JP2021514683A - Seaweed powder and its manufacturing method - Google Patents

Abstract

Provided is a method for producing high quality seaweed powder suitable for food use. This method is used to wash raw, dried or water-rehydrated red seaweed, pre-treat with alkali, pre-treat with acid, hydrolyze with cellulase, dry and grind the treated red seaweed to obtain seaweed powder Includes the step of obtaining. The seaweed powder produced by the techniques described herein has a light color, excellent taste and flavor, good mouthfeel, high gelling ability, excellent stability, and ideal smoothness, suitable for food. It has slipperiness.

Description

Cross-reference to related applications This application claims the interests of provisional patent application No. 62 / 668,656 (Filing date: May 8, 2018) in the United States. Partial continuation application No. 16 / 010,306 (Filing date: June 2018) May 15th). This application also claims the benefit of Provisional Patent Application No. 62 / 781,519 (Filing Date: December 18, 2018) in the United States. These applications are incorporated herein by reference in their entirety.

Technical Field The present invention relates to seaweed powder and a method for producing the same. The seaweed powder described herein can be an alternative to agar. The method of the present invention and the production of seaweed powder can be utilized in the food industry.

Agar is a polysaccharide extracted from red algae such as Gelidiaceae and Gracilaria, and is one of the most widely used algal colloids. Agar has been used as a food in Japan and China for hundreds of years. It first came out in a jelly-like mass, and its form is still available today. After World War II, Western countries industrialized the production of agar powder. Agar powder was initially used for culturing microorganisms and then expanded into the food, cosmetics and pharmaceutical industries. Agar has unique gel properties and gel stability, and has a wide range of uses not only in the food industry but also in the pharmaceutical, cosmetics and biotechnology industries.

Clean Labels and disruptive Greens are gaining in popularity in the food industry, and they are ranked in the Top 10 Innova's 2017 Trends and are natural. Brings a keen interest in being and clean labels. This trend has expanded worldwide over the past few years and is a new standard in the industry. It offers great market potential for edible seaweed powder to replace agar.

U.S. Patent Application Publication No. 2015/0164125 describes a method for producing seaweed powder by collecting seaweed from the seabed, chopping, washing, drying with a seaweed stirrer, storing dry, and grinding to powder. ing. U.S. Pat. No. 4,125,392 describes seaweed filtrates in which raw seaweed is mixed with water and other substances and then decomposed by steam treatment to give a steam-digested mixture. This filter is obtained by scooping the top of the resulting vapor digestion mixture and is used on its own or in the form of liquids or pellets as a starting material for the production of fertilizers or plant growth stimulants. To.

These prior art documents have only produced simple seaweed powders or seaweed masses with low gelling potential and brown or green, strong rocky shore flavors. These prior art seaweed products are not suitable for use as edible gelling agents or stabilizers to replace agar extracted from red seaweed. Therefore, in this field, there is a need to produce higher quality seaweed powder suitable for food.

Outline of the Invention First, the present specification describes a method for producing an edible seaweed powder instead of agar. In this method, raw or dried red seaweed is washed, pretreated with alkali, pretreated with acid, treated with an enzyme such as cellulase, and the treated red seaweed is dried and ground to obtain seaweed powder. including. If necessary, this method involves bleaching the red seaweed with bleach prior to the drying and grinding steps. In some embodiments, the bleaching step is performed prior to the enzyme treatment step. In some embodiments, the bleaching step is performed after the enzyme treatment step. The present invention is a seaweed powder with light color, excellent taste and flavor, good mouthfeel, high gelling ability, excellent stability, and ideal smoothness and slipperiness suitable for "clean label" foods. Provides a simple manufacturing method for.

Next, this specification describes the seaweed powder produced by the above-mentioned method. The seaweed powder produced by the method of the present invention can be used in the food industry instead of agar, for example, as a gelling material for dairy products, jellies and puddings.

This application includes at least one color drawing.

1A-1C show the FTIR results of seaweed powder sample 2 (upper curve) compared with commercially available seaweed powder (sample 10, central curve) and agar (sample 11, lower curve). FIG. 1A shows the entire range. FIG. 1B shows the selected range (enlarged). 1550-1510 cm- ¹ relates to the NH stretch (amide band II) of the protein. FIG. 1C shows the selected range (enlarged). The spectrum around 890 cm ^-1 is mainly related to the CH expansion and contraction of the anomeric carbon of the β-galactose residue. A strong band of 930 cm- ¹ indicates the presence of 3,6-anhydro-D-galactose.

The seaweed powder (Sample 2) obtained by the method described herein has less protein (Fig. 1B) and is 3,6-anhydro-D-, as compared with the commercially available seaweed powder (Sample 10). High in galactose (Fig. 1C). Compared to commercially available agar (Sample 11), Sample 2 contains slightly more protein (FIG. 1B) but slightly less β-galactose and 3,6-anhydro-D-galactose (FIG. 1C).

This specification describes a method for producing high quality seaweed powder suitable for food applications. The method of the present application is a simple seaweed powder with the necessary functions for food such as light color, excellent taste and flavor, good mouthfeel, high gelling ability, excellent stability, and ideal smoothness and slipperiness. It is a manufacturing method. The seaweed powder produced by the method of the present invention can be used in place of agar in the food industry, for example, as a gelling agent in the production of dairy products, jellies and puddings.

In some embodiments, the methods described herein wash the seaweed material with water, pretreat the washed seaweed material with alkali, pretreat the alkali treated seaweed material with acid, and pretreat the seaweed material. Is bleached with a bleaching agent, and the bleached seaweed material is treated with an enzyme to obtain a seaweed powder suitable for food. The bleaching process is optional and may be performed when light colored seaweed powder is required. In some embodiments, the method of the present application further comprises processing the enzyme-treated seaweed by a twin-screw extrusion process, followed by grinding and drying the extruded seaweed.

