JP2008266528A - Method for producing fucoidan - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a fucoidan by which the extraction efficiency of the fucoidan from seaweeds such as a sea tangle, Nemacystus decipiens and Sargassum horneri is raised and to further provide a method for producing the fucoidan by which there is no problem such as corrosion of production equipment or an increase in the number of production steps and production cost can be reduced because an acid, a salt etc. , are not used as an extractant. <P>SOLUTION: The method for producing the fucoidan comprises a step of pulverizing the dried seaweed and affording powder of the seaweed, a step of adding 5-100 pts.wt. of water to 100 pts.wt. of the powder of the seaweed and preparing a composition comprising the powder of the seaweed and water, a step of kneading the resultant composition using an extruder in which the maximum temperature in the cylinder is 60-180°C and a step of extracting the fucoidan. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention is a technique for increasing the extraction efficiency of fucoidan from seaweeds such as kombu, mozuku and akamoku.

  Seaweeds such as kombu, mozuku, and akamoku contain fucoidan. Fucoidan is a sulfated polysaccharide comprising L-fucose as a constituent sugar, has various physiological functions, and is used as a food or cosmetic material. Therefore, it has been desired to efficiently extract fucoidan from seaweed.

  For example, Japanese Patent Application Laid-Open No. 10-165114 (Patent Document 1) discloses a technique for collecting contents such as fucoidan from seaweed by an extraction operation or the like. However, since this method requires complicated equipment and time, the obtained fucoidan is expensive.

  JP-A-61-57519 (Patent Document 2) and JP-A-61-5752019 (Patent Document 3) disclose methods for increasing the extraction efficiency of fucoidan using an enzyme. The yield of fucoidan is low.

  JP-A-2006-160862 (Patent Document 4) discloses freeze-drying seaweed buds and performing a process extraction time in hot water extraction or acid extraction within a range of 0.5 to 72 hours. A method for extracting colorless and odorless high-purity fucoidan with a value within the range of 3 is disclosed.

  Japanese Patent Application Laid-Open No. 10-70970 (Patent Document 5) discloses that a mozuku is pulverized with a blender together with water and this solution is treated at 60 to 100 ° C. for 30 to 3 hours to obtain a weight average molecular weight of 50,000 to 500,000. And a method for extracting a hot water extract having a neutral sugar content of 50 to 90% and a sulfur content of 3 to 17% is disclosed.

  However, these extraction methods have drawbacks that the extraction process is complicated, resulting in high production costs and low extraction efficiency. In addition, since acids, salts, and the like are used as the extractant, there is a problem that the production cost increases due to corrosion of the manufacturing equipment.

  Japanese Patent Laid-Open No. 2000-239302 (Patent Document 6) discloses a fucoidan in which fucoidan is extracted from Okinawa mozuku and an organic acid is used as an extractant, and the pH of the extraction step is in the range of 2-6. The extraction method of is disclosed.

  However, this extraction method also has a problem that the production cost is increased because the production equipment is corroded because acid, salt, and the like are used as the extractant. Furthermore, when a strong acid is used as an extractant, it is necessary to finally neutralize with a strong base, which increases the number of manufacturing steps and increases the amount of impurities contained.

  Furthermore, Japanese Unexamined Patent Application Publication No. 2005-145989 (Patent Document 7) discloses the following fucoidan extraction method.

  Powdered mozuku that has been pulverized and processed into a powdery form is kneaded with 25 times its weight of water, and then mixed with an appropriate amount of water (alcohol-diluted if necessary) in an agitated hot water extractor or high-pressure extraction kettle. After adding, boil at 80 to 90 ° C. for 60 to 120 minutes with stirring, transfer to an alcohol extraction tank to remove the alcohol, and separate and purify the filtered and extracted stock solution with an ultra-high speed centrifuge, then a concentrator Concentrate 4-8 times.

However, even with this method, the fucoidan extraction efficiency is insufficient, and further improvements are required.
JP 10-165114 A JP-A 61-57519 JP-A 61-5752019 JP 2006-160862 A JP-A-10-70970 JP 2000-239302 A JP 2005-145989 A

  The present invention has been made by paying attention to the above points, and an object of the present invention is to provide a method for producing fucoidan that enhances the extraction efficiency of fucoidan from seaweeds such as kombu, mozuku, and akamoku.

