically, it is preferable to stir using a stirring blade at a rotation speed of 5 to 200 rpm, more preferably stirring at a rotation speed of 10 to 100 rpm, and more preferably stirring at a rotation speed of 20 to 80 rpm. preferable. The reason for this is that if the rotation speed of the stirring blade is less than 5 rpm, the extraction efficiency may be significantly reduced. On the other hand, if the rotation speed of the stirring blade exceeds 200 rpm, air bubbles are easily entrained,
Conversely, the extraction efficiency may be reduced, or the production facilities may be large.

The amount of hot pressurized water used In the extraction method of the first embodiment,
The amount of hot pressurized water added to the autoclave per 100 g of Okinawa mozuku is preferably in the range of 50 to 500 g. The reason is that the amount of pressurized hot water used is 50
When the amount is less than 500 g, the extraction efficiency per unit time may be significantly reduced. On the other hand, when the amount of pressurized hot water exceeds 500 g, the amount of impurities increases or the extraction efficiency of fucoidan decreases. This is because there are cases where Therefore, since the balance between the extraction efficiency and the amount of impurities contained becomes better, the amount of the organic acid used is preferably set to a value within the range of 10 to 50 g per 100 g of Okinawa mozuku. More preferably, the value is in the range of 20 g.

(3) Post-processing step of fucoidan In the first embodiment, in order to finally obtain fucoidan (fucoidan powder), the extract obtained in the extraction step is subjected to post-processing (centrifugation, desalting, etc.). , Concentration and powderization).

Centrifugation After the obtained extract is stored in a filter cloth of a centrifuge,
By performing centrifugation, solid-liquid separation can be performed. That is, by performing the centrifugation treatment, it is possible to efficiently separate a solid content such as impurities from a solution containing a large amount of fucoidan. Here, the centrifugation treatment conditions are not particularly limited. For example, after confirming that the extract obtained in the extraction step has reached a temperature of 40 ° C. or less,
3,000-100,000 rpm, 1-3
Preferably, the time is 0 minutes.

Desalting The liquid obtained by centrifugation is preferably subjected to ultrafiltration using an ultrafiltration apparatus, for example, under the condition of a molecular weight cut off of 6,000 or less. By performing the ultrafiltration treatment in this manner, a solution containing a large amount of fucoidan having a narrow molecular weight distribution can be obtained as an ultrafiltration concentrate, and as a result, fucoidan having a salt content and a molecular weight within a predetermined range can be efficiently produced. Obtainable. In addition, the salt concentration in the filtrate (ultrafiltration concentrate) measured by the salt meter is
It is preferable to repeatedly perform an ultrafiltration treatment comprising ultrafiltration concentration and pressurization of filtered water until the value becomes 0.1% by weight or less.

Concentration It is preferable that the concentration of fucoidan in the obtained ultrafiltration concentrate is, for example, at least twice as high as that obtained by a vacuum concentration method or an alcohol precipitation method. By concentrating in this manner, pulverization in a subsequent step becomes easy, and fucoidan powder having a narrow particle size distribution can be obtained.

Powderization For example, using a spray drying device or a freeze drying device,
Fucoidan powder having a narrow particle size distribution can be efficiently obtained. When a spray-drying device is used, a fusing agent such as dextrin is added to a fucoidan concentrated solution obtained by a reduced-pressure concentrating device in an amount of 50 to 500 parts by weight per 100 parts by weight of fucoidan so that powdering is easy. It is preferable to add within the range.

[Second Embodiment] The second embodiment is also a method for extracting fucoidan that sequentially includes the above steps (1) to (3), as in the first embodiment. However, (2)
In the step of extracting fucoidan, an organic acid is used as an extractant. Therefore, such an extractant will be mainly described below.

