KR100367722B1 - Manufacture of water soluble low-molecular alginates by ultrasonication pretreatment and hot water extraction - Google Patents
Manufacture of water soluble low-molecular alginates by ultrasonication pretreatment and hot water extraction Download PDFInfo
- Publication number
- KR100367722B1 KR100367722B1 KR10-2000-0016011A KR20000016011A KR100367722B1 KR 100367722 B1 KR100367722 B1 KR 100367722B1 KR 20000016011 A KR20000016011 A KR 20000016011A KR 100367722 B1 KR100367722 B1 KR 100367722B1
- Authority
- KR
- South Korea
- Prior art keywords
- alginic acid
- extraction
- hot water
- pretreatment
- water
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
Abstract
본 발명은 알긴산 제조공정중의 산, 알칼리 처리와 같은 공정 대신에 초음파 처리와 열수추출만을 행하여 공정을 획기적으로 단축 시키고, 아울러 알긴산의 점도를 낮추고, 분자량이 작은 가용성 알긴산을 제조하는 것으로, 냉수에 쉽게 용해되며, 저점도의 특성을 가지고 있어서 다양한 가공 식품에 첨가물로서 뿐만 아니라, 그 자체로서 기능성 물질의 소재로 이용이 가능할 것으로 판단된다.In the present invention, instead of the acid and alkali treatment in the alginic acid production process, only ultrasonic treatment and hot water extraction are performed to shorten the process drastically, lower the viscosity of the alginic acid, and produce soluble alginic acid having a low molecular weight. It is easily dissolved and has a low viscosity, so it can be used not only as an additive to various processed foods, but also as a material of functional materials.
Description
본 발명은 미역과 다시마로부터 초음파 전처리와 열수 추출로 저점도 및 저 분자량의 알긴산의 제조 방법에 관한 것이다. 기존에 행해지고있는 알긴산 제조 방법은 알칼리 용액 중에서 가온하여 알긴산을 추출하는 것으로 전처리로 산처리의 유무라든지 알칼리 처리 농도를 달리 하거나 가열 조건을 달리하여 만든 나트륨형(Na 형) 알긴산이 대부분이다. 일반적으로 알긴산의 제조공정은 탄산나트륨 처리에의한 알칼리 추출 공정으로 거의 일반화 되어있고, 알긴산 제조 기술은 크게 진보나 변화된 바 없는 상태이다.The present invention relates to a method for producing low viscosity and low molecular weight alginic acid by ultrasonic pretreatment and hot water extraction from seaweed and kelp. Conventional alginic acid production methods are the extraction of alginic acid by heating in an alkaline solution, most of which are sodium-type (Na-type) alginic acid made by pre-treatment with or without acid treatment, or by varying the concentration of alkali treatment or different heating conditions. In general, the alginic acid production process is almost generalized to the alkali extraction process by sodium carbonate treatment, the alginic acid production technology has not been greatly advanced or changed.
알긴산은 알칼리성 용액에서 쉽게 용해되므로 대게 탄산나트륨과 같은 알칼리성 용액으로 추출한다. 이런 조건하에서 제조된 알긴산은 대개 나트륨형 알긴산으로 분자량은 수십만에서 수백만으로 매우 다양하며, 대체적으로 강한 점성을 가진다. 이렇게 제조된 일긴산은 상온에서 용해하는데는 많은 시간이 소요되며, 알콜성 용액에서는 침전하는 특성이 있다. 또한 알긴산 농도가 높아질수록 강한 점성을 가지게되며, 이런 특성은 알긴산이용의 제약점이 되고있다. 또한 알긴산 제조중에 산처리, 알칼리처리, 수세처리등의 과정을 거치면서 많은 공해요소를 유발 시키고 있으며, 공정 및 소요 시간도 매우 길어 제품의 단가가 높아지는 단점을 가지고 있다.Alginic acid is readily soluble in alkaline solutions, so it is usually extracted with an alkaline solution such as sodium carbonate. Alginic acid prepared under these conditions is usually sodium alginic acid, which varies in molecular weight from hundreds of thousands to millions, and has a generally strong viscosity. Ilgin acid thus prepared takes a long time to dissolve at room temperature, and precipitates in an alcoholic solution. In addition, the higher the alginic acid concentration has a stronger viscosity, which is a limitation of the use of alginic acid. In addition, alginic acid during the manufacturing process, such as acid treatment, alkali treatment, washing process, causing a lot of pollution factors, and the process and the time required is very long, the cost of the product has a disadvantage.