  Another object of the present invention is to provide a method for producing fucoidan that does not use acid, salt, or the like as an extractant, so that there is no problem of corrosion of production equipment and the problem of an increase in the number of production steps, and the production cost can be further reduced. There is to do.

In order to achieve the above object, the present invention provides, for example, the following means:
Item 1. Crushing dried seaweed to obtain seaweed powder,
Adding 5 to 100 parts by weight of water to 100 parts by weight of seaweed powder, and preparing a composition containing seaweed powder and water;
A method for producing fucoidan, comprising: a step of kneading the composition using an extruder having a maximum temperature in a cylinder of 60 ° C to 180 ° C; and a step of extracting fucoidan from the kneaded product.

  Item 2. Item 2. The method according to Item 1, wherein the maximum temperature in the cylinder during the extruder treatment is 80 ° C to 150 ° C.

  Item 3. Item 3. The method according to Item 1 or 2, wherein the water weight is 10 to 50 parts by weight with respect to 100 parts by weight of seaweed powder.

  Item 4. 4. The method according to any one of items 1 to 3, comprising a step of performing an enzyme treatment on the kneaded product after the step of kneading using the extruder.

  Item 5. The method according to any one of Items 1 to 4, wherein the step of extracting fucoidan includes a hot water extraction step, and the hot water extraction step is performed in a range of 0.5 to 1 hour.

  The dried seaweed is pulverized to obtain seaweed powder, and 5 to 100 parts by weight of water is added to 100 parts by weight of seaweed powder to prepare a composition containing seaweed powder and water. By kneading using an extruder at 60 ° C. to 180 ° C., the seaweed tissue can be effectively destroyed, and fucoidan can be extracted from the kneaded product with high extraction efficiency.

  Such an extraction method does not use acid, salt, etc. as an extraction agent, unlike the conventional extraction method, and therefore there is no problem of corrosion of manufacturing equipment or an increase in the number of manufacturing processes, and further, the production cost. Can be reduced.

  Hereinafter, the present invention will be described in detail.

  As the form of the raw material used in the present invention, seaweed powder obtained by washing seaweeds such as kombu, mozuku, and akamoku with cold water, freeze-drying or hot-air drying, and grinding the dried seaweed is used.

  As the pulverizer, for example, a known pulverizer such as a fine powder pulverizer (blade mill) can be used.

  The degree of drying of the seaweed is not limited as long as it can be powdered, but is preferably about 1 / twentieth to one thirtieth of the weight of raw seaweed, more preferably one half of 25 (water content 5 to 7%). It was dried and shrunk. The size of the seaweed powder is preferably about 30 to 80 μm.

  When the size of the seaweed powder is less than 30 μm, there is a drawback that dispersibility becomes difficult and workability is deteriorated. When the size of the seaweed powder is larger than 80 μm, the extraction efficiency of fucoidan may be lowered.

  Next, 5 to 100 parts by weight of water is added to 100 parts by weight of seaweed powder to prepare a composition containing seaweed powder and water.

  The amount of water added is preferably 10 to 50 parts by weight of water with respect to 100 parts by weight of seaweed powder, and more preferably 20 to 40 parts by weight of water with respect to 100 parts by weight of seaweed powder.

  When the amount of water added to 100 parts by weight of seaweed powder is less than 5 parts by weight, the kneading process with an extruder tends to be insufficient, and when it exceeds 100 parts by weight, the viscosity of the composition is too low. The kneading process in the ruder tends to be insufficient.

  Next, the composition is kneaded using an extruder having a maximum temperature in the cylinder of 60 ° C to 180 ° C.

  The maximum temperature in the cylinder during the extruder treatment is preferably 80 ° C to 150 ° C, more preferably 90 ° C to 120 ° C.

  Thus, by performing the extruder process before the extraction process, the seaweed tissue can be effectively destroyed.

  When the maximum temperature during the extruder treatment is less than 60 ° C, the destruction of the seaweed tissue is insufficient, and when it exceeds 180 ° C, the composition may be degraded.

Here, as the extruder, a short-shaft extruder can be used. In this specification, the extruder process is usually performed under the following conditions.
(1) Raw material supply rate 20 (kg / h)
(2) Screw rotation speed 300 (rpm)
(3) Addition water 3.0 (l / h)
(4) Material temperature 98 (° C)
(5) Pressure 10 (kgf / cm ² )
(6) Temperature: first chamber 60 ° C, second chamber 100 ° C, third chamber 120 ° C
Next, the kneaded product after the extruder treatment is subjected to an enzyme treatment.

