JP2009084460A - Apparatus for and method of extracting and purifying fucoidan - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To eliminate loss of seaweed raw materials when handling the same for extracting fucoidan in the form of a viscous substance, and to produce a large amount of high-quality fucoidan. <P>SOLUTION: In an apparatus, three tank structures, which are designated as a funnel, an extraction tank and a server tank, are connected as shown in Fig.1. The funnel and the extraction tank is connected to each other through an internal structure comprising an internally contacting screen frame, as shown in Fig.2. By operating valves built on the tanks, fucoidan contained in seaweeds is extracted from a seaweed powder under heating and subsequently subjected to solid-liquid separation and purification by sedimentation. A method for extracting and purifying fucoidan is also provided. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to an apparatus for extracting and purifying fucoidan, which is a kind of viscous polysaccharide contained in gagome kelp, and a method for extracting and purifying fucoidan.

Fucoidan is a polysaccharide containing fucose as a main constituent monosaccharide, and also a sulfated polysaccharide containing glucuronic acid and mannose as constituent sugars. Fucoidan is also a water-soluble dietary fiber. Mainly contained in brown algae gagome and mozuku.
This fucoidan is known to have a physiologically active function. For example, there is a technique for use as an immunostimulator (Patent Document 1), a cancer therapeutic drug (Patent Document 2), or an antibacterial agent (Patent Document 3). It is being considered.

  As described above, fucoidan has a physiologically active function, and therefore a method for producing the same has been developed. Techniques such as a method capable of obtaining a large amount of fucoidan (see Patent Document 4), a method of extracting with acidic hot water (see Patent Document 5), and a method using a microfiltration device (see Patent Document 6 and Patent Document 7) are disclosed. ing.

  As for the production of fucoidan, it is generally produced using known general-purpose equipment for each process. Although there is also a disclosure as a dedicated device (see Patent Document 8), in this case, a combustion process is required and this is a special method. The manufacturing process is not achieved by a series of processes, and has a problem of poor productivity.

In the production of fucoidan, various methods have been devised as described above. Generally, after removing insoluble solids by boiling from a dry sample with hot water to obtain an extract, it is precipitated in the same manner as other water-soluble dietary fibers by adding 1 to 2 volumes of alcohols. It can be recovered as a product.
The production of fucoidan requires an operation of solid-liquid separation, but this operation is usually not easy due to its viscosity.

The disclosure of a method that can acquire a large amount of fucoidan (see Patent Document 4) is a scale that can be acquired in several tens of mg from several g of raw material, and is suitable for large-scale production when planning industrial production. It is hard to say that the technology.
JP 2005-82806 JP Japanese Patent Laid-Open No. 2003-55234 JP 2005-263812 JP JP 2006-233099 A JP 2006-160862 A JP 2006-143817 A Japanese Patent Laid-Open No. 2002-262788 JP 2004-339308 A

Conventionally, the basic process for extracting fucoidan is to mix and stir raw seaweed powder with hot water or water adjusted to acidity, and after a certain period of time, obtain a water-soluble substance obtained as a viscous substance, for example, solid-liquid For separation, the powder that is the extraction residue is separated by a centrifuge, and 1 to 2 times the amount of ethanol or the like is added to and mixed with the water-soluble substance obtained as a supernatant. For example, it is separated by a centrifuge and recovered as a solid content.
In this operation, a method using volume compression by freezing (Patent Document 5), a method using a microfiltration device to remove a pigment component (Patent Document 6), and a low molecular weight other than fucoidan are similarly filtered by a filter device. Although removing (patent document 7) etc. is disclosed, these do not solve the problem about the loss which arises in extraction operation. An object of the present invention is to mass-produce high-quality fucoidan by eliminating the loss of seaweed raw materials that occur during handling because fucoidan is obtained as a viscous substance.