따라서 본 발명에서는 알긴산 제조 공정중의 산, 알칼리 처리와 같은 공정 대신에 초음파 전처리와 열수추출만을 행하여 공정을 단축시키고, 아울러 저점도 알긴산과 분자량이 적은 냉수 가용성 알긴산을 제조하는데 목적이 있다.Accordingly, the present invention aims to shorten the process by performing only ultrasonic pretreatment and hot water extraction instead of the acid and alkali treatment in the alginic acid production process, and to prepare low viscosity alginic acid and cold water soluble alginic acid having a low molecular weight.
도 1은 초음파 전처리에의한 알긴산 제조공정을 나타낸 것이다.1 shows an alginic acid production process by ultrasonic pretreatment.
1) 알긴산 제조공정1) Alginic acid manufacturing process
초음파 전처리를 이용한 알긴산의 추출은 건조원조분말(수분함량 12-14%)에 75배량(w/v)의 증류수를 가한 후 일정시간(30min) 방치한 후, 20-50℃, 30-120분 초음파 전처리한 다음, 동일량의 증류수를 가한다음, 95℃ 항온수조에서 60분간 교반 추출을 행한다. 추출된 반응액을 여과(celite 545)나 원심분리(5,000rpm, 10min)하여 얻어진 추출액에 메탄올을 첨가하여 알긴산을 침전시켜 회수하고 수세Extraction of alginic acid using ultrasonic pretreatment was performed by adding 75 times (w / v) of distilled water to dry aid powder (water content of 12-14%), and then leaving it for a certain time (30 min), then 20-50 ° C. and 30-120 minutes. After ultrasonic pretreatment, the same amount of distilled water was added, followed by stirring extraction for 60 minutes in a 95 ° C. constant temperature water bath. The extracted reaction solution was filtered (celite 545) or centrifuged (5,000 rpm, 10 min), and methanol was added to the extracted solution to precipitate and recover alginic acid.
후 건조하여 최종 알긴산 제품으로 한다. 제조공정은 그림 1과 같다.It is then dried to obtain a final alginic acid product. The manufacturing process is shown in Figure 1.
2) 초음파 전처리 조건에 따른 알긴산 추출2) Alginic Acid Extraction According to Ultrasonic Pretreatment Conditions
초음파 전처리에의한 알긴산 추출과정을 정리하면, 분말원조 2g(수분함량 12-14%)에 증류수 150ml를 가하여, 초음파 처리 온도를 25℃, 50℃의 두 구간을 설정하고, 시긴을 30, 60 및 120분으로하여 초음파(VCX 600) 처리 하였을 때의 결과를 표 1에 정리하였다. 미역과 다시마 모두 초음파 처리온도에 따른 수율 및 용해도의 차이는 거의 없었으며, 점도는 다시마의 경우 50℃ 처리 조건이 높은 값을 보였다. 용해도는 실험조건에 관계없이 대조 실험인 탄산 나트륨 추출구 70-85%에 비해 76-91%로 높았다. 초음파 처리 온도는 별 영향을 미치지 못한 반면, 처리 시간이 길어질수록 용해도는 약간씩 증가하는 경향을 나타내었으나, 그 정도는 크지 않았다. 결구 초음파 처리는 온도에 관계없이 60분 이상 초음파 처리를 행하면 알긴산의 추출 수율이나 용해도 및 점도와 같은 물성에 큰 영향을 미치지 않는 것으로 나타났다. 따라서 초음파 처리 조건은 25℃에서 60분 전처리하는 조건으로 결정하였다.After arranging the extraction process of alginic acid by ultrasonic pretreatment, 150 ml of distilled water was added to 2 g of powder aid (water content of 12-14%), and the ultrasonic treatment temperature was set at 25 ° C and 50 ° C. Table 120 summarizes the results of the ultrasonic wave treatment (VCX 600) at 120 minutes. There was little difference in yield and solubility according to sonication temperature in seaweed and kelp, and the viscosity of kelp was 50 ℃. Solubility was 76-91% higher than 70-85% of sodium carbonate extract, which was a control experiment regardless of experimental conditions. While the sonication temperature had little effect, the solubility tended to increase slightly as the treatment time increased, but not so much. The sonication of the catheter did not significantly affect the physical properties such as extraction yield, solubility, and viscosity of alginic acid after 60 minutes of sonication regardless of temperature. Therefore, the ultrasonic treatment conditions were determined under the conditions of pretreatment at 25 ° C. for 60 minutes.