  In the enzyme treatment, about 20 to 40 times, particularly 30 times, distilled water is added to the weight of the kneaded product, and the enzyme reaction conditions are 120 minutes, a temperature of 45 to 50 ° C., and a pH of 6.5 to 7.0. Is preferred.

  A conventionally well-known enzyme can be used, for example, at least one of a fibrinolytic enzyme and a fucose sulfate free enzyme can be used.

  Among these, it is preferable to use a fibrinolytic enzyme because the range of pH value is wider and high extraction efficiency is obtained, and cellulase, hemicellulase, or alginic acid lyase is more preferable.

  The amount of enzyme used is preferably, for example, a value within the range of 0.1 to 20 g per 1000 g of Okinawa mozuku. The reason for this is that when the amount of enzyme used is less than 0.1 g, the extraction efficiency per unit time may be significantly reduced, and when the amount of enzyme used exceeds 20 g, the amount of impurities increases or fucoidan is obtained. It may be difficult to adjust the average molecular weight.

  Next, fucoidan is extracted with hot water from the kneaded product after the enzyme treatment. In the hot water extraction step, it is preferable to perform hot water extraction at 60 ° C. to 100 ° C. for 30 to 60 minutes. More preferably, hot water extraction at 90 ° C. to 100 ° C. is performed for 30 to 60 minutes.

  If the extraction temperature is less than 60 ° C, the extraction efficiency may be significantly reduced. If the extraction temperature exceeds 100 ° C, production management may be difficult, or fucoidan may be excessively decomposed.

  The pH value at the time of extraction is preferably set to a value within the range of 3-6.

  If the pH value is less than 3, the enzyme may be activated or deteriorated, and the corrosiveness to the production equipment may be increased. If the pH value exceeds 6, the extraction efficiency is significantly reduced. Therefore, since the balance between the corrosiveness to the production facility and the extraction efficiency becomes better, the pH value during the extraction is more preferably set to a value within the range of 3.5 to 5.5. More preferably, the value is in the range of -5.0.

  If the extraction time is less than 0.5 hours, the extraction efficiency may be significantly reduced, and if the extraction time exceeds 1 hour, it is economically disadvantageous.

  Next, the extract obtained in the extraction step is cooled to room temperature and suction filtered.

  Concentrate the filtrate to 1/4 volume with an evaporator. Add 4 times the amount of ethanol as the concentrate and let stand.

  Filter by suction filtration. The obtained precipitate becomes a hot water extract.

  Next, a 1% hot water extract aqueous solution is prepared.

Add these amounts of 0.1 M MgCl ₂ and mix. Further, ethanol is added and allowed to stand so that 5% by weight of the total amount is ethanol. Suction filtered and the filtrate is dialyzed.

  After dialysis, powderize using a freeze-drying device or spray-drying device. The obtained powder becomes fucoidan.

  As described above, the present invention improves the extraction efficiency (hot water extraction time 0.5 to 1 hour) by pulverizing freeze-dried or hot-air dried seaweed, followed by an extruder treatment and an enzyme treatment. Features.

  Therefore, according to the present invention, by performing the extruder process before the extraction process, the production facility can be obtained at a high extraction rate without corroding the production facility or excessively decomposing fucoidan.

  The fucoidan of the present invention can be added to foods and drinks, cosmetics, pharmaceuticals, etc., and can utilize the useful action of fucoidan.

  Hereinafter, the present invention will be specifically described by way of examples. The present invention is not limited to the examples.

In addition, the hot water extraction method in the following examples was as follows.
(Hot water extraction process)
The sample is subjected to 90 ° C. hot water extraction for 30-60 minutes.

  Next, the extract obtained in the extraction step is cooled to room temperature and suction filtered. Concentrate the filtrate to 1/4 volume with an evaporator. Add 4 times the amount of ethanol as the concentrate and let stand. Filter by suction filtration. The obtained precipitate becomes a hot water extract.

Next, a 1% hot water extract aqueous solution is prepared. Add these amounts of 0.1 M MgCl ₂ and mix. Further, ethanol is added and allowed to stand so that 5% by weight of the total amount is ethanol. Suction filtered and the filtrate is dialyzed.

After dialysis, powderize using a freeze-drying device or spray-drying device. The obtained powder becomes fucoidan.
(Example 1-1)
600 ml of hot water (90 ° C.) was added to 20 g of dried akamoku, and extraction was performed for 30 to 60 minutes.

