WO2021118211A2 - Seaweed extract having reduced arsenic, and preparation method therefor - Google Patents

Abstract

The present invention relates to a seaweed extract having a remarkably reduced amount of heavy metal, particularly arsenic, in seaweed, and a preparation method therefor, and to a seaweed extract, having reduced arsenic, that can be applied as an eco-friendly material to health functional food, medicines, cosmetics, and the like.

Description

Arsenic-reduced seaweed extract and manufacturing method thereof

The present invention relates to a seaweed extract containing only a trace amount of arsenic or hardly containing arsenic due to reduced arsenic, and a method for preparing the same.

The immune response is a self-defense mechanism to protect our body, and it includes the process of removing or neutralizing various infectious agents, allergens, and unnecessary metabolites in the body, and plays a role in suppressing the occurrence of diseases by maintaining homeostasis. The immune response in the body is largely divided into innate immune response and acquired immune response, and each immune cell in charge of the immune response has different characteristics. Cells mediating the innate immune response include natural killer cells (NK cells), neutrophils, monocytes, macrophages, and dendritic cells, such as cells responsible for phagocytosis. Among them, macrophages and dendritic cells are immune As an initiator of the reaction, it acts to phagocytose in response to an antigen coming from the outside, secreting cytokines to increase the activity of innate immune cells, or by delivering antigens from the outside to immune T cells to induce activation of the acquired immune system NK cells can directly kill cancer cells by releasing cytotoxic granules, and can simultaneously activate macrophages and T cells by secreting cytokines such as IFN (interferon)-γ. Immune cells involved in the acquired immune response include T cells and B cells, and after the innate immune response, T cells and B cells are activated while recognizing specific antigens presented by phagophagocytes such as macrophages and dendritic cells. This occurs, and the acquired immune response is amplified by the action of cytokines expressed by activated T cells.

Recently, various chemical agent-based anticancer drugs that can directly kill cancer cells have been developed, but various studies are being conducted to suppress cancer cells by increasing immunity in the body due to the cause of serious toxicity. Various studies show anticancer activity by increasing the content of cytokines involved in immune enhancement or by increasing the activity of immune cells that can directly kill cancer cells by using natural ingredients contained in natural products. It stimulates various immune cells to increase the homeostasis of the living body and reduce the incidence of disease. Sargassumhorneri, a brown algae belonging to the family Mozambidae , is a species widely used for food in the Asia-Pacific region. Research on health functionalities is intensifying.

According to the studies so far, it has been reported that Osteoporosis prevention, antioxidant and anticancer effects, and herpes virus inhibitory effects, etc. have been reported, and various studies on new effects and application products using hoesaengi cap are in progress.

However, due to recent marine pollution, the content of heavy metals in seaweeds, such as algae, such as algae, increases, and the arsenic content is particularly high, so there is a problem in that there is a limit to applying it to various application products, pharmaceuticals, cosmetics, etc. Accordingly, when purifying fucoidan from seaweed extract, a patent on a method for removing heavy metals from seaweed extract using a chelating agent has been known, but it has to go through a complicated and complicated process of removing the chelating agent used therein, and the chelating agent in the extract There may be residual problems.

The present invention was accomplished by finding a method for effectively reducing heavy metals, particularly arsenic, from seaweeds, preferably seaweeds such as algae, and more specifically, reducing arsenic, a problem in seaweeds, using self-restraint treatment and titanium dioxide This method effectively removes more than 95% of total arsenic and inorganic arsenic, thereby securing safety and providing a seaweed extract that can be usefully used as a raw material for health functional foods, cosmetics, and pharmaceuticals.

The present invention for solving the above problems relates to a method for producing an arsenic-reduced seaweed extract or a method for reducing arsenic from seaweed, comprising: a first step of preparing a self-contained dried seaweed; a second step of performing a hydrothermal extraction process on a mixture of the self-treated dried seaweed and water to obtain a hot water extract; Step 3 of filtering the hot water extract to obtain a first filtrate; A fourth step of mixing the first filtrate and TiO ₂ powder and then performing a first arsenic reduction treatment by stirring; Step 5 of filtering the first arsenic reduction treatment to obtain a second filtrate; a sixth step of preparing a concentrate by performing a concentration process on the second filtrate so as to have a solid content of 17 to 20% brix; 7 step of mixing the concentrate and TiO ₂ powder and then performing a secondary arsenic reduction treatment by stirring; And after centrifuging the secondary arsenic-reduced concentrate _{to remove TiO 2} powder, and then freeze-drying 8 step; includes a process comprising a.