Seaweeds are also called large algae, marine algae or seagrass. Seaweed materials used in the methods of the invention include red algae, such as Gracilaria, Gelidiaceae, Porphyra, and Ahnfeltia. In some embodiments, at least two, at least three, or at least four of the disclosed red algae can be used in combination.

Seaweed material is washed with water before each treatment. Any seaweed material can be used, including dried seaweed, raw seaweed or water-rehydrated seaweed. It is known in the art that dried seaweed can be obtained by removing water from raw seaweed. It can be returned to water by immersing the dried seaweed in water. In some embodiments, the dried seaweed is returned to water during the washing process. When using dried seaweed, the ratio of dried seaweed: water in the washing step is 1: 1 to 1:40, 1: 3 to 1:30, 1: 5 to 1:25, 1: 5 to 1: It may be 20, 1: 10 to 1:20 or 1: 5 to 1:10, and when using raw seaweed or seaweed rehydrated with water, the ratio of raw seaweed: water in the washing step is , 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5, 1: 1 to 1:10 or 1: 1 to 1:15.

Alkali that can be used in the method of the present invention includes sodium hydroxide, potassium hydroxide, calcium hydroxide or a combination of these alkalis. Various forms of alkali (eg, hydrates) can be used in the present invention. In the pretreatment step, the seaweed: alkali ratio may be 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The concentration of the alkaline solution is 1% -10%, 3% -15%, 5% -15%, 5% -10%, 10% -20%, 3% -20% or 10% -30% (weight%). ) May be. In some embodiments, the temperature of the alkaline pretreatment step is 40 ° C to 80 ° C, 65 ° C to 95 ° C, 50 ° C to 100 ° C or 70 ° C to 120 ° C. In some embodiments, the time of alkali pretreatment is 0.5 hours to 24 hours, 0.5 hours to 20 hours, 0.5 hours to 15 hours, 0.5 hours to 12 hours, 0.5 hours to 8 hours. , 0.5 hours to 6 hours, 1 hour to 4 hours, 1.5 hours to 3 hours or 0.5 hours to 4 hours.

Acids that can be used in the methods of the invention include hydrochloric acid, nitric acid, phosphoric acid and oxalic acid. Alternatively, a combination of disclosed acids can be used, such as a combination of at least two acids, at least three acids or at least four acids. In the pretreatment step, the seaweed: acid ratio may be 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The concentration of the acid solution is 0.05% to 5%, 0.1% to 3%, 0.1% to 2%, 0.1% to 1% or 0.1% to 0.5% (% by weight). ) May be. In some embodiments, the acid pretreatment time may be 5 minutes to 240 minutes, 10 minutes to 180 minutes, 10 minutes to 120 minutes, 10 minutes to 60 minutes, or 20 minutes to 60 minutes.

If necessary, the seaweed is treated with bleach to give a light colored seaweed powder. Bleach that can be used in the method of the present invention includes hypochlorous acid, sodium hypochlorite and chlorine dioxide. Alternatively, the disclosed bleach combinations, such as at least two bleach combinations or at least three bleach combinations, can be used. In the bleaching step, the seaweed: bleach ratio may be 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The effective chlorine concentration of bleach is 0.01% to 5%, 0.02% to 3%, 0.05% to 2%, 0.05% to 1% or 0.05% to 0.5% ( By weight%). In some embodiments, the time of the bleaching step may be 5 minutes to 240 minutes, 10 minutes to 180 minutes, 10 minutes to 120 minutes, 10 minutes to 60 minutes or 20 minutes to 60 minutes.

In some embodiments, the pretreated or bleached seaweed has less than 5% red seaweed impurities, less than 4%, less than 3%, less than 2% or less than 1%, and a sulfate content of less than 3% and less than 2%. Less than 1% or less than 0.5% and light brown to light yellow.

Enzymatic treatment catalyzes the hydrolysis of cellulose and / or related polysaccharides in pretreated and / or bleached seaweed and improves the palatability of the resulting seaweed powder. For this purpose, various enzymes such as cellulase, hemicellulase, pectinase, amylase, xylanase, pentosanase, glucanase, esterase and the like can be used. In some embodiments, one or more enzymes can be used to treat the seaweed. Examples of suitable enzymes are 1,4-β-D-glucan glucanohydrolases, endo-1,4-β-D- obtained from the genus Trichoderma, Aspergillus or Penicillium. Includes, but is not limited to, glucanase, 1,4-β-D-glucan cellobiohydrolase, exo-1,4-β-D-glucanase, β-1 4-glucosidase, acid cellulase, medium A cellulase containing a sex cellulase and an alkaline cellulase. In some embodiments, combinations of at least two, at least three or more of these cellulases can be used. In the enzyme treatment step, the seaweed: enzyme ratio may be 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The enzyme concentration may be 10 U / g to 500 U / g, 20 U / g to 400 U / g, 30 U / g to 300 U / g, 50 U / g to 200 U / g or 75 U / g to 150 U / g. In some embodiments, the time of the enzyme treatment step is 0.5 hours to 12 hours, 0.5 hours to 8 hours, 0.5 hours to 6 hours, 1 hour to 3 hours or 1 hour to 4 hours. The pH may be 2.0 to 10.0, 3.0 to 9.0, 3.0 to 8.0, 4.0 to 7.0, or 5.0 to 6.0. Alternatively, the temperature may be 15 ° C to 100 ° C, 20 ° C to 90 ° C, 30 ° C to 80 ° C, 20 ° C to 70 ° C, 30 ° C to 60 ° C, 40 ° C to 50 ° C.