In the extraction for 30 minutes, 45 minutes, and 60 minutes, the content of the hot water extract (fucoidan) was measured. The results are shown in Table 1 and FIG.
(Example 1-2)
20 g of dried akamoku was pulverized using a fine powder pulverizer (blade mill) to obtain akamoku powder having a major axis of 40 μm.

The change with time of the hot water extract (fucoidan) was measured in the same manner as in Example 1-1 except that this akamoku powder was used. The results are shown in Table 1 and FIG.
(Example 1-3)
20 g of dried akamoku was pulverized using a fine powder pulverizer (blade mill) to obtain akamoku powder having a major axis of 40 μm.

Next, 3 ml of water was added to 20 g of red powder and heated and kneaded using an extruder under the following processing conditions.
(1) Screw rotation speed 300 (rpm)
(2) Material temperature 98 (° C)
(3) Pressure 10 (kgf / cm ² )
The change with time of the hot water extract (fucoidan) was measured in the same manner as in Example 1-1, except that the obtained red kumoku kneaded material was used. The results are shown in Table 1.
(Example 1-4)
20 g of dried akamoku was pulverized using a fine powder pulverizer (blade mill) to obtain akamoku powder having a major axis of 40 μm.

Next, 3 ml of water was added to 20 g of red powder and heated and kneaded using an extruder under the following processing conditions.
(1) Screw rotation speed 300 (rpm)
(2) Material temperature 98 (° C)
(3) Pressure 10 (kgf / cm ² )
600 ml of water was added to the obtained kneaded product, and this composition was subjected to an enzyme treatment. The enzyme treatment was performed using cellulase as an enzyme at 45 ° C. to 50 ° C. for 2 hours at pH 6.5 to 7.0.

  The change with time of the hot water extract (fucoidan) was measured in the same manner as in Example 1-1 except that the obtained enzyme-treated composition was used. The results are shown in Table 1.

  From the above Examples 1-1 to 1-4, it can be seen that the content of the hot water extract (fucoidan) was increased by subjecting the dried red peach powder to an extruder treatment.

  As shown in Table 4, the content of 4.2% hot water extract (fucoidan) was increased by subjecting the dried red peach powder to an extruder treatment. Moreover, the content of 1.3% hot water extract (fucoidan) was increased by pulverization.

（実施例２−１）
乾燥アカモク２０ｇに６００ｍｌの水を加え、この組成物に酵素処理を行った。酵素処理条件は、酵素としてアルギン酸リアーゼ又はセルラーゼを用い、４５℃〜５０℃、２時間、ｐＨ６．５〜７．０で行った。

(Example 2-1)
600 ml of water was added to 20 g of dried akamoku, and this composition was subjected to enzyme treatment. The enzyme treatment conditions were as follows. Alginate lyase or cellulase was used as the enzyme, and the reaction was performed at 45 ° C. to 50 ° C. for 2 hours at pH 6.5 to 7.0.

  The resulting enzyme-treated composition was measured for viscosity and reducing sugar amount.

  The viscosity measurement results are shown in Table 2, and the reducing sugar content measurement results are shown in Table 3.

In Table 2, “control” refers to a case where no enzyme treatment is performed.
(Example 2-2)
20 g of dried akamoku was pulverized using a fine powder pulverizer (blade mill) to obtain akamoku powder having a major axis of 40 μm.

  The viscosity and amount of reducing sugar of the enzyme-treated composition were measured in the same manner as in Example 2-1, except that this akamoku powder was used.

The viscosity measurement results are shown in Table 2, and the reducing sugar content measurement results are shown in Table 3.
(Example 2-3)
20 g of dried akamoku was pulverized using a fine powder pulverizer (blade mill) to obtain akamoku powder having a major axis of 40 μm.

Next, 3 ml of water was added to 20 g of red powder and heated and kneaded using an extruder under the following processing conditions.
(1) Screw rotation speed 300 (rpm)
(2) Material temperature 98 (° C)
(3) Pressure 10 (kgf / cm ² )
The viscosity and amount of reducing sugar of the enzyme-treated composition were measured in the same manner as in Example 2-1, except that the obtained red kumoku kneaded material was used.

  The viscosity measurement results are shown in Table 2, and the reducing sugar content measurement results are shown in Table 3.