Another object of the present invention relates to an arsenic-reduced seaweed extract prepared by the above method.

Another object of the present invention is to provide an applied product such as a health functional food, cosmetics, and pharmaceuticals containing the arsenic-reduced seaweed extract.

The present invention can efficiently remove heavy metals, particularly arsenic, from seaweed extract, and since it is possible to manufacture and supply a stable seaweed extract with a very low arsenic content or almost no arsenic, health that is highly harmless to the human body It can be widely used as an eco-friendly material for functional foods, pharmaceuticals and/or cosmetics.

1 is a graph of the measurement result of arsenic reduction in the extract according to the self-sufficiency time.

Figure 2 is a graph of the measurement result of arsenic reduction in the extract according to the type of reducing agent.

Figure 3 is a graph of the measurement result of arsenic reduction in the extract according to the temperature conditions during the primary arsenic reduction treatment.

Figure 4 is a graph of the measurement result of the reduction of arsenic in the extract of hoesaengnijaban according to the _{TiO 2} powder concentration during the primary arsenic reduction treatment at 80°C.

5 is a graph of the measurement result of the reduction of arsenic in the extract of hoesaengmojaban according to the concentration of the _{TiO 2} powder during the secondary arsenic reduction treatment.

Hereinafter, the present invention will be described in more detail.

The method for producing an arsenic-reduced seaweed extract or method for reducing arsenic from seaweeds of the present invention comprises the following steps: preparing a self-treated dried seaweed; a second step of obtaining a hot water extract by performing a hot water extraction process for 3 to 6 hours at 80 to 95° C. on a mixture of the self-treated dried seaweed and water; Step 3 of filtering the hot water extract to obtain a first filtrate; A fourth step of mixing the first filtrate and TiO ₂ powder and then performing a first arsenic reduction treatment by stirring; Step 5 of filtering the first arsenic reduction treatment to obtain a second filtrate; a sixth step of preparing a concentrate by performing a concentration process such that the second filtrate has a solid content of 17 to 20% brix; 7 step of mixing the concentrate and the TiO ₂ powder and then performing a secondary arsenic reduction treatment by stirring; _{And after removing the TiO 2} powder by centrifuging the secondary arsenic reduction-treated concentrate, step 8 of performing freeze-drying; a process including a can be performed.

Step 1-1 of washing the minced seaweed dried seaweed in step 1; Step 1-2 of immersing the washed seaweed and water to swell the seaweed; Steps 1-3 of self-treating a mixture of swollen seaweed and water; and steps 1-4 of washing and dehydrating the self-contained seaweed, and then performing hot air drying to obtain a self-contained dried hoesaengi hat.

In step 1-1, after the raw seaweed material (for example, hoesaeng hatban, etc.) is minced, the minced seaweed may be washed. In a preferred embodiment, foreign substances may be completely removed from the seaweed by washing with 3,000 to 5,000 parts by weight of constant (or purified water) based on 100 parts by weight of the chopped seaweed.

In step 1-2, the seaweed is swollen by immersing it in the washed seaweed and water for 30 minutes to 90 minutes, preferably 40 minutes to 80 minutes, and more preferably 50 minutes to 70 minutes. It is a process for obtaining dried seaweed.

And, in steps 1-3, the swollen seaweed and water are mixed in a weight ratio of 1:15 to 35, preferably, 1:15 to 25 by weight to prepare a mixture, and then, the mixture is heated at 70 to 120° C. for 20 to 50 minutes. Minutes, preferably by heating for 25 minutes to 40 minutes under 90 ~ 100 ℃, and self-treatment, it is possible to partially remove the heavy metal in the seaweed. At this time, if the amount of water used with respect to the swollen seaweed is less than 15 weight ratio, the heavy metal may not be sufficiently removed, and it is uneconomical to exceed 35 weight ratio.

In addition, if the temperature is less than 70 ℃ during self-sugar treatment, there may be a problem that the amount of heavy metal removed in seaweed is too small, and if it exceeds 120 ℃, there may be a problem in that the loss of active ingredients is large.