In order to efficiently produce fucoidan from seaweed, a production apparatus that integrates extraction, solid-liquid separation, and purification, and a method for producing fucoidan using this apparatus are provided.
That is, the present invention
1. An apparatus for extracting and purifying fucoidan from seaweed, the apparatus comprising a funnel for introducing raw material powder, an extraction tank for extracting fucoidan coupled under the funnel, and a fucoidan disposed adjacent to the funnel and the extraction tank. A server tank for purification is provided, and the funnel, the extraction tank, and the server tank all have a conical bottom shape, and a filter provided between the funnel and the extraction tank and a funnel portion extending from the funnel into the extraction tank. And a fucoidan extraction / purification apparatus, further comprising a connecting pipe connecting the lower end of the extraction tank and the lower end of the server tank. 2. The fucoidan extraction / purification device according to 1 above, wherein a thin tube for introducing steam, a serpentine tube for steam heating or water cooling of the extraction tank, and a leak valve are provided in the extraction tank. No. 1 valve for opening and closing the connection with the atmosphere provided at the upper end of the funnel, No. 2 and No. 3 for discharging the extraction liquid or derivation of the extraction liquid provided at the lower end of the extraction tank, provided in the connecting pipe And a valve No. 5 and a valve No. 6 for introducing an extraction liquid and discharging a purified liquid provided at the lower end of the server tank, and a valve No. 7 provided at the upper end of the server tank. 3. The fucoidan extraction / purification apparatus according to 1 or 2 above. 4. The fucoidan extraction / purification device according to any one of 1 to 3 above, wherein a water level gauge is provided at the upper and lower positions of the server tank.

The present invention also provides: A method for extracting and purifying fucoidan from seaweed by the following steps using a funnel for introducing raw material powder, an extraction tank coupled under the funnel, and a server tank for purifying fucoidan disposed adjacent to the funnel and the extraction tank.
1) The process of injecting seaweed powder as a raw material into the funnel and injecting the cleaning liquid into the extraction tank 2) With the funnel open to the atmosphere, the extraction tank is heated and the funnel is connected to the lower end of the funnel The process of raising the cleaning liquid in the extraction tank and mixing the raw powder and cleaning liquid in the funnel 3) Stop the introduction of steam and return the cleaning liquid to the extraction tank by using the reduced pressure in the extraction tank. The solid component containing fucoidan is left on the filter provided between the extraction tank and the solid tank, and the remaining washing liquid is discharged from the lower end of the extraction tank. 4) Seal the funnel and extraction tank. At the same time, the extraction liquid and steam are introduced into the extraction tank, the extraction liquid is raised from the funnel, the fucoidan on the filter is dissolved, and the fucoidan is contained on the filter. The process of refining fucoidan by separating the extract and the residue to be purified 5) The extract containing fucoidan is fed to the server tank via a connecting pipe that connects the lower end of the extraction tank and the lower end of the server tank. Step of transferring 6) In the server tank, the purified fucoidan is precipitated as an insoluble solid, and the fucoidan is recovered from the lower end of the server tank as an insoluble suspension. In the step 1), fucoidan is extracted and extracted from seaweed by dissolving and removing water-soluble substances such as amino acids, salts, pigments and sugar alcohols using a washing solution of an aqueous ethanol solution containing acetic acid. 6. Purification method 7. The method for extracting and purifying fucoidan as described in 5 or 6 above, wherein in step 3), the extraction tank is cooled with water through a serpentine tube surrounding the extraction tank from the outside, and the inside of the extraction tank is decompressed. Extracting and refining fucoidan according to any one of 5 to 7 above, wherein in step 4), an extraction solution containing calcium chloride is used to solid-liquid separate alginic acid as a solid residue on a filter. Method 9 In the step 5), when the extract containing the fucoidan in the extraction tank is transferred to the server tank, the valve provided on the upper part of the server tank is opened to open the server tank to the atmosphere, and the extract in the extraction tank The above is characterized in that steam, compressed air and compressed inert gas are further introduced into the upper portion of the extraction tank and pressurized, and the remaining extract in the extraction tank is sent to the server tank. 9. Method for extracting and purifying fucoidan according to any one of 5 to 8. 10. In the above step 6), ethanol corresponding to twice the amount of the extract is introduced into the server tank to precipitate the purified fucoidan as an insoluble solid content. A method for extracting and purifying fucoidan is provided.

As described above, in the operation method of this apparatus, it is possible to heat the extraction tank using water vapor, and use water vapor or inert gas to utilize the differential pressure between pressurization and depressurization. It is possible to carry out solid-liquid separation and to purify fucoidan in a separate tank connected by a connecting pipe.
In order to provide this function, the bottom shape of the tank is conical. Moreover, it is devised so that it may become a secret structure by the operation of the valve installed in the piping part which is the doorway to the outside. In addition, for the purpose of cooling the remaining heat, the cooling water is circulated around the extraction tank.

  The viscous polysaccharide contained in the kelp of brown algae generally contains 10-40 g of fucoidan per 1 kg of dry leaf weight. Further, it contains 200 to 300 g of alginic acid. Fucoidan obtained by extracting these viscous polysaccharides contained in brown algae with, for example, hot water of tap water to obtain a dry powder contains a considerable amount of alginic acid. As an operation method of the apparatus of the present invention, the solution used at the time of extraction solves this problem. Hereinafter, description will be made sequentially.