Various acids or alkalis can be used to adjust the pH. For example, the pH adjusting alkali is selected from the group consisting of sodium hydroxide, potassium hydroxide and combinations thereof. The acid for pH adjustment is selected from the group consisting of hydrochloric acid, nitric acid, phosphoric acid and at least two or three combinations of these acids.

The methods described herein further include processing the enzyme-treated seaweed by a twin-screw extrusion process, if desired, at processing temperatures of 70 ° C. to 200 ° C., 80 ° C. to 150 ° C. , 100 ° C. to 150 ° C., 100 ° C. to 140 ° C., 120 ° C. to 140 ° C. or 110 ° C. to 130 ° C. The twin-screw extrusion process can be performed in the absence or presence of water. For example, the seaweed: water ratio may be 1: 0 to 1: 5, 1: 1 to 1: 3 or 1: 0 to 1: 2.

In some embodiments, the washed seaweed is pretreated at 65 ° C. to 95 ° C. using a 5% to 15% (% by weight) alkaline solution in a ratio of 1: 2 to 1: 5 and 0.1% to. Pretreated with 0.5% (% by weight) acid solution at a ratio of 1: 2 to 1: 5 and 75 U / g to 250 U / g of cellulase at a ratio of 1: 2 to 1: 5. Then, the treatment is performed at 40 ° C. to 60 ° C., and then the twin-screw screw extrusion treatment is performed at 110 ° C. to 140 ° C.

The enzyme-treated seaweed or the twin-screw extruded seaweed can be crushed and dried to obtain a seaweed powder. In some embodiments, the water gel strength of the dried seaweed powder is at least 50 g / cm ² , at least 75 g / cm ² , at least 100 g / cm ² , at least 120 g / cm ² or at least 150 g / cm ² . In some embodiments, the dried seaweed powder is light brown to light yellow. In some embodiments, the melting point of the dried seaweed powder is 100 ° C. or lower, 90 ° C. or lower, 85 ° C. or lower, 75 ° C. or lower, or 60 ° C. or lower.

In some embodiments, the seaweed powder obtained by the techniques described herein has the following components:
It contains 40% or more soluble dietary fiber, about 20% to 35% insoluble dietary fiber, 75% or more total dietary fiber, 2% or less sulfate, and 5% or less protein.
In some embodiments, the seaweed powder obtained by the techniques described herein has the following properties:
It has a gel strength of 100 g / cm ² or more (1.5%) and a melting point of 60-95 ° C. (1.0%).

The following examples are intended to illustrate various embodiments of the invention. Therefore, the following specific embodiments should not be construed as limiting the scope of the invention. It will be apparent to those skilled in the art that various equivalents can be manufactured, modified and modified without departing from the scope of the invention, and such equivalent embodiments are described herein. It is understood that it is included in the book. In addition, all references cited herein are incorporated by reference in their entirety, as described herein.

Example 1 Materials and methods The algae used in the examples are as follows:

Other reagents include:
Food-grade hypochlorous acid and sodium hypochlorite with an effective chlorine concentration of 10%; food-grade chlorine dioxide with an effective chlorine concentration of 50%; food-grade 99% sodium hydroxide, potassium hydroxide, calcium hydroxide; Food grade 36% hydrochloric acid; and food grade 99% sulfuric acid, nitrate, oxalic acid, phosphate; 50,000 U / g acidic cellulase, neutral cellulase, alkaline cellulase. HAAKE Process 11 A parallel twin screw extruder was used in a particular process.

Example 2 Production of seaweed powder from dried Gracilaria 10 kg of dried Gracilaria and 50 kg of water are mixed in a tank, stirred at 60 rpm for 30 minutes to wash the seaweed, and then the water is removed to obtain 50 kg of clean seaweed. It was. The seaweed was mixed with 50 kg of a 3% sodium hydroxide solution in a reaction tank, the mixture was heated, stirred at 50 ° C. and 60 rpm for 30 minutes, and then the seaweed was washed with 500 kg of water. Water was removed to give 48 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 50 kg of 0.1% hydrochloric acid were mixed in a tank, stirred for 10 minutes, washed with 100 kg of water, and then the water was removed to obtain 46 kg of acid pretreated seaweed. This pretreated seaweed is mixed with 50 kg of a 0.05% bleaching hypochlorous acid (HClO) solution, stirred at 60 rpm for 10 minutes, then the hypochlorous acid solution is removed and the seaweed is mixed with 100 kg of water. Washed. Water was removed to give 46 kg of pretreated seaweed. The pretreated seaweed was yellow with red impurities of 0.5% or less and sulfate content of 0.3% or less.

Subsequently, the pretreated seaweed was mixed with 46 kg of an acidic cellulase solution of 30 U / g, adjusted to pH 3.0 with hydrochloric acid, and stirred at 20 ° C. and 60 rpm for 30 minutes. The cellulase solution was then removed and the seaweed was washed with 100 kg of water. 40 kg of cellulase-treated seaweed was obtained.

HAAKE Process 11 Seaweed was processed at a set heating temperature of 100 ° C. using a parallel twin-screw extruder. Then, the extruded seaweed was dried and crushed to obtain 3.5 kg of seaweed powder.

Example 3 Production of seaweed powder from raw Gracilaria 50 kg of raw Gracilaria and 150 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 49 kg of clean seaweed. The seaweed and 120 kg of 6% sodium hydroxide solution were mixed in a reaction tank. The mixture was heated and stirred at 85 ° C. and 60 rpm for 120 minutes. The seaweed was washed with 600 kg of water and the water was removed to obtain 48 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 120 kg of 0.38% phosphoric acid solution were mixed in a tank, stirred for 30 minutes and then washed with 100 kg of water. Water was removed to give 48 kg of acid pretreated seaweed. This acid pretreated seaweed was mixed with 120 kg of a 0.1% sodium hypochlorite solution as a bleaching agent, stirred at 60 rpm for 30 minutes, the sodium hypochlorite solution was removed, and the mixture was washed with 100 kg of water. Water was removed to give 45 kg of pretreated seaweed. The pretreated seaweed had a red impurity of 0.8% or less, a sulfate content of 0.2% or less, and was pale yellow.