Compared with the raw seaweed of step 1-1, the self-recovery-treated seaweed in step 1-3 may have a total arsenic content reduction rate of 45% or more, preferably 49.0% or more, and also, the raw seaweed of step 1-1 Compared with , the self-recovery-treated seaweed may have an inorganic arsenic content reduction rate of 70% or more, preferably 75% or more. And, compared with the raw seaweed in step 1-1, the self-recovery-treated seaweed may have a sodium content reduction rate of 85% or more, preferably 90% or more.

In addition, in steps 1-4, the self-treated seaweed may be washed in a general manner and dehydrated in a general manner to remove water and the like from the seaweed. And, the hot air drying can be obtained by performing the hot air drying at 40 ℃ ~ 60 ℃ self-restraint dried hoesaengi hat.

Next, step 2 is a process of obtaining a hot water extract, and a mixture of dried seaweed and water in a weight ratio of 1:30 to 45, preferably 1:35 to 40 by weight, is mixed at 80 to 95° C. A hot water extract can be prepared by performing the hot water extraction process for ~ 6 hours, preferably at 85 ~ 95 °C for 3.5 ~ 5 hours. At this time, if the amount of water used is less than 30 weight ratio, the active ingredient of hoesaengi hat may not be sufficiently extracted, and if it exceeds 45 weight ratio, there may be a problem that the production time of the hot water extract is too long due to excessive water usage.

Next, step 3 is to perform a filtration process to remove foreign substances from the hot water extract, at this time, the filtration can be performed by a general filtration method used in the art, and in a preferred embodiment, 50 to 60 μm A first filtrate can be obtained by performing filtration with a bag filter of

Next, Step 4 is the first as the process of filtration of water the primary non-small reduction, the first filtration in water 100 parts by weight, TiO ₂ powder, 0.7 ~ 5 parts by weight, preferably TiO ₂ powder, 1-4 wt. Part, more preferably TiO ₂ After mixing 1.5 to 3.5 parts by weight of powder, it may be carried out by stirring for 30 minutes to 60 minutes, preferably 45 minutes to 60 minutes. At this time, _{if the amount of TiO 2} powder used is less than 0.7 parts by weight, there may be a problem that the reduction rate of total arsenic and/or inorganic arsenic from the first filtrate is too low, and even if it exceeds 5 parts by weight, it is uneconomical because there is no further increase in the arsenic reduction rate. And, in the case of the primary arsenic reduction treatment, the stirring is preferably performed at 20 ° C. to 90 ° C., preferably under 50 ° C. to 85 ° C., and more preferably under a temperature of 65 to 85 ° C. At this time, the stirring temperature is 20 If it is less than ℃, the arsenic reduction rate may be low, and even if it exceeds 90℃, it is uneconomical because the effect of further reducing arsenic is insignificant.

The primary arsenic reduction treatment may have a reduction rate of total arsenic content of 88.0% or more, preferably 90.0% ~ 93.0%, compared to raw seaweeds, and a reduction rate of inorganic arsenic content compared to raw seaweeds of 80.0% or more, preferably 85.0% ~ 90.0%.

Next, step 5 is a step of filtering the primary arsenic reduction treatment to obtain a second filtrate, and at this time, the filtration is performed in the same manner as in step 3 to remove foreign substances from the first arsenic reduction treatment. .

Next, step 6 is a process of preparing a concentrate by concentrating the second filtrate, in this case, the concentration can be performed using a general concentrator used in the art, and a preferred embodiment, for example, a centrifugal thin film Using a concentrator (evaporator, CEP-LABO, Okawahara, Japan), centrifugal thin film concentration was performed at 80 ~ 85 ℃ and 1,000 ~ 1,500 rpm conditions, solid content 16.5 ~ 22.0% brix, preferably solid content 17.0 ~ A concentrate of 20.0% can be prepared.

