JP2005120193A - Extraction method and manufacturing method of porphyran - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a manufacturing method of porphyran, which gives enhanced productivity by simplifying the manufacturing steps, which facilitates handling and management of materials for use through disusing hazardous substances as the materials to be used for extraction or purification upon manufacturing porphyran, and which improves safety of the product by preventing the putrefaction of the porphyran extract from occurring. <P>SOLUTION: A plate laver is dispersed, with the algae disintegrated, into water, and this mixed liquid is placed in an autoclave and boiled to conduct hot water extraction. The extract is centrifugally dehydrated with a centrifugal dehydrator to conduct solid-liquid separation. The liquid portion of the extract is filtered using diatomaceous earth as a filtering aid. The liquid portion filtered is filtered and concentrated using ultrafiltration equipment. The concentrated liquid is filtered through a porous synthetic resin to perform deodorization and decoloring, which is followed by sterilization treatment with a sterilizing apparatus. The concentrated liquid that has been subjected to the sterilization treatment is dried with a spray drier and pulverized to obtain powders of porphyran. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

The present invention relates to a porphyran extraction method and production method.
More specifically, the present invention relates to a product that has improved productivity by simplifying the production process of porphyran. Further, in the production of porphyran, the present invention relates to a product that does not use a hazardous material as a material for extraction and purification, facilitates handling and management, and improves product safety. Further, the present invention relates to a product that improves the safety of products by preventing the decay of porphyran extract.

  Porphyran is a kind of high molecular weight polysaccharide containing a sulfate group extracted from the algal body of the red seaweed Amanori, and occupies about 30 to 35% of the dried seaweed mass. Porphyran is expected to be used in various fields such as foods, cosmetics, and pharmaceuticals because of its various usefulness for physiological functions of the living body such as water retention and ultraviolet light impermeability.

  As a method for producing this porphyran, conventionally, (1) after hot water extraction of a dried seaweed of the genus Amanori, an alkyltrimethylammonium compound is added as a precipitant to the hot water extract and left to form a precipitate. After removing the precipitant and reprecipitating with ethyl alcohol (see Patent Document 1), (2) adding acetic acid and calcium acetate to the same hot water extract concentrate as above to adjust the pH to 3-6 After adjustment, ethyl alcohol is added and allowed to stand to form a precipitate, the precipitate is washed with 80% -ethyl alcohol and then dehydrated with 100% -ethyl alcohol (see Patent Document 2), (3) red algae The algal bodies of the genus Amanori are extracted with 20 times the amount of distilled water, filtered, added with different concentrations of ethyl alcohol, separated and precipitated, dissolved in distilled water, dialyzed, and then dried. Exclusion chromatographed except protein contaminants and are further methods (see Patent Document 3) separated and purified by adsorption on the surface of the lipophilic substances, such as is proposed.

Japanese Patent Laid-Open No. 10-60002

Japanese Patent Laid-Open No. 10-60003

Japanese Patent Laid-Open No. 11-310603

Needless to say, the industrial production of porphyran requires manufacturing processes, product safety, and low cost.
However, the production methods described in Patent Documents 1 to 3 not only require complicated operations and long-time treatments, but also yield (yield) decreases if high purity porphyran is obtained. This is not necessarily suitable for industrial implementation because productivity is extremely low and manufacturing costs are high.

  Specifically, the production methods described in Patent Documents 1 to 3 use a nori raw material after pulverization. In order to pulverize the laver, a dedicated pulverizer is required, and the cost for introducing the device is also high. Furthermore, in the production process, the porphyran extract and the laver material are separated into solid and liquid, but when filtering finely ground laver, the finer the powder, the higher the performance required for the filtration device, It will be expensive.

Moreover, the manufacturing method of patent documents 1-3 uses the organic solvent, for example, ethanol, methanol etc., as a flocculant of the fine powder nori raw material. However, ethanol and methanol are handled as dangerous materials, and from the viewpoint of safety, sufficient handling is required for their handling, storage, management, and use. In addition, facilities for storing and managing them are also required.
Together, these are factors that raise the production cost of porphyran, and this increase in production cost is a major issue when industrializing the production of porphyran.