The pretreated seaweed was mixed with 120 kg of a 100 U / g cellulase solution, adjusted to pH 5.0 with hydrochloric acid, heated, and stirred at 50 ° C. and 60 rpm for 120 minutes. The cellulase solution was removed and the seaweed was washed with 100 kg of water. 41 kg of cellulase-treated seaweed was obtained.

HAAKE Process 11 The treated seaweed was processed at a set heating temperature of 128 ° C. using a parallel twin-screw screw extruder. Then, the extruded seaweed was dried and crushed to obtain 3.8 kg of seaweed powder.

Example 4 Production of seaweed powder from dried Gracilaria 10 kg of dried Gracilaria and 150 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 50 kg of clean seaweed. The seaweed and 250 kg of 20% sodium hydroxide solution were mixed in a reaction tank. The mixture was heated and stirred at 100 ° C. and 60 rpm for 12 hours. The seaweed was then washed with 600 kg of water. Water was removed to give 45 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 225 kg of 0.5% nitric acid were mixed in a tank, stirred for 2 hours, and washed with 100 kg of water. Water was removed to give 42 kg of acid pretreated seaweed. This acid pretreated seaweed was mixed with 210 kg of a 0.5% sodium hypochlorite solution as a bleaching agent, stirred at 60 rpm for 120 minutes, then the sodium hypochlorite solution was removed and washed with 200 kg of water. Water was removed to give 42 kg of pretreated seaweed. The pretreated seaweed was pale yellow with red impurities of 0.4% or less and sulfate content of 0.1% or less.

The pretreated seaweed was mixed with 210 kg of a 300 U / g neutral cellulase solution, adjusted to pH 8.0, heated, and stirred at 70 ° C. and 60 rpm for 6 hours. The cellulase solution was removed and the seaweed was washed with 200 kg of water. 32 kg of cellulase-treated seaweed was obtained.

The treated seaweed was mixed with 64 kg of water and processed using a HAAKE Process 11 parallel twin-screw extruder at a set heating temperature of 140 ° C. Then, the extruded seaweed was dried and crushed to obtain 2.5 kg of seaweed powder.

Example 5 Production of seaweed powder from dried Gracilaria 10 kg of dried Gracilaria and 120 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 50 kg of clean seaweed. The seaweed and 150 kg of 10% sodium hydroxide solution were mixed in a reaction tank. The mixture was heated and stirred at 90 ° C. and 60 rpm for 4 hours, after which the seaweed was washed with 600 kg of water. Water was removed to give 48 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 150 kg of 0.4% sulfuric acid were mixed in a tank, stirred for 1 hour, and washed with 100 kg of water. Water was removed to give 48 kg of acid pretreated seaweed. This acid pretreated seaweed was mixed with 150 kg of a 0.3% hypochlorous acid solution as a bleaching agent, and the mixture was stirred at 60 rpm for 1 hour. The sodium hypochlorite solution was then removed and the seaweed was washed with 100 kg of water. Water was removed to give 46 kg of pretreated seaweed. The pretreated seaweed was pale yellow with red impurities of 0.6% or less and sulfate content of 0.3% or less.

The pretreated seaweed was mixed with 150 kg of a 200 U / g alkaline cellulase solution, adjusted to pH 8.0 with hydrochloric acid, heated, and stirred at 60 ° C. and 60 rpm for 4 hours. The cellulase solution was removed and the seaweed was washed with 100 kg of water. 42 kg of cellulase-treated seaweed was obtained.

The treated seaweed was mixed with 42 kg of water and processed using a HAAKE Process 11 parallel twin-screw extruder at a set heating temperature of 120 ° C. Then, the extruded seaweed was dried and crushed to obtain 3.5 kg of seaweed powder.

Example 6 Production of seaweed powder from dried Gracilaria 10 kg of dried Gracilaria and 150 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 50 kg of clean seaweed. The seaweed and 120 kg of 4% sodium hydroxide solution were mixed in the reaction tank. The mixture was heated, stirred at 85 ° C. and 60 rpm for 2 hours and then washed with 600 kg of water. Water was removed to give 49 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 150 kg of 0.4% sulfuric acid were mixed in a tank, stirred for 45 minutes, and washed with 100 kg of water. Water was removed to give 46 kg of acid pretreated seaweed. This acid pretreated seaweed was mixed with 150 kg of a chlorine dioxide solution which is a 0.3% bleaching agent, and stirred at 60 rpm for 1 hour. The chlorine dioxide solution was removed and washed with 100 kg of water. Water was removed to give 46 kg of pretreated seaweed. The pretreated seaweed had a red impurity of 0.8% or less, a sulfate content of 0.4% or less, and a light brown color. Then, the extruded seaweed was dried and crushed to obtain 4.2 kg of seaweed powder.

Example 7 Production of seaweed powder from Ahnfeltia
10 kg of Ahnfeltia and 150 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 49 kg of clean seaweed. The seaweed and 120 kg of 5% sodium hydroxide solution were mixed in the reaction tank. The mixture was heated, stirred at 88 ° C. and 60 rpm for 120 minutes, then washed with 500 kg of water. Water was removed to give 47 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 120 kg of 0.39% oxalic acid solution were mixed in a tank, stirred for 30 minutes, and washed with 100 kg of water. Water was removed to give 48 kg of acid pretreated seaweed. This acid pretreated seaweed was mixed with 120 kg of a 0.15% bleaching hypochlorous acid solution and stirred at 60 rpm for 30 minutes. The hypochlorous acid solution was then removed and the seaweed was washed with 100 kg of water. Water was removed to give 46 kg of pretreated seaweed. The pretreated seaweed was pale yellow with red impurities of 0.5% or less and sulfate content of 0.3% or less.