Next, the secondary arsenic reduction treatment of step 7 is based on 100 parts by weight of the concentrate, _{2 to 20 parts by weight of TiO 2} powder, preferably 6 to 20 parts by weight, more preferably 10 to 20 parts by weight. After that, it can be carried out by stirring for 30 minutes to 60 minutes, preferably for 30 minutes to 50 minutes. At this time, _{if the amount of TiO 2} powder used is less than 2 parts by weight, there may be a problem that the reduction rate of total arsenic and/or inorganic arsenic from the second filtrate is too low, and even if it exceeds 20 parts by weight, it is uneconomical because there is no further increase in the arsenic reduction rate. And, in the secondary arsenic reduction treatment, stirring is preferably performed at 20 ° C. to 90 ° C., preferably at 50 ° C. to 85 ° C., more preferably at 65 to 85 ° C. At this time, the stirring temperature is 20 If it is less than ℃, the arsenic reduction rate may be low, and even if it exceeds 90℃, it is uneconomical because the effect of further reducing arsenic is insignificant. In addition, the stirring method may be performed in the same manner as the primary arsenic reduction treatment method.

The secondary arsenic-reduced concentrate may have a total arsenic content reduction rate of 94.0% or more, preferably 95.0% or more, compared to the raw seaweed material, and the inorganic arsenic content reduction rate compared to the seaweed raw material is 96.0% or more, preferably 98.5% or more, more Preferably, it may be 99.5% or more.

Next, step 8 is a process for obtaining a freeze-dried seaweed extract by centrifuging the secondary arsenic-reduced concentrate _{to remove TiO 2 powder, then freeze-drying.}

At this time, the centrifugation may be performed for 5 minutes to 20 minutes under 4,000 to 6,000 rpm, and preferably, it is preferable to perform 5 minutes to 15 minutes under 4,500 to 5,500 rpm. And, the freeze-drying may be performed by a general freeze-drying method used in the art.

The seaweed extract prepared through the method described above with reduced arsenic (or the method for reducing arsenic from seaweed extract) can secure human safety from heavy metals such as arsenic, so it can be used in health functional foods, cosmetics and pharmaceuticals. It can be usefully used as a raw material.

An immune activity enhancing composition may be prepared as follows using the seaweed extract prepared by the above method, preferably, the arsenic-reduced oxalic larvae extract, and a health functional food may be prepared using the composition.

Immune activity enhancing composition of the present invention includes a natural extract complex mixed with the arsenic-reduced hoesaengnijaban extract and hoesaengnimojaban supercritical extract as an active ingredient.

And, the mixing ratio of the hoesaengnimojaban extract and the hoesaengnimojaban supercritical extract is 8.5 to 9.7: 0.3 to 1.5 by weight, preferably 8.8 to 9.5: 0.4 to 1.2 by weight, more preferably 9.2 to 9.5: 0.4 to 0.8 by weight can be

The first step of preparing a powder with an average particle diameter of 5 mm or less by pulverizing the hoesaeng hatban supercritical extract having a moisture content of 10% or less; a second step of performing a supercritical extraction process on the powder to obtain a supercritical extract; and a third step of preparing a concentrate by concentrating the supercritical extract under reduced pressure.

The supercritical extraction process of step 2 may be performed for 4 to 5 hours at a pressure condition of 350 to 450 bar and a temperature condition of 45 to 60° C., preferably at a pressure condition of 370 to 420 bar and 45 to 55° C. It can be carried out for 4 to 5 hours under the temperature condition of, At this time, if the pressure condition is out of the above range, there may be a problem in the content of the active ingredient and the color change of the extract, and if the temperature condition is out of the above range, the extraction yield And there may be a problem in the content change of the active ingredient.

In addition, in the supercritical extraction process, supercritical carbon dioxide may be used as a solvent, and fermentation alcohol may be used as an auxiliary solvent, and the solvent is at a flow rate of 2.5 to 3.5 L/min, preferably 2.7. ~ 3.2 L / min supplied at a flow rate, the auxiliary solvent is preferably carried out while supplying at a flow rate of 0.2 ~ 0.4 L / min, preferably 0.25 ~ 0.35 L / min.

The concentration under reduced pressure of the supercritical extract in step 3 can be performed by a general reduced pressure concentration method in the art, and a preferred example is a rotary evaporator (HS-20SP, Hahnshin S&T, Korea) at 50 °C. It is possible to completely concentrate the extract containing the fermented alcohol in to obtain the final hoesaengimojaban supercritical extract in the form of a concentrate.

Such, the immune activity enhancing composition of the present invention improves the cell proliferation and cytokine (IL-2, IFN-γ) secretion ability of splenocytes, and high activity against NK cells and/or macrophages of splenocytes. Having a bar, it is possible to provide an excellent immune enhancing effect.