The inventors of the present invention have tried numerous experiments on the extraction or purification of industrially useful porphyran, not on the laboratory level.
In other words, in order to reduce the manufacturing cost, firstly, the extraction process was reviewed, and secondly, the purification process was reviewed. Specifically, in the extraction process, we are mainly researching the possibility of simplifying the crushing process of the seaweed raw material or eliminating the crushing process itself, and in the refining process, mainly use dangerous substances such as ethanol and methanol. Research has been conducted on the possibility of purification without the need for purification.

During the research of the extraction process, the raw laver was divided into three types: fine powder, coarse powder, and unground, and samples were made. I had left it at room temperature for 20 hours. These samples differed only in the form of the raw materials, and even though they were produced in the same manner and left under the same conditions, there was a difference in the degree of decay.
That is, the unmilled product was not spoiled and remained in the nori smell. On the other hand, the raw laver was fine and the coarse powder was rotten and gave off an ammonia odor.
In manufacturing, if the spoiled extract is misused, toxins may remain in the product, creating a safety issue. This is a major problem when porphyran is used as a food additive, health food, and the like.

In addition, when producing Porphyran industrially, if the production plant is always in operation for 24 hours, Porphyran is produced without decaying through a series of production processes. It doesn't matter much if the times are slightly different.
However, for example, when the production plant is stopped due to a power failure or the like, if the stop time becomes longer, the extract may be spoiled in the apparatus. In other words, in industrial production, the extraction and purification process of porphyran is automatically performed at the production plant. However, when the production plant stops, for example, the extract liquid stays in the transport pipe for about half a day. The possibility of corruption cannot be denied. Therefore, in the production of porphyran, it is necessary to take measures assuming that the production plant is stopped.

(Object of the present invention)
An object of the present invention is to provide a porphyran extraction method and a production method in which productivity is improved by simplifying the porphyran production process.

  Another object of the present invention is to avoid the use of hazardous materials in the materials used for extraction and purification in the production of porphyran, thereby facilitating the handling and management of the materials used and improving the product safety. It is another object of the present invention to provide a method for extracting and producing porphyran.

  Still another object of the present invention is to provide a porphyran extraction method and a production method that improve the safety of the product by preventing the decay of the porphyran extract produced in the porphyran production process.

  The means of the present invention taken in order to solve the above problems are as follows.

In the first invention,
A step of hot water extraction of plate laver or waste laver to obtain an extraction mixture,
Dehydrating the extraction mixture and separating the residue to obtain an extract;
Filtering and concentrating the extract;
Including,
This is a method for extracting porphyran.

In the second invention,
The temperature of hot water is 120 to 160 ° C.,
It is the extraction method of porphyran which concerns on 1st invention.

In the third invention,
Processing steps by the porphyran extraction method according to the first or second invention,
Sterilizing the concentrated extract;
Drying the sterilized concentrated extract;
Including,
This is a method for producing porphyran.

The term “plate laver or waste laver” as used in the claims and specification includes laver that has been discarded in the past, such as waste laver or discolored laver that does not turn into a product.
The type of seaweed used as a raw material is Asakusanori or Susabiori, which is a genus of red algae, but is not limited thereto. Porphyran is also contained in low-grade seaweed in large quantities, so in addition to plate seaweed that is usually used for food, it is possible to use scrap seaweed or discolored seaweed that does not turn into a product as described above. it can.

  Examples of the filter used for filtration include a ceramic filter, a reverse osmosis membrane, and an ultrafiltration membrane. In addition to the diatomaceous earth film and the synthetic resin film, for example, a collodion film, a gelatin film, a cellophane film, or a porous polymer film having various pore sizes can be used as the ultrafiltration membrane.