In the specific example of the extraction apparatus of the present invention, the capacity of the extraction tank required for processing 1 kg of the sample is about 100 liters, and the extraction tank has a diameter of 600 mm.
Since the size of this extraction device can be changed according to the amount to be processed, it is not particularly limited. However, when describing the present invention, a device of this size will be used.

The funnel has a truncated cone structure with an opening of about 70 degrees at the bottom of a cylinder having a length of 650 mm and a diameter of 500 mm. This funnel is fixed so that a filter coupling in which a sieve frame defined by JISZ8801 is inscribed can be removed.
The filter coupling is a device that connects the extraction tank and the funnel. A funnel fixed with a filter coupling and an inner packing structure is inserted into the extraction tank. FIG. 2 shows an assembly structure of the funnel and the extraction tank with a focus on the filter coupling of the parts constituting the fucoidan extraction device.
The extraction tank has a thin tube for introducing steam.

Like the funnel, the server tank is cylindrical with a length of 1300 mm and a diameter of 500 mm, and the bottom has a conical shape with an opening of 50 degrees. The extraction tank and the server tank are connected by a connecting pipe having five valves.
The funnel and server tank have canopies, and each canopy has valves (valves 1 and 7). By the valve operation, the tank becomes an airtight container, and a constant pressure operation and pressure reduction operation are possible.

The auxiliary equipment for operating this equipment includes a narrow pipe that introduces steam from the heat source into the extraction tank, a jacket-type snake pipe that heats the tank and its operation valve, and the same snake pipe that is used for heating to cool the extraction tank. There is the operation valve.
This device is equipped with a pressure valve, leak valve, thermometer, pressure gauge, and water level meter for safe operation and monitoring of the operating state.

(Prescription of seaweed cleaning solution)
An acidic alcohol solution is used for the seaweed washing solution. For example, a solution containing 0.1 ml to 6 ml of acetic acid can be used per liter of an ethanol solution having a concentration of 50% v / v to 70% v / v.

(Fucoidan extract formulation)
Use mineral solution. For example, an aqueous solution containing 0.5 g to 650 g of calcium chloride dihydrate per liter can be used.

(Types of solutions used for fucoidan purification)
Solution alcohol used for the purification of fucoidan can be used. For example, it is desirable to use ethanol having a purity of 50% v / v to 70% v / v and high purity when mixed with fucoidan extract.
At this time, it becomes insoluble, but pure or salt water is used when the precipitated fucoidan is rendered water-soluble again. For example, an aqueous solution of sodium chloride or potassium chloride having a concentration of 0.0% (w / v) to 10% (w / v) can be used. At this time, about 1 to 100 mM of EDTA · 2Na (ethylenediaminetetraacetic acid · disodium) can be added to remove the remaining minerals.

According to the present invention, fucoidan can be extracted and purified from a dry powder of kelp such as gagome without loss of solid content. The three steps of raw material cleaning, extraction, and purification can be performed consistently with this equipment, because this process is performed in a continuous tank that can be sealed from the supply of raw materials to the extraction and migration of fucoidan. is there.
That is, since there is no work such as material transfer to another device or container transfer in each process, there is a great effect that production efficiency is good without loss.
This production method and apparatus structure can reduce the risk of contamination from outside. In addition, the device is easy to design for scale expansion for mass production. Solid-liquid separation between the seaweed raw material and the fucoidan extract solution is economical because it does not require capital investment such as a centrifugal separator or an ultrafiltration device because it is separated by filtration or sedimentation with a pressure difference. In addition, since no flame is used in the vicinity of the installation location of the apparatus, there is an excellent effect that the labor work in operation of the apparatus is safe.

  The features of the present invention will be specifically described below. The following description is intended to facilitate understanding of the present invention, and is not limited thereto. That is, all modifications, other embodiments, and other examples based on the technical idea of the present invention are included in the present invention.

  The apparatus having the structure shown in FIG. 1 was manufactured into an apparatus having a size shown in paragraph [0012] and subsequent paragraphs. The Example of the method of extracting fucoidan from gagome kelp using this apparatus is shown. The extraction method is the order of washing, extraction, and purification of the raw materials. At this time, there is a solid-liquid separation step in the method of using the washing solution, the extraction solution, and the purification solution.