First, the organic acids used in the second embodiment include citric acid, acetic acid, propionic acid, butyric acid, valeric acid, stearic acid, malonic acid, succinic acid, glutaric acid,
Examples include at least one selected from the group consisting of adipic acid, maleic acid, fumaric acid, phthalic acid, glycolic acid, and benzoic acid. In addition, citric acid is more preferably used because the pH value is easily adjusted and a high extraction efficiency is obtained. Furthermore, even when citric acid and another organic acid are used in combination, the amount of citric acid used should be 50% by weight or more when the amount of organic acid used is 100% by weight. Is more preferable, and more preferably 70% by weight or more.
More preferably, the value is 0% by weight or more. In addition,
The amount of organic acid used per 1000 g of Okinawa mozuku
The value is preferably in the range of 1 to 30 g. The reason for this is that if the amount of the organic acid used is less than 1 g, the extraction efficiency per unit time may be significantly reduced, while if the amount of the organic acid used exceeds 30 g, the amount of impurities increases. Or the extraction efficiency of fucoidan may decrease. Therefore, since the balance between the extraction efficiency and the amount of impurities contained becomes better,
The amount of organic acid used per 1000 g of Okinawa mozuku
The value is preferably in the range of 2 to 25 g, and
More preferably, the value is in the range of 0 g.

[Third Embodiment] In the third embodiment, as in the first and second embodiments, the above (1) to (3)
This is a method for extracting fucoidan, which comprises the steps of: However, (2) in the step of extracting fucoidan, a mixture of an organic acid and an inorganic acid is used as an extractant. Therefore, such an extractant will be mainly described below.

First, as the organic acid used in the third embodiment, the same organic acid as described in the second embodiment is used.
Similar amounts can be used. Therefore, description of the organic acid used in the third embodiment is omitted here.

On the other hand, examples of the inorganic acid used in the third embodiment include at least one selected from the group consisting of formic acid, hydrochloric acid, sulfuric acid, and nitric acid. However, in order to effectively prevent corrosion of the production equipment, it is preferable that the pH at the time of extraction is set to a value within the range of 3 to 6, even when an inorganic acid is added. Therefore, the total amount of extractant is 1
When the content is 00% by weight, the amount of the inorganic acid less than 0.05N is preferably set to a value of less than 50% by weight, more preferably a value within a range of 0.1 to 30.0% by weight. And more preferably 1.0 to 10.0
Weight%.

As a modification of the second embodiment, it is preferable to use an organic acid and an inorganic acid separately. However, also in this case, in order to effectively prevent corrosion of the manufacturing equipment, it is preferable that the amount of the inorganic acid having the above-described concentration be within the range of use.

[0042]

[Example 1] (Production of fucoidan) 250 kg of salted okinawa mozuku (mozuku production area: Nakijin) was washed three times with running water,
After removing the salt on the surface, it was housed in a 1000 liter container, and immersed in tap water for 1 hour while flowing water. Next, take out the Okinawa mozuku from the container and use a cutter mixer to lengthen the Okinawa mozuku (long side).
Was about 2 mm. Fucoidan was extracted from the fragmented Okinawa mozuku under the following extraction conditions, and finally 5 kg of fucoidan powder (powder) was produced under the following post-treatment conditions.

Extraction container: stainless steel 304 autoclave / capacity 1000 liter Extractant: pressurized hot water Water consumption: 200 g / Okinawa mozuku 100 g Extraction temperature: 120 ° C. Extraction pH: 7.0 Extraction time: 0.5 hour Centrifugation Separation: 100,000 rpm for 60 min. Ultrafiltration treatment: Removal of molecular weight cut off of 6000 or less / Treatment time: 60 min Concentration treatment: Concentration of fucoidan concentration to about 2 times Powdering: Spray dry method (Shaping agent: Dextrin weight) 1: 1 ratio) / Average particle size (100 mesh or less)

(Evaluation of fucoidan) (1) Component evaluation The content of fucoidan in the obtained fucoidan powder was measured by an anthrone sulfate method, and it was found to be 52.5% by weight.
Met. In addition, when the amount of sulfated-fucose-containing polysaccharide in fucoidan was measured by the carbazole method, 16.
It was 9% by weight. When the amount of sulfuric acid in fucoidan was measured by ion chromatography, it was 15.0.
% By weight. Furthermore, by 550 degreeC heating incineration method,
The ash content in fucoidan was measured to be 22% by weight or less, and the water content in fucoidan was measured by a 105 ° C. heat drying method to be 6% by weight or less.