  If the temperature of hot water during hot water extraction is less than 120 ° C., sufficient extraction efficiency of porphyran cannot be obtained. Moreover, there exists a problem that it is necessary to heat within a very high pressure, and industrialization is somewhat difficult to make the temperature of hot water over 160 degreeC. In addition, it is more preferable to extract within the range of 120-125 degreeC from a viewpoint of preventing the influence on the quality by the high temperature of the porphyran used as a product.

(A) According to the method for extracting or producing porphyran according to the present invention, plate laver or waste laver is used as a raw material, so that a step of further pulverizing it as in the conventional method becomes unnecessary. Further, since the solid-liquid separation of the extract is performed by ultrafiltration, there is no step such as fractional precipitation using an organic solvent such as ethanol or methanol, as in the conventional method.
Therefore, since the production process of porphyran can be simplified, production in a shorter time than before can be achieved, and a higher-purity porphyran can be obtained and productivity can be increased. Moreover, the cost of expensive equipment such as a pulverizer and organic solvents such as ethanol and methanol is not required. Moreover, since the productivity is high as described above, the manufacturing cost of porphyran can be reduced, and excellent industrialization becomes possible.

(B) In producing porphyran, since organic materials such as ethanol and methanol, which are hazardous materials, are not used as materials for extraction and purification, the materials used can be handled, stored and managed relatively easily. In addition, since there is no concern that such materials remain in the product, the safety of the product can be improved, and a porphyran with higher added value can be produced.

(C) By using plate laver or waste laver as a raw material, it is possible to extend the time until the porphyran extract rots compared to the case of using a ground algal body as a raw material, and it is difficult for rot to occur. Become.
As a result, even when the production plant is stopped for a long time due to a power failure or the like, for example, the possibility that the extract liquid staying in the device will be spoiled can be reduced, and the safety of the product can be improved. it can.

(D) What the temperature of hot water at the time of hot water extraction is 120-160 degreeC can improve the extraction efficiency of porphyran more, and can improve productivity at the time of industrialization.

  The present invention will be described in detail based on examples described below.

FIG. 1 is a flowchart showing a method for producing porphyran according to the present invention.
With reference to FIG. 1, the manufacturing method of the porphyran which concerns on this invention is demonstrated.

(1) The seaweed used as a raw material is plate seaweed or waste seaweed. In this case, a plate of seaweed that had been discolored (dry weight 1 kg) was used.

(2) The plate seaweed was dissolved in water (30 L) by dissolving algal bodies, and this mixed solution was placed in a high-pressure kettle and boiled to perform hot water extraction. Most of the protein contained in the seaweed is contained in the residue and not in the liquid, so the purity of porphyran can be increased. The hot water extraction was performed at an extraction temperature of 120 ° C. and the extraction time was 120 minutes. This obtained the extraction liquid mixture (mixture liquid of an extract liquid and a residue).

(3) The extracted mixed solution was subjected to centrifugal dehydration using a centrifugal dehydrator, and solid-liquid separation was performed. Thereby, it isolate | separated into the extract (liquid component) and solid residue containing porphyran. The solid residue was discarded.

(4) The extract was filtered using diatomaceous earth as a filter aid.
(5) The filtered extract was filtered and concentrated using an ultrafiltration device (concentration step: a ceramic filter was used as the ultrafiltration membrane). The waste liquid generated in the concentration process was discarded.

(6) The concentrated solution was filtered through a porous synthetic resin to perform deodorization and decolorization (the same effect can be obtained by using an activated carbon filter).
(7) The concentrated solution that had been deodorized and decolored was sterilized with a sterilizer.
(8) The concentrated sterilized liquid was dried by spray drying and pulverized. As a result, 200 g of porphyran powder having a purity of porphyran of 95% or more was obtained.