The pretreated seaweed was mixed with 120 kg of an acidic cellulase solution of 110 U / g, adjusted to pH 4.80 with hydrochloric acid, heated, and stirred at 45 ° C. and 60 rpm for 180 minutes. The cellulase solution was removed and the seaweed was washed with 100 kg of water. 42 kg of cellulase-treated seaweed was obtained.

HAAKE Process 11 The treated seaweed was processed at a set heating temperature of 130 ° C. using a parallel twin-screw extruder. Then, the extruded seaweed was dried and crushed to obtain 3.6 kg of seaweed powder.

Example 8 Production of seaweed powder from dried Gelidium 10 kg of dried Gelidium and 100 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 50 kg of clean seaweed. The seaweed and 100 kg of 5% sodium hydroxide solution were mixed in a reaction tank. The mixture was heated, stirred at 60 ° C. and 60 rpm for 6 hours, then washed with 600 kg of water. Water was removed to give 49 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 100 kg of 0.2% phosphoric acid solution were mixed in a tank, stirred for 1 hour, and washed with 100 kg of water. Water was removed to give 48 kg of acid pretreated seaweed. This acid pretreated seaweed was mixed with 150 kg of a 0.06% sodium hypochlorite solution as a bleaching agent, and the mixture was stirred at 60 rpm for 1 hour. The sodium hypochlorite solution was removed and the seaweed was washed with 100 kg of water. Water was removed to give 46 kg of pretreated seaweed. The pretreated seaweed had a red impurity of 0.5% or less, a sulfate content of 0.4% or less, and was light brown.

The pretreated seaweed was mixed with 150 kg of an 80 U / g acidic cellulase solution, adjusted to pH 5.5, heated, and stirred at 40 ° C. and 60 rpm for 1.5 hours. The cellulase solution was removed and the seaweed was washed with 100 kg of water. 43 kg of cellulase-treated seaweed was obtained.

The treated seaweed was mixed with 43 g of water and processed using a HAAKE Process 11 parallel twin-screw extruder at a set heating temperature of 115 ° C. Then, the extruded seaweed was dried and crushed to obtain 3.2 kg of seaweed powder.

Example 9 Production of seaweed powder from dried Porphyra 10 kg of dried Porphyra and 150 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 50 kg of clean seaweed. The seaweed and 200 kg of a 15% calcium hydroxide solution were mixed in a reaction tank, stirred at 90 ° C. and 60 rpm for 6 hours, and then washed with 500 kg of water. Water was removed to give 50 kg of alkaline pretreated seaweed. Alkaline pretreated seaweed and 150 kg of 0.4% phosphoric acid solution were mixed in a tank, stirred for 45 minutes, and washed with 150 kg of water. Water was removed to give 49 kg of acid pretreated seaweed. This acid pretreated seaweed was mixed with 150 kg of a 0.25% sodium hypochlorite solution, stirred at 60 rpm for 45 minutes, then the sodium hypochlorite solution was removed and washed with 100 kg of water. Water was removed to give 48 kg of pretreated seaweed. The pretreated seaweed was pale yellow with red impurities of 0.4% or less and sulfate content of 0.5% or less.

The pretreated seaweed was mixed with 150 kg of a 220 U / g acidic cellulase solution, adjusted to pH 6.0, heated, and stirred at 60 ° C. and 60 rpm for 1.5 hours. The cellulase solution was removed and the seaweed was washed with 100 kg of water. 46 kg of cellulase-treated seaweed was obtained.

The treated seaweed was mixed with 46 kg of water and processed using a HAAKE Process 11 parallel twin-screw extruder at a set heating temperature of 135 ° C. Then, the extruded seaweed was dried and crushed to obtain 3.8 kg of seaweed powder.

Example 10 Production of seaweed powder from dried Gracilaria 10 kg of dried Gracilaria and 150 kg of water were mixed in a tank and stirred at 60 rpm for 30 minutes to wash the seaweed. Water was removed to obtain 58 kg of clean seaweed. This treated seaweed was light brown with 0.8% or less of red impurities. Then, the seaweed was dried and pulverized to obtain 6.2 kg of seaweed powder.

Example 11 Analysis of Seaweed Powder Table 2 summarizes the treatment methods of Examples 2 to 10 for producing various seaweed powders.

The gel strength was measured as follows. 3.0 g of dried seaweed powder and 197 g of distilled water were mixed in a pre-weighed beaker. The mixture was heated in a water bath at 90 ° C. for 30 minutes with gentle stirring using a spoon until the seaweed powder was dissolved in distilled water. The watery gel was cooled at room temperature for 3 hours. The beaker containing the gel was placed in a constant temperature bath at 20 ° C. and stored for at least 20 hours before measuring the gel strength. The gel strength was measured with TXAT2i (texture analyzer).

The melting point and gelation temperature were measured as follows. 2 g of the sample and 200 ml of deionized water were mixed. The gelation temperature and melting point were measured using the Anton Paar MCR301 rheometer with the following settings.
1. 1. Temperature rise rate: 2 ° C / min, 0.4Hz, 1%,
2. Stabilization: 15 minutes, 0.4 Hz, 1%,
3. 3. Cooling rate: 2 ° C / min, 0.4Hz, 1%,
4. Stabilization: 15 minutes, 0.4 Hz, 1%.

The sulfate test was performed as follows. 100 mg of the sample was dissolved in 20 ml of water (heated if necessary), and 3 ml of the barium chloride test solution and 5 ml of hydrochloric acid were added. The test solution was diluted and filtered if a precipitate formed. The solution or filtrate was boiled for 5 minutes. A white crystal precipitate was observed.