Hereinafter, the present invention will be described in more detail through Examples and Experimental Examples. However, the following examples are provided to aid the understanding of the present invention, and should not be construed as limiting the scope of the present invention by the following examples.

[Example]

Example 1: Self-restraint treatment of raw hoesaengi hatban

The raw material of the hoesaengi hat (around Wando, Jeollanam-do) was chopped and prepared.

Next, foreign substances were removed by washing with about 40,000 parts by weight of purified water with respect to 100 parts by weight of the chopped hoesaengi hat raw material.

Next, by immersing the washed hoesaengi hat and water for 60 minutes, a swollen hoesaengi hat was obtained.

Next, the swollen hoesaeng hat and water were mixed in a weight ratio of 1:20, and then the mixture was heat-treated at 100° C. for 10 minutes to perform self-storage. Separately, the same mixture was heat-treated at 100° C. for 30 minutes to perform self-restraint. .

Next, after washing and dehydrating each of Saengsaengi hats subjected to self-restraint treatment for 10 minutes and 30 minutes, hot air drying was performed at 50° C. to obtain dried hoesaengi hats subjected to self-restraint treatment (10 minutes/30 minutes).

Experimental Example 1: Analysis of inorganic elements

Total arsenic, inorganic arsenic, and sodium content analysis was performed on each of the dried hoesaeng hats subjected to self-restraint for 10 minutes and 30 minutes in Preparation Example 1, and the results are shown in Table 1 and FIG. 1 below.

division		Content (mg/kg dry weight)
		total arsenic	inorganic arsenic (Inorganc As)	Na (g/100g dry weight)
hoesaengi hat raw material (Control)		64.2	29.8	4.3
division	self-restraint process time	-	-	-
lab scale (lab scale)	10 minutes	35.1 (reduction rate 45.3%)
	30 minutes	31.7 (reduction rate 50.6%)	3.6 (reduction rate 94.4%)	0.2 (Reduction rate 99.7%)
pilot scale (pilot scale)	30 minutes	39.8 (reduction rate 38.0%)	5.7 (reduction rate 91.1%)	1.0 (reduction rate 98.4%)

In the case of arsenic, when comparing the results of 10 minutes and 30 minutes on the lab scale, the total arsenic content of 35.1 mg/kg and 31.7 mg/kg was confirmed, respectively, and the higher 50.6% low in the extract after 30 minutes. showed a decrease. In addition, sodium was confirmed to have a reduction rate of 99.7%, and it was confirmed that most of the sodium was removed by self-restraint treatment for 30 minutes.

The result of self-restraint for 30 minutes on the industrial pilot scale showed a reduction rate of 38.0% lower than that of the lab scale, but in the case of inorganic arsenic and sodium, the reduction rate was more than 90% regardless of the scale. seemed

However, it was confirmed that an additional arsenic reduction process was required due to an excessive content of 1 mg/kg, which is the inorganic arsenic standard of general foods during the Food Encyclopedia.

Example 2: Arsenic content according to treatment by reducing agent

A dried hoesaengi hat was prepared in Example 1, which was self-retained for 30 minutes.

Next, the hot water extraction process was performed at 90° C. for 4 hours with a mixture of the self-restrained dried hoesaeng jaban and purified water (water) in a weight ratio of 1:37 to obtain a hot water extract.

Next, the hot water extract was filtered through a 55 μm bag filter to obtain a filtrate.

With respect to 100 parts by weight of the filtrate, 5 parts by weight of each of acid clay, iron oxide powder, or titanium dioxide powder were mixed and mixed, followed by stirring at about 25° C. for 40 minutes. Arsenic reduction treatment was performed.

And, the total arsenic content for each of them was measured, and the total arsenic reduction rate compared to the hot water extract (filtrate) filtered before the arsenic reduction treatment is shown in Table 2 and FIG. 2 below.

division	reducing agent	After arsenic reduction treatment, Total Arsenic Content (mg/kg)	filtrate contrast Total Arsenic Reduction (%)
filtered hot water extract (HW extraction)	-	2.1	-
of hot water extract filtrate	acid clay	0.54	74.5
	iron oxide powder	0.68	67.7
	titanium dioxide powder	0.35	83.3

Looking at Table 2, all three reducing agents showed arsenic reduction rates of 65% or more, but among them, titanium dioxide powder showed a total arsenic reduction rate of 83.3% compared to the control group, a hot water extract without a reducing agent.