(2) Yield The yield of fucose in the obtained fucoidan powder was calculated on the basis of the used amount of the raw material Okinawa mozuku, and a value of 23% was obtained.

(3) Average molecular weight The average molecular weight (average weight molecular weight) of the obtained fucoidan powder was measured by gel filtration method.
000. Accordingly, it was confirmed that the average molecular weight was within the range of the preferable average molecular weight of the present invention.

(4) Number of bacteria The number of general bacteria in the obtained fucoidan powder was measured by a standard agar medium method.
It was confirmed that the number was less than 300. In addition, when the coliform group in the obtained fucoidan powder was measured by the BGLB method, it was confirmed to be negative.

(5) Anticancer activity To human promyelocytic leukemia cells (50,000 cells) cultured on a petri dish by a standard agar medium method, the obtained fucoidan powder was added at a concentration of 1 μg / ml. The culture was continued. As a result, after 18 hours of culture, the number of cells was about 3
When the number of cells decreased to 10,000 cells and the culture was continued, the number of cells decreased to 0 (disappeared) at a culture time of 40 hours. on the other hand,
In the control without the addition of fucoidan powder, the number of cells increased to about 60,000 at a culturing time of 18 hours, and further culturing was continued.
The number of cells increased to about 150,000. Therefore, it was confirmed that the obtained fucoidan powder had an excellent anticancer effect on human promyelocytic leukemia cells.

(6) Apoptosis-inducing action To human promyelocytic leukemia cells (50,000 cells) cultured on a petri dish by the standard agar medium method, the obtained fucoidan powder was added at a concentration of 1 μg / ml, and The culture was continued and apoptosis (percentage of dead cells) was measured. As a result, at the start of culture, apoptosis was about 20%, but at 22 hours of culture, apoptosis increased to about 70%, and at 48 hours of culture, apoptosis further increased to about 90%. At 70 hours, apoptosis further increased to about 100% and all cells became dead. On the other hand, in the control without addition of fucoidan powder, the culture time was 22 hours,
At 8 hours and 70 hours, apoptosis was about 20%, respectively, with no change in apoptosis. Therefore, it was confirmed that the obtained fucoidan powder had an excellent apoptosis-inducing effect on human promyelocytic leukemia cells.

(7) Corrosion Small pieces (length 10) of stainless steel 304 constituting the extraction container
cm, width 2.54 cm, thickness 0.1 mm) to 100 m
l of the extractant and kept at a temperature of 120 ° C.
No corrosion was observed after 1000 hours or 2000 hours.

Example 2 (Production of fucoidan) Extraction temperature was from 120 ° C. to 115 ° C.
The fucoidan powder was produced in the same manner as in Example 1 except that the powder was lowered.

(Evaluation of fucoidan) As in Example 1,
For the obtained fucoidan powder, (1) component evaluation, (2) yield, (3) average molecular weight, (4) bacterial count,
(5) anticancer action, (6) apoptosis inducing action, (7)
When the corrosiveness was evaluated, the same result as in Example 1 was obtained in Example 2.

Example 3 (Production of fucoidan) Instead of using only pressurized hot water as the extractant, pressurized hot water to which citric acid (citric acid concentration: 0.1% by weight) was added was used. Otherwise, a fucoidan powder was produced in the same manner as in Example 1.

(Evaluation of fucoidan) As in Example 1,
For the obtained fucoidan powder, (1) component evaluation, (2) yield, (3) average molecular weight, (4) bacterial count,
(5) anticancer action, (6) apoptosis inducing action, (7)
When the corrosivity was evaluated, in Example 3,
The yield was improved, and the same results as in Example 1 were obtained for other evaluation items.

[Examples 4 and 5] (Production of fucoidan) Raw Okinawa mozuku (Example 4) and salted product (Example 5) from Chinen were used instead of salted products from Nakijin as Okinawa mozuku. Otherwise, a fucoidan powder was produced in the same manner as in Example 1.