초음파 처리온도(℃): A-25℃, B-50℃Ultrasonication temperature (℃): A-25 ℃, B-50 ℃
2) 열수추출 조건에 따른 알긴산 추출2) Alginic Acid Extraction According to Hot Water Extraction Conditions
초음파 전처리된 시료에 동량의 증류수를 가한 다음, 열수 추출 조건을 달리하면서 알긴산 추출 수율, 용해도 및 점도 등의 특성을 측정한 결과 표 2와 같다. 60, 80 및 95℃의 온도 조건하에서 추출시간을 달리하면서 추출한 결과, 추출시간에 따른 수율 차이는 크지 않았으며, 추출 온도별 추출 수율은 큰 차이가 있다는 것을 알 수 있다. 특히 60℃와 95℃와의 차이는 약 9-9.5%로 2배정도 수율에 차이가 있다는 것을 알 수 있다. 80℃ 온도 조건에서도 큰 수율의 증가가 없는 것으로보아 초음파 전처리에의한 알긴산 추출은 특정온도 이상에서 추출 처리되어야함을 알 수 있었는데, 본 연구의 결과로는 95℃ 조건에서는 30분 처리나 60분 처리가 거의 차이가 없는 것으로 보아 이 온도 조건하에서는 30분 처리로도 알긴산 추출에는 문제가 없었다. 동일한 조건에서 추출처리된 미역과 다시마 사이에는 수율에 큰 차이를 보였으며, 특히 95℃ 온도 조건에서는 2배정도의 수율 차이를 보였다. 이러한 결과는 미역과 다시마가 가지고 있는 원료의 구조적 측면과 추출 처리후 알긴산 및 기타 다당류의 존재 형상에 따라 제조 과정중 손실등의 이유로 차이가 큰 것으로 여겨졌다. 이상의 결과는 초음파 전처리후 열처리 조건이 알긴산 추출 수율을 결정하는 요소이며, 원료의 성상에 따른 차이도 크다는 것이 확인 되었다.The same amount of distilled water was added to the ultrasonic pretreated sample, and the characteristics of alginic acid extraction yield, solubility and viscosity were measured while varying the hot water extraction conditions. As a result of extracting with different extraction time under temperature conditions of 60, 80 and 95 ℃, the yield difference according to the extraction time was not large, it can be seen that the extraction yield for each extraction temperature has a big difference. In particular, the difference between 60 ℃ and 95 ℃ is about 9-9.5% can be seen that there is a difference in yield about twice. Alginic acid extraction by ultrasonic pretreatment should be extracted above a certain temperature, as there is no significant increase in yield even at 80 ℃. As a result of this study, 30 minutes or 60 minutes at 95 ℃ Since the treatment showed little difference, there was no problem in the extraction of alginic acid even after 30 minutes of treatment under these temperature conditions. Under the same conditions, the yields of seaweed and kelp extracted were significantly different, especially at 95 ° C. These results were considered to be different due to structural loss of seaweed and kelp and the loss of alginic acid and other polysaccharides after extraction. The above results confirmed that the heat treatment condition after the ultrasonic pretreatment is a factor for determining the yield of alginic acid extraction, and the difference according to the properties of the raw material is also confirmed.
추출시간(min): A- 30분, B- 60분Extraction time (min): A-30 minutes, B-60 minutes
3) 추출된 알긴산의 분자량3) Molecular weight of extracted alginic acid
상기한 초음파 전처리 및 열수 추출방법, 기존의 탄산나트륨 추출방법과 시판제품 분자량을 측정한 결과는 표3과 같다.The result of measuring the ultrasonic pretreatment and hot water extraction method, conventional sodium carbonate extraction method and the commercial product molecular weight is shown in Table 3.
시판되고있는 알긴산의 경우, 제품 종류에 따라 차이는 있지만 대개 분자량이 100만 이상인 것으로 알려져 있고, 본 연구에서도 기존의 탄산나트륨을 이용한 추출법으로 제조된 알긴산의 분자량이 80만을 넘는 것으로 측정되었다. 본 발명의 초음파 전처리 및 열수 추출한 알긴산의 경우는 분자량이 이들 물리적 처리조건의 경우보다도 훨씬 작았는데, 미역을 원료로 제조한 알긴산은 180,000-200,000 정도 였으며, 다시마를 원료로한 알긴산은 320,000-380,000 정도였다. 이러한 결과는 초음파 전처리를 통해 제조된 알긴산은 탄산나트륨을 이용해 제조한 알긴산이 가지는 물성적 특성을 어느정도 유지하면서 분자량이 작은 저분자 알긴산이라는 사실을 확인할 수 있었다.Commercially available alginic acid is known to have a molecular weight of more than 1 million, although there are differences depending on the type of product, and in this study, the molecular weight of alginic acid prepared by the extraction method using sodium carbonate was measured to be over 800,000. In the case of the alginate extracted by ultrasonic pretreatment and hydrothermal extraction of the present invention, the molecular weight was much smaller than those of these physical treatment conditions. Alginate prepared from seaweed was about 180,000-200,000, and alginate based on kelp was about 320,000-380,000. It was. These results confirm that alginic acid prepared by ultrasonic pretreatment is a low molecular weight alginic acid having a small molecular weight while maintaining some of the physical properties of alginic acid prepared using sodium carbonate.