  From the above experimental results, it can be seen that the content of the hot water extract (fucoidan) was increased by subjecting the dried red mock powder to an extruder treatment and further an enzyme treatment.

（実施例３）
以下の実施例で用いたエクストルーダーの処理条件は次のとおりである。
（エクストルーダーの処理条件）
（１）原料供給量 20（ｋｇ／ｈ）
（２）スクリュー回転数300（ｒｐｍ）
（３）添加水3.0（ｌ／ｈ）
（４）材料温度９８（℃）
（５）圧力１０（ｋｇｆ／ｃｍ^２）
（６）エクストルーダー内の温度
第１室 ６０℃、第２室 １００℃、第３室 １２０℃
（実施例３−１）温度条件
アカモク粉末（平均粒径50μｍ）のエクストルーダー処理における温度の検討を行った。

(Example 3)
The processing conditions of the extruder used in the following examples are as follows.
(Extruder processing conditions)
(1) Raw material supply rate 20 (kg / h)
(2) Screw rotation speed 300 (rpm)
(3) Addition water 3.0 (l / h)
(4) Material temperature 98 (° C)
(5) Pressure 10 (kgf / cm ² )
(6) Temperature in the extruder 1st chamber 60 ° C, 2nd chamber 100 ° C, 3rd chamber 120 ° C
(Example 3-1) Temperature conditions The temperature in the extruder treatment of akamoku powder (average particle size 50 μm) was examined.

Extruder treatment of akamoku powder was performed by setting the water weight to 20 weights with respect to 100 weights of raw materials, the extruder pressure to 10 kgf / cm ² , and changing the temperature in the cylinder between 60-150 ° C. The obtained kneaded product was subjected to hot water extraction, and the increase rate of the hot water extract was measured.

The result is shown in FIG.
(Example 3-2) Pressure conditions The pressure in the extruder treatment of red mock powder (average particle size 50 μm) was examined.

The temperature inside the cylinder was set to 100 ° C., the water weight was set to 20 weights with respect to 100 weights of the raw material, and the extruder outlet pressure was changed between 1 to 15 kgf / cm ² to perform the extruder treatment of akamok powder.

  The obtained kneaded product was subjected to hot water extraction, and the increase rate of the hot water extract was measured.

The result is shown in FIG.
(Example 3-3) Water content condition The water content in the extruder process of the red powder (average particle diameter of 50 μm) was examined.

The temperature in the cylinder was set to 100 ° C., the pressure of the extruder was set to 10 kgf / cm ² , and the amount of water with respect to 100 wt.

  The obtained kneaded product was subjected to hot water extraction, and the increase rate of the hot water extract was measured.

The result is shown in FIG.
(Example 3-4)
The change of hot water extract content due to the difference in the particle size of red powder was measured.

  The average particle size of the akamoku powder was changed between 10 and 100 μm, and the obtained akamoku powder was subjected to hot water extraction, and the content of the hot water extract was measured.

  The result is shown in FIG.

The figure which shows the increase rate of a hot-water extract by the change of extruder temperature conditions. The figure which shows the increase rate of a hot-water extract by the change of extruder pressure conditions. The figure which shows the increase rate of a hot-water extract by the change of extruder water conditions. The figure which shows content of the hot water extract by the difference in the average particle diameter of a red powder. The figure which shows a time-dependent change of the hot water extract of Akamok. The figure which shows a time-dependent change of the hot water extract of a red powder (average particle diameter of 50 micrometers).

Claims (5)

Crushing dried seaweed to obtain seaweed powder,
Adding 5 to 100 parts by weight of water to 100 parts by weight of seaweed powder, and preparing a composition containing seaweed powder and water;
A step of kneading the composition using an extruder having a maximum temperature in the cylinder of 60 ° C. to 180 ° C., and a step of extracting fucoidan from the kneaded product,
For producing fucoidan. The method according to claim 1, wherein the maximum temperature in the cylinder during the extruder treatment is 80C to 150C. The method according to claim 1 or 2, wherein the water content is 10 to 50 parts by weight with respect to 100 parts by weight of the seaweed powder. The method according to any one of claims 1 to 3, further comprising a step of enzyme-treating the kneaded product after the step of kneading using the extruder. The method according to any one of claims 1 to 4, wherein the step of extracting fucoidan includes a hot water extraction step, and the hot water extraction step is performed in a range of 0.5 to 1 hour.

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