The soluble dietary fiber content of the sample was measured by the method specified by AOAC. See, for example, AOAC985.29 and AOAC991.43. The protein content of the sample was measured by the Kjeldahl method published as ISO 20483: 2006.

The results of the basic analysis of the seaweed powder samples 1 to 9 obtained in Examples 2 to 10 are summarized in Table 3 in comparison with commercially available seaweed powder and agar.

Sample 10 is a commercially available Gracilaria seaweed powder obtained from Viet Delta Industrial Company Limited (manufactured by washing with water, drying and crushing into powder), and Sample 11 is a commercially available product obtained from the Green-Fresh Group. Both were used as controls in the analysis. Sample 9 prepared by a conventional method was also used as a control. Samples 2 and 6 gave the best results in various tests. Samples 1, 3, 4, 5, 7 and 8 also gave acceptable results in various tests.

The results of typical Fourier transform infrared spectroscopy (FTIR) of Sample 2 are shown in FIG. 1 in comparison with Sample 10 which is a commercially available seaweed powder and Sample 11 which is a commercially available agar. The spectrum of about 890 cm ^-1 is mainly related to the CH expansion and contraction of the anomeric carbon of the β-galactose residue. A strong band of 930 cm- ¹ indicates the presence of 3,6-anhydro-D-galactose. 1550 to 1510 cm- ¹ is the NH stretch (amide band II) of the protein. In short, FTIR obtained a seaweed powder having a low protein content and a large 3,6-anhydro-D-galactose content as compared with commercially available seaweed powder and agar by the method described herein. Is shown.

Example 12 Use of seaweed powder in the preparation of agitated yogurt Samples 1 to 4 and 6 to 9 of the seaweed powder prepared by the above method were used for the preparation of agitated yogurt. Sample 10 which is a commercially available seaweed powder and sample 11 which is a commercially available agar were used as controls. The sample or control is dry mixed with sugar, the mixture is dispersed in milk at 50-60 ° C. and stirred for 15 minutes, the target weight of water is added, homogenized at 65-68 ° C., 180/50 bar and at 95 ° C. Pasteurize for 5 minutes, cool to 43 ° C, add inoculum, incubate until pH reaches 4.6, smooth the mixture and post-ferment, refrigerate to 4 ° C to produce agitated yogurt. ..

The yogurt ingredients are shown in Table 4.

The viscosity and pH of each yogurt were measured immediately after production. A sensory test was also performed. In addition, yogurt was observed after storage for 10 and 20 days. Details of the test results are shown in Table 5.

There was no significant difference in the final pH of all yogurts. The yogurt made from the seaweed powder of Samples 2 and 6 had the highest viscosity and was close to the yogurt made from Sample 11, which is a commercially available agar. The viscosity of the yogurt made from the seaweed powder of Samples 1, 3, 4, 5, 7 and 8 was lower than that of the yogurt made from Sample 11, but it was still acceptable. The yogurt made from Sample 9 and Sample 10, which is a commercially available seaweed powder, had a lower viscosity than other yogurts. If the viscosity is low, the yogurt will feel lighter. In addition, the yogurts prepared with Samples 9 and 10 had poor water retention as compared with other yogurts, and showed a bitter and sticky feeling.

All yogurts made from the seaweed powder of Samples 1-8 and 11 were stable after 20 days of storage and no water separation was observed after 10 or 20 days of storage. The yogurt made from the seaweed powder of Samples 9 and 10 separated 2 mm of water.

Example 13 Use of seaweed powder in the preparation of set-type yogurt Samples 1 to 4 and 6 to 9 of the seaweed powder produced by the above method were used in the preparation of set-type yogurt. Sample 10 which is a commercially available seaweed powder and sample 11 which is a commercially available agar were used as controls. Dry mix the sample or control with sugar, disperse the mixture in milk at 50-60 ° C., stir for 15 minutes, add target weight of water, homogenize at 65-68 ° C., 180/50 bar, at 95 ° C. Pasteurize for 5 minutes, cool to 43 ° C, store in containers, add inoculum to each container, incubate until pH reaches 4.4, post-ferment, refrigerate to 4 ° C, set yogurt Manufactured. The ingredients are the same as those listed in Table 4 above.

The pH of each yogurt was measured immediately after production. A sensory test and a shear stress test by HAAKE Viscostester were also performed. In addition, yogurt was observed after storage for 10 and 20 days. Details of the test results are shown in Table 6.

The results of the gel shear stress test are shown in order from the highest to the lowest gelling ability of yogurt made from seaweed powder or control: S11> S2> S6> S3> S8> S1> S7> S4> S5> S10> S9. .. Gel strength is represented by the peak value, and brittleness is represented by the passage of time until the peak is reached. The brittleness of all yogurts was similar, but the gel strength was different. The gel strength of S9 made from the seaweed powder of Sample 9 (a sample prepared by a usual method) and S10 made from the seaweed powder of Sample 10 (commercially available seaweed powder) was lower than that of other yogurts.

Further, the yogurt prepared from Sample 9 and Sample 10, which is a commercially available seaweed powder, had an undesired astringency and stickiness, and was inferior in water retention as compared with other yogurts.

All yogurts made from the seaweed powder of Samples 1-8 and 11 were stable after 20 days of storage and no water separation was observed after 10 or 20 days of storage. The yogurt made from the seaweed powder of Samples 9 and 10 was separated from 2 mm and 3 mm of water, respectively.