본 발명은 탄산나트륨을 이용하는 복잡한 제조 공정을 단축할 수 있고, 저분자 이면서 저점도로 냉수에 쉽게 녹는 수용성알긴산 이라는 것과, 나트륨이 붙어있지않은 알긴산으로 기존의 알긴산이 가지고 있는 나트륨 때문에 사용이 될 수 없었던 분야까지 알긴산의 이용 범위를 크게 넓힐 수 있는 발명이라는 점에서 용도 개발이 적절하게 이루어 진다면 경제성이 있는 고효율의 알긴산이 될 수 있다.The present invention can shorten the complicated manufacturing process using sodium carbonate, and it is water-soluble alginic acid that is easily dissolved in cold water with low molecular weight and low viscosity, and alginate without sodium attached to the field that could not be used because of the sodium of alginic acid. In view of the invention that can greatly expand the range of use of alginic acid can be a high efficiency alginic acid with economical efficiency if the application development is made properly.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2000-0016011A KR100367722B1 (en) | 2000-03-29 | 2000-03-29 | Manufacture of water soluble low-molecular alginates by ultrasonication pretreatment and hot water extraction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2000-0016011A KR100367722B1 (en) | 2000-03-29 | 2000-03-29 | Manufacture of water soluble low-molecular alginates by ultrasonication pretreatment and hot water extraction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20010093417A KR20010093417A (en) | 2001-10-29 |
| KR100367722B1 true KR100367722B1 (en) | 2003-01-14 |
Family
ID=19659554
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR10-2000-0016011A KR100367722B1 (en) | 2000-03-29 | 2000-03-29 | Manufacture of water soluble low-molecular alginates by ultrasonication pretreatment and hot water extraction |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR100367722B1 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020011842A (en) * | 2000-08-04 | 2002-02-09 | 박권필 | Alginic Acid Extraction from Seaweed |
| KR100678591B1 (en) * | 2005-03-29 | 2007-02-02 | 윤광섭 | Extraction method of Acanthopanax senticosus |
| CN103333271B (en) * | 2013-07-31 | 2015-09-09 | 青岛海之林生物科技开发有限公司 | A kind of production method of high-quality calcium alginate |
| CN105754011B (en) * | 2016-03-21 | 2018-01-30 | 青岛海之林生物科技开发有限公司 | A kind of preparation technology of water soluble algae acid |
| KR102013268B1 (en) * | 2019-02-13 | 2019-08-22 | (주)클래시스 | Method for preparing laminaria japonica extract using focused ultrasonic treatment, and laminaria japonica extract obtained therefrom |
| KR102416674B1 (en) * | 2020-07-13 | 2022-07-05 | 주식회사 씨위드 | Method of Extracting alkali-soluble alginate from Brown Seaweed by using surfactant-treatment |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3773753A (en) * | 1972-01-10 | 1973-11-20 | Kelco Co | Process for production of alginates |
| JPS6351401A (en) * | 1986-08-19 | 1988-03-04 | Nichiden Kagaku Kk | Production of polysaccharides |
| KR920000242A (en) * | 1990-06-05 | 1992-01-29 | 테트라베르케 독토르 데어 나트르빈센샤프덴 울리히 벤쉬 게엠베하 | Medicinal feed for systemic treatment of external parasites and external bacterial diseases of fish |
| JPH05178751A (en) * | 1991-04-27 | 1993-07-20 | Lab Andromaco Sa | Preparation of polymer having activity to hematopoietic system |
| KR0173167B1 (en) * | 1995-12-22 | 1999-02-01 | 신철주 | Process for purifyng the water soluble carbohydrate from opuntia |
| KR100192601B1 (en) * | 1996-03-14 | 1999-06-15 | 손송남 | Extracting process of sea tangle`s extract |
| KR19990069029A (en) * | 1998-02-04 | 1999-09-06 | 김공수 | Water-soluble low molecular chitin, chitosan and oligosaccharides thereof |
| KR20000012173A (en) * | 1999-03-26 | 2000-03-06 | 김공수 | Method of manufacturing polysaccharites having low molecular weight and oligosaccharites |
-
2000
- 2000-03-29 KR KR10-2000-0016011A patent/KR100367722B1/en not_active IP Right Cessation
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3773753A (en) * | 1972-01-10 | 1973-11-20 | Kelco Co | Process for production of alginates |
| JPS6351401A (en) * | 1986-08-19 | 1988-03-04 | Nichiden Kagaku Kk | Production of polysaccharides |