Example 3: Arsenic content according to titanium dioxide powder treatment

(1) Arsenic content measurement according to arsenic reduction treatment temperature

A filtrate of the hot water extract of hoesaengi hatban of Example 2 was prepared.

Next, with respect to 100 parts by weight of the filtrate, after mixing 5 parts by weight of titanium dioxide powder, each at room temperature (25 ℃, room temp.), 30 ℃, 50 ℃, 70 ℃ and 90 ℃ a total of 5 temperature conditions The arsenic reduction treatment was performed by stirring for 1 hour.

Next, each of the arsenic-reducing-treated filtrates was centrifuged at 5,000 rpm for 10 minutes to remove titanium dioxide powder, and then freeze-dried to obtain arsenic-reducing-treated freeze-dried R.

And, the total arsenic content for each of them was measured, and the results are shown in Table 3 and FIG. 3 below, and the reduction ratio (removal ratio) compared to the total arsenic extract (filtrate) filtered before arsenic reduction treatment is the reduction rate.

Temperature	After arsenic reduction treatment, Total Arsenic Content (mg/kg)	filtrate contrast Total Arsenic Reduction (%)
Room temperature (25℃, room temp.)	0.31	82.47
30℃	0.38	78.87
50℃	0.15	91.69
70℃	0.07	96.07
90℃		ND 1)	100
1) ND : Not detected.

The total arsenic concentration of the arsenic-reduced hydrothermal extract treated at 50°C was 0.15 mg/kg, which was lower than the 0.31 mg/kg result of titanium dioxide treatment at room temperature, and 0.07 at 70°C. At mg/kg and 90℃, it was confirmed to be a trace level, and the reduction rate showed a tendency to increase as the temperature increased. In the case of the highest temperature of 90 ℃, the total arsenic content was detected in very small amounts, but it was confirmed that the proper treatment temperature of titanium dioxide was 50 ℃ ~ 85 ℃, preferably about 65 ~ 85 ℃ in terms of safety reasons and total arsenic reduction rate. .

(2) Arsenic content measurement according to the amount of titanium dioxide powder used during arsenic reduction treatment

A filtrate of the hot water extract of hoesaengi hatban of Example 2 was prepared.

Next, with respect to 100 parts by weight of the filtrate, 0.5 parts by weight, 1 part by weight, 2 parts by weight, 3 parts by weight and 5 parts by weight of titanium dioxide powder were mixed to prepare 5 types of mixtures, and then at 80 °C temperature condition Each was stirred for 1 hour to perform arsenic reduction treatment, respectively.

Next, each of the arsenic-reducing-treated filtrates was centrifuged at 5,000 rpm for 10 minutes to remove titanium dioxide powder, and then freeze-dried to obtain arsenic-reducing-treated freeze-dried R.

And, the total arsenic content for each of them was measured, and the results are shown in Table 4 and FIG. 4 below, and the reduction ratio (removal ratio) compared to the total arsenic extract (filtrate) filtered before arsenic reduction treatment is the reduction rate.

Titanium dioxide powder usage	After arsenic reduction treatment, Total Arsenic Content (mg/kg)	filtrate contrast Total Arsenic Reduction (%)
Filtrate (Crtl) of the hot water extract of hoesaengnimojaban of Example 2	1.76	-
0.5 parts by weight	0.76	60.3
1 part by weight	0.52	73.03
2 parts by weight	0.33	82.97
3 parts by weight	0.31	83.62
5 parts by weight	0.3	84.41

Referring to Table 4 and FIG. 4, the total arsenic reduction rate increased as the addition ratio of titanium dioxide increased, and the total arsenic content was confirmed to be at a very trace level after the addition of 2 parts by weight, indicating that the difference in the arsenic reduction rate was insignificant. Therefore, it could be confirmed that the addition amount of titanium dioxide in the hot water extract of hoesaengnijaban is 0.7 to 5 parts by weight, preferably 1 to 4 parts by weight, and more preferably 1.5 to 3.5 parts by weight.