(Cleaning seaweed ingredients)
Valves 2, 3, and 4 at the bottom of the extraction tank are closed, and a cleaning solution of 30 liters of 70% (V / V) ethanol containing 30 ml of acetic acid is injected into the extraction tank.
Then, a filter coupling sieve frame is installed, and 900 g of gagome kelp powder is introduced from the top of the funnel. Then, with the funnel valve # 1 open, the leak valve is closed and heated with steam.

When the heating temperature reaches 70 ° C., the ethanol washing liquid reaches the funnel through the inner funnel and mixes with the gagome kelp powder.
After a few minutes, the introduction of steam is stopped. When heat is released by passing cooling water through the serpentine tube, the extraction tank is in a reduced pressure state, and the extract is recovered from the funnel to the extraction tank, and solid-liquid separation is performed by a filter of a sieve frame in the filter coupling.

  Water-soluble substances such as amino acids, salts, pigments, and sugar alcohols are extracted and removed from Gagome kelp. Polysaccharides such as fucoidan are not extracted and remain as solids on the sieve frame in the filter coupling. The washing liquid was collected by opening the lower valve of the extraction tank.

(Fucoidan extraction)
Pour 30 liters of extraction solution containing 39 g of calcium chloride into the extraction tank. Steam is introduced into the jacket and narrow tube of the extraction tank and heated. The extraction tank with the valve closed has a temperature of approximately 75 ° C. to 100 ° C., and the extract reaches the funnel through the inner funnel and is mixed with the washing powder of gagome kelp.
At this time, the actual temperature of the extract in the funnel is 80 ° C to 90 ° C. The extraction time may be about 5 minutes. Stop the introduction of steam, introduce water into the external serpentine of the extraction tank, and cool it.

  This extract has reduced viscosity inherent to Gagome, and the extract is collected in the extraction tank and subjected to solid-liquid separation with a filter of a sieve frame in the filter coupling. By this operation, alginic acid becomes insoluble due to the presence of calcium and remains on the filter. As a result, fucoidan enters the extract among the polysaccharides in the solid content on the sieve frame in the filter coupling. As a result, fucoidan is purified.

(Purification of fucoidan)
Calcium chloride-containing extract containing fucoidan in the extraction tank opens valve 7 on the canopy of the server tank, closes valve 3 and valve 5 in the connecting pipe, valve 2, valve 4 and valve 6 When the number is released, the liquid is fed until the water surface matches according to the principle of Pascal.
After that, when the valve No. 1 of the funnel canopy is closed and steam is again introduced from the narrow tube, the extraction tank is pressurized and the extract is transferred to the server tank.
At this time, compressed air or inert gas other than steam is connected to the leak valve of the extraction tank and can be transferred in the same manner even when pressurized. When the transfer is completed, the valves No. 4, No. 5 and No. 6 of the connecting pipe are closed, and ethanol corresponding to twice the amount of the extract is introduced from the server tank canopy.

As a result, fucoidan becomes insoluble and settles. Sedimentation starts after ethanol is added, but in order to recover the flocs of fucoidan that has settled, it may be allowed to stand for several hours to overnight. In this solution state, the fucoidan is stable, and the standing time is only related to the ease of the fucoidan recovery operation, and does not affect the quality.
Since the next extraction operation can be performed, the extraction tank may be left in the meantime. If standing still is sufficient, valves 5 and 6 at the bottom of the server tank are opened and only the purified fucoidan that has settled is collected.

Since the bottom of the server tank has a conical shape, the residue of the sedimented fucoidan in the tank is small and effective. Fucoidan was purified as an insoluble suspension.
The purified fucoidan can be obtained by lyophilizing it into a powder, or by adding pure water or salt water again so that the alcohol content is several percent or less.
For example, in this example, 0.9% sodium chloride containing 10 mM EDTA · 2Na was added to obtain fucoidan that became water-soluble again.

  Using this apparatus, 50 g of dried fucoidan powder was recovered from 900 g of dried gagome kelp. This value is consistent with the amount of fucoidan normally contained in gagome. As a result of infrared spectroscopic analysis, fucoidan obtained by this apparatus showed the spectrum shown in FIG.

  The present invention relates to a technique for efficiently extracting viscous polysaccharides of seaweed. Anti-tumor activity and anti-inflammatory action are known, and it will be possible to secure the necessary amount of fucoidan from seaweed that is expected to be used in advanced industries such as functional foods and pharmaceuticals in the future. The expansion of production scale is easy by changing the tank scale, and the structure is simple, so it can be used for mass production of fucoidan.