All yogurts made from the seaweed powder of Samples 1-8 and 11 were stable after 20 days of storage and no water separation was observed after 10 or 20 days of storage. The yogurt made from the seaweed powder of Samples 9 and 10 was separated from 2 mm and 3 mm of water, respectively.
Hereinafter, the scope of claims at the time of filing of the present application will be added as an embodiment.
[1] A method for producing high-quality seaweed powder suitable for food use.
The seaweed material comprises washing the seaweed material with water, said seaweed material being a dry, raw or water rehydrated seaweed material.
The seaweed was pretreated with alkali and
The seaweed is pretreated with acid and
The pretreated seaweed was treated with an enzyme, the enzyme being cellulase,
This gives seaweed powder,
Method.
[2] The method according to [1], further comprising bleaching the seaweed with a bleaching agent before or after the enzyme treatment step.
[3] The ratio of seaweed: bleaching solution in the bleaching step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. 2].
[4] The effective chlorine concentration in the bleaching step is 0.01% to 5%, 0.02% to 3%, 0.05% to 2%, 0.05% to 1% or 0.05% to 0. The method according to [2], which is 5.5% (% by weight).
[5] The method according to [2], wherein the time of the bleaching step is 5 minutes to 240 minutes, 10 minutes to 180 minutes, 10 minutes to 120 minutes, 10 minutes to 60 minutes, or 20 minutes to 60 minutes.
[6] The method according to [2], wherein the bleaching agent is selected from the group consisting of hypochlorous acid, sodium hypochlorite, chlorine dioxide and combinations thereof.
[7] The method according to [1], further comprising processing the treated seaweed material by a twin-screw extrusion process.
[8] The temperature of the twin-screw extrusion process is 70 ° C. to 200 ° C., 80 ° C. to 150 ° C., 100 ° C. to 150 ° C., 100 ° C. to 140 ° C. or 110 ° C. to 130 ° C., according to [7]. the method of.
[9] The method according to [7], wherein the seaweed: water ratio in the twin-screw extrusion treatment is 1: 0 to 1: 5, 1: 1 to 1: 3 or 1: 0 to 1: 2. ..
[10] The method according to [1], further comprising crushing and drying the extruded seaweed.
[11] The method according to [1], wherein the pretreated seaweed has less than 1% of red impurities, less than 0.5% sulfate content, and light brown to light yellow.
[12] The method according to [1], wherein the seaweed material is red algae.
[13] The method according to [1], wherein the seaweed material comprises Gracilaria, Gelidiaceae, Porphyra, Ahnfeltia, or a combination thereof.
[14] The ratio of raw seaweed to water in the washing step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5, 1: 1 to 1:10 or 1: 1. The ratio of seaweed to dried seaweed: water is 1: 1 to 1:40, 1: 3 to 1:30, 1: 5 to 1:25, 1: 5 to 1:20, The method according to [1], which is 1: 10 to 1:20 or 1: 5 to 1:10.
[15] The ratio of seaweed: alkaline solution in the alkaline pretreatment step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. , [1].
[16] The concentration of the alkaline solution in the alkaline pretreatment step is 1% to 10%, 3% to 15%, 5% to 15%, 10% to 20%, 3% to 20% or 10% to 30%. The method according to [1], which is (% by weight).
[17] The method according to [1], wherein the temperature of the alkaline pretreatment step is 40 ° C to 80 ° C, 65 ° C to 95 ° C, 50 ° C to 100 ° C or 70 ° C to 120 ° C.
[18] The time of the alkali pretreatment step is 0.5 hours to 24 hours, 0.5 hours to 20 hours, 0.5 hours to 15 hours, 0.5 hours to 12 hours, 0.5 hours to 8 hours. The method according to [1], wherein the time is 0.5 hours to 6 hours, 1 hour to 4 hours, 1.5 hours to 3 hours or 0.5 hours to 4 hours.
[19] The ratio of seaweed: acid solution in the acid pretreatment step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. , [1].
[20] The concentration of the acid solution in the acid pretreatment step is 0.05% to 5%, 0.1% to 3%, 0.1% to 2%, 0.1% to 1% or 0.1. The method according to [1], which is% to 0.5% (% by weight).
[21] The time of the acid pretreatment step is 5 minutes to 240 minutes, 10 minutes to 180 minutes, 10 minutes to 120 minutes, 10 minutes to 60 minutes, or 20 minutes to 60 minutes, according to [1]. Method.
[22] The method according to [1], wherein the alkali is selected from the group consisting of sodium hydroxide, potassium hydroxide and a combination thereof.
[23] The method according to [1], wherein the acid is selected from the group consisting of hydrochloric acid, nitric acid, phosphoric acid, oxalic acid and combinations thereof.
[24] The ratio of seaweed: enzyme solution in the enzyme treatment step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The method according to [1].
[25] The pH of the enzyme treatment step is 2.0 to 10.0, 3.0 to 9.0, 3.0 to 8.0, 4.0 to 7.0 or 5.0 to 6.0. The method according to [1].
[26] The enzyme concentration in the enzyme treatment step is 10 U / g to 500 U / g, 20 U / g to 400 U / g, 30 U / g to 300 U / g, 50 U / g to 200 U / g or 75 U / g to 150 U /. The method according to [1], which is g.
[27] The temperature of the enzyme treatment step is 15 ° C to 100 ° C, 20 ° C to 90 ° C, 30 ° C to 80 ° C, 20 ° C to 70 ° C, 30 ° C to 60 ° C, 40 ° C to 50 ° C. 1].
[28] The time of the enzyme treatment step is 0.5 hours to 12 hours, 0.5 hours to 8 hours, 0.5 hours to 6 hours, 1 hour to 3 hours, or 1 hour to 4 hours. 1].
[29] The method according to [1], wherein the enzyme is selected from the group consisting of acidic cellulase, neutral cellulase, alkaline cellulase and combinations thereof.
[30] A seaweed powder suitable for food use, produced by the method described in [1].
[31] The seaweed powder according to [30], which contains at least 20% of insoluble dietary fiber.