| KR920000242A (en) * | 1990-06-05 | 1992-01-29 | 테트라베르케 독토르 데어 나트르빈센샤프덴 울리히 벤쉬 게엠베하 | Medicinal feed for systemic treatment of external parasites and external bacterial diseases of fish |
| JPH05178751A (en) * | 1991-04-27 | 1993-07-20 | Lab Andromaco Sa | Preparation of polymer having activity to hematopoietic system |
| KR0173167B1 (en) * | 1995-12-22 | 1999-02-01 | 신철주 | Process for purifyng the water soluble carbohydrate from opuntia |
| KR100192601B1 (en) * | 1996-03-14 | 1999-06-15 | 손송남 | Extracting process of sea tangle`s extract |
| KR19990069029A (en) * | 1998-02-04 | 1999-09-06 | 김공수 | Water-soluble low molecular chitin, chitosan and oligosaccharides thereof |
| KR20000012173A (en) * | 1999-03-26 | 2000-03-06 | 김공수 | Method of manufacturing polysaccharites having low molecular weight and oligosaccharites |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20010093417A (en) | 2001-10-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8110677B2 (en) | Microwave-assisted extraction of polysaccharide from Artemisia sphaerocephala | |
| JP6225321B1 (en) | Method for producing polysulfate pentosan | |
| CN110845634B (en) | Polysaccharide extract in oil-tea camellia seed cake and extraction method thereof | |
| US4224219A (en) | Method for producing water soluble corn protein derivatives by reacting with alkylene oxide | |
| CN102532294A (en) | Method for extracting zein | |
| CN105544265A (en) | Method for separating and extracting cellulose and lignin from bamboo wood | |
| KR100367722B1 (en) | Manufacture of water soluble low-molecular alginates by ultrasonication pretreatment and hot water extraction | |
| JP7141774B2 (en) | Method for preparing purified solution of poplar xylooligosaccharide, purified solution of poplar xylooligosaccharide prepared by the method, solid xylooligosaccharide and use thereof | |
| Jacquemin et al. | Comparison of different twin-screw extraction conditions for the production of arabinoxylans | |
| CN106480128B (en) | Method for improving efficiency of cellulose in hydrolyzing rice straws by using lactic acid and guanidine hydrochloride | |
| Fišerová et al. | Hemicelluloses extraction from beech wood with water and alkaline solutions | |
| CN109181352B (en) | Method for modifying black sesame melanin into water-soluble melanin | |
| RU2322456C1 (en) | Method for preparing pectin | |
| KR100367716B1 (en) | Manufacture of water soluble low-molecular alginate by autoclaving pretreatment and hot water extraction | |
| FI66429C (en) | FOERFARANDE FOER PRODUKTION AV GLUKOS FRAON CELLULOSA-MATERIALSOM INNEHAOLLER HEMICELLULOSA OCH LIGNIN | |
| US2638470A (en) | Process for the production of alginic acid sulfate | |
| KR100367721B1 (en) | Manufacture of water soluble low-molecular alginate by microwave pretreatment and hot water extraction | |
| CN106632699A (en) | Preparation method of high-transparency hydroxy ethyl cellulose (HEC) | |
| KR20100059306A (en) | Method for processing ginseng | |
| Jackson et al. | The use of bacteriophage-mediated depolymerisation in investigations of the structure of the capsular polysaccharide from klebsiella serotype K71 | |
| JPS645041B2 (en) | ||
| CN112538050A (en) | Preparation method of cellulose solution | |
| KR100457444B1 (en) | PROCESS FOR THE PREPARATION OF β-CHITOSANS FROM SQUID CARTILAGES | |
| JP2007097466A (en) | Method for producing n-acetyl-d-glucosamine by enzymatic hydrolysis | |
| Wolf et al. | Depolymerization of hemicelluloses utilizing hydrothermal and acid catalyzed processes proceed by ultrafiltration as fractionation media |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E902 | Notification of reason for refusal | ||
| E701 | Decision to grant or registration of patent right | ||
| GRNT | Written decision to grant | ||
| FPAY | Annual fee payment |
Payment date: 20091127 Year of fee payment: 8 |
|
| LAPS | Lapse due to unpaid annual fee |