Example 4: Arsenic content according to titanium dioxide powder treatment

A filtrate of the hot water extract of hoesaengi hatban of Example 2 was prepared.

Next, the filtrate of the hot water extract was concentrated using a centrifugal thin film concentrator (evaporator, CEP-LABO, Okawahara, Japan) under the conditions of 82° C. and 1,200 rpm, and concentrated to a solid content of 17.6% brix. was obtained.

Next, with respect to 100 parts by weight of the concentrate, 2 parts by weight, 4 parts by weight, 6 parts by weight, 10 parts by weight, and 20 parts by weight of titanium dioxide powder were mixed to prepare 5 types of mixtures, and then at 80 °C temperature Each of the arsenic reduction treatments were performed by stirring under the conditions for 1 hour.

And, the total arsenic content was measured for each, and the results are shown in Tables 4 and 5 below, and the reduction ratio (removal ratio) compared to the total arsenic extract (filtrate) filtered before arsenic reduction treatment is the reduction rate.

Titanium dioxide powder usage	After arsenic reduction treatment, Total Arsenic Content (mg/kg)	filtrate contrast Total Arsenic Reduction (%)
Concentrate (Crtl) of the hot water extract of hoesaengi hatban of Example 2	24.02	-
2 parts by weight	8.87	63.1
4 parts by weight	6.25	74
6 parts by weight	5.52	77
10 parts by weight	2.82	83.6
20 parts by weight	1.82	89.4

Referring to Table 5 and FIG. 5, in the case of the concentrate of the hot water extract of hoesaengnimojaban of Example 2 as a control, the arsenic content increased during the concentration process. And, it was confirmed that the arsenic reduction rate tends to increase as the amount of titanium dioxide powder added increases, showing the highest arsenic reduction rate of 89.4% at 20 parts by weight.

Preparation Example 1

A dried hoesaengi hat was prepared in Example 1, which was self-retained for 30 minutes.

Next, the hot water extraction process was performed at 90° C. for 4 hours with a mixture of the self-restrained dried hoesaeng jaban and purified water (water) in a weight ratio of 1:37 to obtain a hot water extract.

Next, the hot water extract was filtered through a 55 μm bag filter to obtain a first filtrate.

With respect to 100 parts by weight of the filtrate, 2 parts by weight of titanium dioxide powder was mixed, and the mixture was stirred at about 80° C. for 60 minutes to perform a primary arsenic reduction treatment.

Next, the first arsenic reduction treatment was filtered through a 55 μm bag filter to obtain a second filtrate.

Next, the second filtrate was concentrated using a centrifugal thin film concentrator (evaporator, CEP-LABO, Okawahara, Japan) at 82° C. and 1,200 rpm conditions to obtain a solid content of 17.6% brix. obtained.

Next, with respect to 100 parts by weight of the concentrate, 10 parts by weight of titanium dioxide powder was mixed, and the resultant was stirred at about 80° C. for 60 minutes to perform a secondary arsenic reduction treatment.

Next, the secondary arsenic-reduced concentrate was centrifuged at 5,000 rpm for 10 minutes to separate and remove the titanium dioxide powder in the concentrate, and then freeze-dried to obtain an arsenic-reduced extract.

And, the total arsenic content, inorganic arsenic content and arsenic reduction rate compared to the raw material, the second filtrate treated with the primary arsenic reduction, and the freeze-dried extract from the second arsenic reduction treatment was measured, and the results are shown in Table 6 below.

division	Analysis result of 2 types of hazardous substances (mg/kg)
	Total Arsenic (As)	Inorganic Arsenic (i-As)
hoesaengi hat raw material	115.46	53.72
Second filtrate treated with primary arsenic reduction	9.79 (Reduction rate 91.52%)	6.23 (Reduction rate 88.40%)
Secondary arsenic-reduced freeze-dried extract	5.06 (Reduction rate 95.62%)	0.15 (Reduction rate 99.72%)

Total arsenic and inorganic arsenic were detected at 115.46 mg/kg and 53.72 mg/kg, respectively, in the raw material of the black fern cap, respectively. and 0.15 mg/kg, confirming that the arsenic reduction rate was greater than 95%.