(Evaluation of fucoidan) As in Example 1,
For the obtained fucoidan powder, (1) component evaluation, (2) yield, (3) average molecular weight, (4) bacterial count,
(5) anticancer action, (6) apoptosis inducing action, (7)
When the corrosiveness was evaluated, the same results as in Example 1 were obtained in Examples 4 and 5.

[Comparative Example 1] (Production of fucoidan) Hydrochloric acid was used as an extractant, the concentration of hydrochloric acid was 0.2 N, and the extraction temperature was from 120 ° C to 25 ° C.
The fucoidan powder was produced in the same manner as in Example 1 except that the extraction time was changed from 0.5 hours to 16 hours.

(Evaluation of fucoidan) As in Example 1,
The obtained fucoidan powder was evaluated for (1) component evaluation, (3) average molecular weight, and (7) corrosivity. As a result, the corrosiveness of the stainless steel 304 due to the extractant was confirmed, and the average molecular weight of the obtained fucoidan powder was 70,000. For component evaluation,
It was equivalent to Example 1.

Comparative Example 2 (Production of fucoidan) A fucoidan powder was produced in the same manner as in Comparative Example 1, except that the extraction temperature in Comparative Example 1 was changed from 25 ° C. to 95 ° C.

(Evaluation of fucoidan) As in Example 1,
The obtained fucoidan powder was evaluated for (1) component evaluation, (3) average molecular weight, and (7) corrosivity. As a result, further corrosiveness due to the extractant was confirmed, and the average molecular weight of the obtained fucoidan powder was 50,
000 or less. In addition, about component evaluation, it was equivalent to Example 1.

[0061]

As described above in detail, according to the method for extracting fucoidan of the present invention, there is no problem such as corrosion in the manufacturing equipment (for example, corrosion does not occur for 1000 hours or more), and the desired method can be obtained. Average molecular weight (for example, 1
Fucoidan (fucoidan powder) having a value within a range of from 0.000 to 500,000) can be obtained efficiently. Further, according to the method for extracting fucoidan of the present invention, by using only pressurized hot water as an extractant, the amount of impurities in fucoidan can be reduced,
In addition, fucoidan was extracted with high efficiency, and the bactericidal effect of fucoidan was also obtained. Further, according to a preferred embodiment of the method for extracting fucoidan of the present invention, by using an organic acid or an organic acid and an inorganic acid as an extractant, there is no problem such as corrosion in production equipment, and a higher extraction efficiency. Can be obtained.

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) A61P 31/18 A61K 31/00 631M 35/00 635 A61K 31/715 31/715

Claims (7)

[Claims] 1. A method for extracting fucoidan from Okinawa mozuku with hot pressurized water using an autoclave, wherein the extraction temperature is set to a value within a range of more than 100 to 120 ° C.,
A method for extracting fucoidan, wherein the extraction pressure is set to a value within a range of 1.0 to 2.0 atmospheres and the extraction time is set to a value within a range of 0.2 to 16 hours. 2. The amount of pressurized hot water added to the autoclave is 50 to 500 g per 100 g of the Okinawa mozuku.
The method for extracting fucoidan according to claim 1, wherein the value is within the range of fucoidan. 3. The length of the Okinawa mozuku is 0.1 to 5
3. The method for extracting fucoidan according to claim 1, wherein the value is within a range of 0 mm. 4. The method for extracting fucoidan according to any one of claims 1 to 3, wherein the Okinawa mozuku is treated with an organic acid salt. 5. The organic acid salt is citric acid, acetic acid, propionic acid, butyric acid, valeric acid, stearic acid, malonic acid, succinic acid, glutaric acid, adipic acid, maleic acid, fumaric acid, phthalic acid, glycolic acid. The method for extracting fucoidan according to any one of claims 1 to 4, wherein the salt is a salt of at least one organic acid selected from the group consisting of benzoic acid. 6. The pressurized hot water contains an organic acid and / or an inorganic acid, and the pH of the pressurized hot water is set to a value within a range of 2 to 6. The method for extracting fucoidan according to any one of claims 1 to 5. 7. The fucoidan having an average molecular weight of 10,
The method for extracting fucoidan according to any one of claims 1 to 6, wherein the value is within a range of 000 to 500,000.