Claims (31)

A method of producing high quality seaweed powder suitable for food applications.
The seaweed material comprises washing the seaweed material with water, said seaweed material being a dry, raw or water rehydrated seaweed material.
The seaweed was pretreated with alkali and
The seaweed is pretreated with acid and
The pretreated seaweed was treated with an enzyme, the enzyme being cellulase,
This gives seaweed powder,
Method. The method of claim 1, further comprising bleaching the seaweed with a bleaching agent before or after the enzyme treatment step. 2. The ratio of seaweed: bleaching solution in the bleaching step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The method described. The effective chlorine concentration in the bleaching step is 0.01% to 5%, 0.02% to 3%, 0.05% to 2%, 0.05% to 1% or 0.05% to 0.5%. The method according to claim 2, wherein (% by weight). The method according to claim 2, wherein the time of the bleaching step is 5 minutes to 240 minutes, 10 minutes to 180 minutes, 10 minutes to 120 minutes, 10 minutes to 60 minutes, or 20 minutes to 60 minutes. The method according to claim 2, wherein the bleaching agent is selected from the group consisting of hypochlorous acid, sodium hypochlorite, chlorine dioxide and combinations thereof. The method of claim 1, further comprising processing the treated seaweed material by a twin-screw extrusion process. The method according to claim 7, wherein the temperature of the twin-screw extrusion process is 70 ° C. to 200 ° C., 80 ° C. to 150 ° C., 100 ° C. to 150 ° C., 100 ° C. to 140 ° C. or 110 ° C. to 130 ° C. The method according to claim 7, wherein the seaweed: water ratio in the twin-screw extrusion treatment is 1: 0 to 1: 5, 1: 1 to 1: 3 or 1: 0 to 1: 2. The method of claim 1, further comprising crushing and drying the extruded seaweed. The method according to claim 1, wherein the pretreated seaweed contains less than 1% of red seaweed as an impurity, less than 0.5% of sulfate content, and is light brown to light yellow. The method according to claim 1, wherein the seaweed material is red algae. The method according to claim 1, wherein the seaweed material comprises Gracilaria, Gelidiaceae, Porphyra, Ahnfeltia, or a combination thereof. The ratio of raw seaweed to water in the washing step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5, 1: 1 to 1:10 or 1: 1 to 1. : 15 or dry seaweed: water ratios 1: 1 to 1:40, 1: 3 to 1:30, 1: 5 to 1:25, 1: 5 to 1:20, 1:10 The method according to claim 1, wherein the method is ~ 1:20 or 1: 5 to 1:10. The claim that the ratio of the seaweed: alkaline solution in the alkaline pretreatment step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The method according to 1. The concentration of the alkaline solution in the alkaline pretreatment step is 1% to 10%, 3% to 15%, 5% to 15%, 10% to 20%, 3% to 20% or 10% to 30% (weight%). ), The method according to claim 1. The method according to claim 1, wherein the temperature of the alkaline pretreatment step is 40 ° C to 80 ° C, 65 ° C to 95 ° C, 50 ° C to 100 ° C or 70 ° C to 120 ° C. The time of the alkali pretreatment step is 0.5 hours to 24 hours, 0.5 hours to 20 hours, 0.5 hours to 15 hours, 0.5 hours to 12 hours, 0.5 hours to 8 hours, 0. The method of claim 1, wherein the method is 5 hours to 6 hours, 1 hour to 4 hours, 1.5 hours to 3 hours or 0.5 hours to 4 hours. The claim that the ratio of the seaweed: acid solution in the acid pretreatment step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The method according to 1. The concentration of the acid solution in the acid pretreatment step is 0.05% to 5%, 0.1% to 3%, 0.1% to 2%, 0.1% to 1% or 0.1% to 0. The method according to claim 1, which is 5.5% (% by weight). The method according to claim 1, wherein the time of the acid pretreatment step is 5 minutes to 240 minutes, 10 minutes to 180 minutes, 10 minutes to 120 minutes, 10 minutes to 60 minutes, or 20 minutes to 60 minutes. The method of claim 1, wherein the alkali is selected from the group consisting of sodium hydroxide, potassium hydroxide and combinations thereof. The method of claim 1, wherein the acid is selected from the group consisting of hydrochloric acid, nitric acid, phosphoric acid, oxalic acid and combinations thereof. Claim 1 in which the ratio of seaweed: enzyme solution in the enzyme treatment step is 1: 1 to 1: 3, 1: 1 to 1: 5, 1: 2 to 1: 5 or 1: 1 to 1:10. The method described in. The pH of the enzyme treatment step is 2.0 to 10.0, 3.0 to 9.0, 3.0 to 8.0, 4.0 to 7.0 or 5.0 to 6.0. The method according to claim 1. The enzyme concentration in the enzyme treatment step is 10 U / g to 500 U / g, 20 U / g to 400 U / g, 30 U / g to 300 U / g, 50 U / g to 200 U / g or 75 U / g to 150 U / g. , The method according to claim 1. The temperature of the enzyme treatment step is 15 ° C. to 100 ° C., 20 ° C. to 90 ° C., 30 ° C. to 80 ° C., 20 ° C. to 70 ° C., 30 ° C. to 60 ° C., 40 ° C. to 50 ° C., claim 1. The method described. According to claim 1, the time of the enzyme treatment step is 0.5 hours to 12 hours, 0.5 hours to 8 hours, 0.5 hours to 6 hours, 1 hour to 3 hours, or 1 hour to 4 hours. The method described. The method of claim 1, wherein the enzyme is selected from the group consisting of acidic cellulase, neutral cellulase, alkaline cellulase and combinations thereof. A seaweed powder suitable for food use, produced by the method according to claim 1. The seaweed powder according to claim 30, which contains at least 20% insoluble dietary fiber.

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