(Function)
According to the porphyran extraction method or production method according to the present invention, plate laver or waste laver is used as a raw material, so that the pulverizing step as in the conventional method is not necessary. Further, since the solid-liquid separation of the extract is performed by ultrafiltration, there is no step such as fractional precipitation using an organic solvent such as ethanol or methanol, as in the conventional method.
Therefore, since the production process of porphyran can be simplified, production in a shorter time than before can be achieved, and a higher-purity porphyran can be obtained and productivity can be increased.
Moreover, the cost of expensive equipment such as a pulverizer and organic solvents such as ethanol and methanol is not required. Moreover, since the productivity is high as described above, the manufacturing cost of porphyran can be reduced, and excellent industrialization becomes possible.

  As mentioned above, when producing porphyran, organic materials such as ethanol and methanol, which are hazardous materials, are not used as materials for extraction and purification, so handling, storage and management of the materials used can be made relatively easy. . In addition, since there is no concern that such materials remain in the product, the safety of the product can be improved, and a porphyran with higher added value can be produced.

Furthermore, by using plate laver or waste laver as a raw material for laver, the reason is not clear compared to the case of using a ground algal body as a raw material, but it can prolong the time until the porphyran extract rots. Yes, it is less likely to rot.
As a result, even when the production plant is stopped for a long time due to a power failure or the like, for example, the possibility that the extract liquid staying in the device will be spoiled can be reduced, and the safety of the product can be improved. it can.

  In the extraction of porphyran by the method according to the present invention, an experiment was conducted to determine how much difference in extraction efficiency is caused by the difference in temperature and extraction time of hot water to be extracted.

(Experimental example 1)
FIG. 2 is a graph showing a difference in extraction efficiency due to a difference in temperature and extraction time of hot water to be extracted.
In the experiment, hot water extraction of the seaweed was performed in an oil bath using plate seaweed (paper leaf-like seaweed) as a raw material. The extraction conditions were such that the extraction time was 15 minutes, 30 minutes, 60 minutes, and 120 minutes for extraction temperatures of 100 ° C., 105 ° C., and 120 ° C., respectively.
The raw laver used was 0.2 g, and the amount of water used for extraction was 20 ml. After the extraction, a disposable filter (pore size 0.45 μm) was used, and the extracted mixed solution was filtered to obtain 2 ml of the extracted solution.
In this way, 12 liquid samples were prepared, and the extraction efficiency was examined for each.
The extraction efficiency was examined by anthrone method. Moreover, since porphyran is contained in the plate nori as a raw material in a mass of about 30% of the dry mass, the content mass was set to 100%, and the proportion of porphyran obtained as a product was converted as the extraction efficiency.

As can be seen from this graph (FIG. 2), the higher the extraction temperature, the better the extraction efficiency. Also, the extraction efficiency was better as the extraction time was longer.
It should be noted that the difference in extraction efficiency between the extraction temperature of 105 (100) ° C. and 120 ° C. was remarkable, and the difference was more remarkable especially when the extraction time was 30 minutes or more.
Thereby, when a nori raw material is a plate nori, when extraction temperature was 120 degreeC and extraction time was 30 minutes or more, it turned out that efficient extraction can be performed.

  Further, in the extraction of porphyran by the method according to the present invention, an experiment was conducted to determine how much difference in extraction efficiency is caused by the difference in the form of the nori raw material and the extraction time.

(Experimental example 2)
FIG. 3 is a graph showing the difference in extraction efficiency due to the difference in the shape and extraction time of the laver to be extracted.
In the experiment, the nori raw material was made into three forms of fine powder, coarse powder, and plate nori (paper leaf nori), and hot water extraction of the nori was performed in an oil bath. The extraction conditions were such that the extraction time was 15 minutes, 30 minutes, 60 minutes, and 120 minutes for an extraction temperature of 120 ° C.
The raw material used was 0.2 g, and the amount of water used for extraction was 20 ml. After the extraction, a disposable filter (pore size 0.45 μm) was used, and the extracted mixed solution was filtered to obtain 2 ml of the extracted solution.
In this way, 12 liquid samples were prepared, and the extraction efficiency was examined for each.