Through the above Examples and Experimental Examples, it can be confirmed that the seaweed extract prepared by the method for reducing arsenic from the seaweed extract of the present invention or the method for preparing the method for preparing the seaweed extract with reduced arsenic has a very low arsenic content. Thus, it was confirmed that the seaweed extract prepared by this method was suitable for use in various products such as health functional foods, cosmetics and pharmaceuticals.

Claims (10)

1. 1st step of preparing the self-treated dried seaweed;

   A second step of obtaining a hot water extract by performing a hot water extraction process for 3 to 6 hours at 80 to 95° C. on a mixture of the self-treated dried seaweed and water;

   Step 3 of filtering the hot water extract to obtain a first filtrate;

   A fourth step of mixing the first filtrate and TiO ₂ powder and then performing a first arsenic reduction treatment by stirring;

   Step 5 of filtering the first arsenic reduction treatment to obtain a second filtrate;

   a sixth step of preparing a concentrate by performing a concentration process on the second filtrate so as to have a solid content of 17 to 20% brix;

   7 step of mixing the concentrate and the TiO ₂ powder and then performing a secondary arsenic reduction treatment by stirring; and

   After centrifuging the secondary arsenic-reduced concentrate _{to remove TiO 2} powder, the 8 step of freeze-drying;

   A method for producing an arsenic-reduced seaweed extract comprising a.
2. The method according to claim 1, wherein the dried seaweed treated in step 1 is

   Step 1-1 washing the minced seaweed;

   Step 1-2 of immersing the washed seaweed and water for 30 to 90 minutes to swell the seaweed;

   Steps 1-3 of heating a mixture of swollen seaweed and water for 20 to 50 minutes at 70 to 120° C. for self-restraint; and

   Steps 1-4 of washing and dehydrating the self-contained seaweed, and then performing hot air drying to obtain a self-contained dried sagebrush;

   A method for producing an arsenic-reduced seaweed extract, characterized in that it is prepared by performing a process comprising a.
3. The method according to claim 2, wherein the mixture of steps 1-3 contains swollen seaweed and water in a weight ratio of 1:15 to 35 by weight.
4. The method according to claim 1, wherein the mixture in step 2 contains the self-treated dried seaweed and water in a weight ratio of 1:30 to 45 by weight.
5. The method of claim 1, wherein the first arsenic reduction treatment in step 4 is performed by mixing 0.7 to 5 parts by weight of _{TiO 2 powder with respect to 100 parts by weight of the first filtrate, followed by stirring for 30 to 60 minutes.} A method for producing an arsenic-reduced seaweed extract comprising
6. The method according to claim 1, wherein each of the filtration in steps 3 and 5 is performed using a bag filter of 50 to 60 μm.
7. The method of claim 1, wherein the secondary arsenic reduction treatment in step 7 is performed by mixing 2 to 20 parts by weight of _{TiO 2 powder with respect to 100 parts by weight of the concentrate, followed by stirring for 30 to 60 minutes.} A method for preparing an arsenic-reduced seaweed extract.
8. [Claim 8] The method for producing an arsenic-reduced seaweed extract according to any one of claims 1 to 7, wherein the seaweeds include algae.
9. A seaweed extract prepared by the method of any one of claims 1 to 7, comprising:

   An arsenic-reduced seaweed extract, characterized in that the reduction rate of the total arsenic content compared to the raw seaweed material is 94.0% or more, and the inorganic arsenic content reduction rate is 96.0% or more compared to the raw seaweed material.
10. 1st step of preparing the self-treated dried seaweed;

    A second step of obtaining a hot water extract by performing a hot water extraction process for 3 to 6 hours at 80 to 95° C. on a mixture of the self-treated dried seaweed and water;

    Step 3 of filtering the hot water extract to obtain a first filtrate;

    A fourth step of mixing the first filtrate and TiO ₂ powder and then performing a first arsenic reduction treatment by stirring;

    Step 5 of filtering the first arsenic reduction treatment to obtain a second filtrate;

    a sixth step of preparing a concentrate by performing a concentration process on the second filtrate so as to have a solid content of 17 to 20% brix;

    7 step of mixing the concentrate and the TiO ₂ powder and then performing a secondary arsenic reduction treatment by stirring; and

    After centrifuging the secondary arsenic-reduced concentrate _{to remove TiO 2} powder, the 8 step of freeze-drying;

    A method for reducing arsenic of seaweed, comprising:

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