It is a figure which shows the whole example of the fucoidan extraction apparatus in connection with embodiment of this invention. It is an example of the figure which shows the assembly structure of a funnel and an extraction tank centering on the filter coupling of the components which comprise the fucoidan extraction apparatus in connection with embodiment of this invention. It is a figure which shows the example of the infrared spectroscopy analysis result of the fucoidan extracted from gagome kelp using the fucoidan extraction apparatus in connection with embodiment of this invention.

Claims (10)

  An apparatus for extracting and purifying fucoidan from seaweed, the apparatus comprising a funnel for introducing raw material powder, an extraction tank for extracting fucoidan coupled under the funnel, and a fucoidan disposed adjacent to the funnel and the extraction tank. A server tank for purification is provided, and the funnel, the extraction tank, and the server tank all have a conical bottom shape, and a filter provided between the funnel and the extraction tank and a funnel portion extending from the funnel into the extraction tank. And a connecting pipe that connects the lower end of the extraction tank and the lower end of the server tank.   2. The fucoidan extraction / purification apparatus according to claim 1, wherein the extraction tank is provided with a thin tube for introducing steam, a serpentine tube for steam heating or water cooling of the extraction tank, and a leak valve.   No. 1 valve for opening and closing the connection with the atmosphere provided at the upper end of the funnel, No. 2 and No. 3 for discharging the extraction liquid or derivation of the extraction liquid provided at the lower end of the extraction tank, provided in the connecting pipe And a valve No. 5 and a valve No. 6 for introducing an extraction liquid and discharging a purified liquid provided at the lower end of the server tank, and a valve No. 7 provided at the upper end of the server tank. The fucoidan extraction / purification device according to claim 1 or 2.   The fucoidan extraction / purification device according to any one of claims 1 to 3, wherein a water level gauge is provided over the upper and lower positions of the server tank. A method for extracting and purifying fucoidan from seaweed by the following steps using a funnel for introducing raw material powder, an extraction tank coupled under the funnel, and a server tank for purifying fucoidan disposed adjacent to the funnel and the extraction tank.
1) The process of injecting seaweed powder as a raw material into the funnel and injecting the cleaning liquid into the extraction tank 2) With the funnel open to the atmosphere, the extraction tank is heated, and from the funnel connected to the lower end of the funnel The process of raising the cleaning liquid in the extraction tank and mixing the raw powder and cleaning liquid in the funnel 3) Stop the introduction of steam and return the cleaning liquid to the extraction tank by using the reduced pressure in the extraction tank. The solid component containing fucoidan is left on the filter provided between the extraction tank and the solid tank, and the remaining washing liquid is discharged from the lower end of the extraction tank. 4) Seal the funnel and extraction tank. At the same time, the extraction liquid and steam are introduced into the extraction tank, the extraction liquid is raised from the funnel, the fucoidan on the filter is dissolved, and the fucoidan is contained on the filter. The process of refining fucoidan by separating the extract and the residue to be purified 5) The extract containing fucoidan is fed to the server tank via a connecting pipe that connects the lower end of the extraction tank and the lower end of the server tank. Step 6) In the server tank, the purified fucoidan is settled as an insoluble solid, and the fucoidan is recovered from the lower end of the server tank as an insoluble suspension.   6. The fucoidan according to claim 5, wherein in step 1), a water-soluble substance such as an amino acid, a salt, a pigment, or a sugar alcohol is dissolved and removed from seaweed using a washing solution of an aqueous ethanol solution containing acetic acid. -Method of purification.   7. The method for extracting and purifying fucoidan according to claim 5 or 6, wherein, in the step 3), the extraction tank is water-cooled through a serpentine tube surrounding the extraction tank from the outside, and the inside of the extraction tank is decompressed.   Extracting fucoidan according to any one of claims 5 to 7, wherein in the step 4), an extraction solution containing calcium chloride is used for solid-liquid separation of alginic acid as a solid residue on a filter. How to purify.   In the step 5), when the extract containing the fucoidan in the extraction tank is transferred to the server tank, the valve provided on the upper part of the server tank is opened to open the server tank to the atmosphere, and the extract in the extraction tank After the liquid is supplied, steam, compressed air, and compressed inert gas are further introduced into the upper portion of the extraction tank and pressurized, and the remaining extract liquid in the extraction tank is sent to the server tank. Item 9. A method for extracting and purifying fucoidan according to any one of Items 5 to 8. 10. In the step 6), ethanol corresponding to twice the amount of the extract is introduced into the server tank to precipitate the purified fucoidan as an insoluble solid content. A method for extracting and purifying the fucoidan described.

Images