As can be seen from this graph (FIG. 3), the extraction efficiency was better as the extraction time was longer.
Moreover, what the form of the nori raw material is a powder had the extraction efficiency superior to the plate nori.
However, between the powder and the plate nori, the plate nori was only slightly lower, and the difference in extraction efficiency was within about 10 to 20%. Therefore, in view of improvement in productivity due to simplification of the manufacturing process and the like, it has been found that it is essentially no problem to use plate laver as a raw material in the industrialization of porphyran production.

  Next, the difference in the progress of rot due to the difference in the form of the nori raw material of the extract extracted by the method according to the present invention was confirmed by experiments.

(Experimental example 3)
The nori raw material forms were fine powder, coarse powder, and plate nori (paper leaf nori), and hot water extraction of the nori was performed in an oil bath. The extraction conditions were two conditions of 120 ° C. for 30 minutes and 120 ° C. for 60 minutes.
In each form, the raw materials used were 0.2 g, and the amount of water used for extraction was 20 ml.
After the extraction, a disposable filter (pore size 0.45 μm) was used, and the extracted mixed solution was filtered to obtain 2 ml of the extracted solution.

  Extracted under the above conditions for each form of each nori raw material by the above method, sample 1 extracted at 120 ° C. for 30 minutes as fine powder, sample 2 at 120 ° C. for 60 minutes, sample 120 for coarse powder 30 ° C, sample 3 for 30 minutes, 120 ° C for coarse powder, sample 4 for 60 minutes, 120 ° C for plate nori, 5 for sample for 30 minutes, 120 ° C for 60 minutes for plate nori 6 (see Table 1).

Each sample was placed in a 2 ml sealed container, and the color and smell of the extract were observed. All the samples had a light yellow transparent color, and the smell was the seaweed smell itself.
Each sample was allowed to stand at room temperature overnight (about 20 hours). And after leaving to stand, the color and smell of the extract were observed for each sample (see Table 2).

As shown in Table 2, the extract of the nori raw material was powder, and the color was cloudy and had a decayed ammonia odor. This tendency was stronger for fine powder with finer grains than for coarse powder. In addition, when the seaweed material was made from plate seaweed, there was no change in color and there was no ammonia odor.
To clarify this reason, the sugar content and protein content of each sample were examined, but there was almost no difference due to the difference in the seaweed raw materials.
Therefore, the difference in the progress of the rotting due to the difference in the form of the nori raw material seems to be caused by the extraction of the more easily rotting component by making the nori raw material into powder.

  According to this experimental result, the rotting of the extract is delayed by making the laver raw material into plate laver, and even when the production plant is stopped for a long time (at most 20 hours from the experimental result) due to a power outage accident or the like, for example. It has been found that the possibility that the extract liquid staying in the apparatus may be rotted can be reduced, and the safety of the product can be improved.

  Note that the terms and expressions used in the present specification are merely explanatory and not restrictive, and do not exclude terms and expressions equivalent to the above terms and expressions. The present invention is not limited to the illustrated embodiment, and various modifications can be made within the scope of the technical idea.

The flowchart which shows the manufacturing method of the porphyran which concerns on this invention. The graph which shows the difference of the extraction efficiency by the difference of the temperature of hot water to extract, and extraction temperature. The graph which shows the difference of the extraction efficiency by the difference in the form of the nori to extract, and extraction temperature.

Claims (3)

A step of hot water extraction of plate laver or waste laver to obtain an extraction mixture,
Dehydrating the extraction mixture and separating the residue to obtain an extract;
Filtering and concentrating the extract,
Including,
Extraction method of porphyran. The temperature of hot water is 120 to 160 ° C.,
The porphyran extraction method according to claim 1. A processing step by the porphyran extraction method according to claim 1 or 2,
Sterilizing the concentrated extract;
Drying the sterilized concentrated extract;
Including,
A method for producing porphyran.

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