KR19990064740A - Production of Polysaccharides by the Extrusion Process - Google Patents

Production of Polysaccharides by the Extrusion Process Download PDF

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KR19990064740A
KR19990064740A KR1019990016100A KR19990016100A KR19990064740A KR 19990064740 A KR19990064740 A KR 19990064740A KR 1019990016100 A KR1019990016100 A KR 1019990016100A KR 19990016100 A KR19990016100 A KR 19990016100A KR 19990064740 A KR19990064740 A KR 19990064740A
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polysaccharide
present
apple
peel
pectin
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KR1019990016100A
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Korean (ko)
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황재관
김종태
김철진
변유량
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황재관
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Abstract

본 발명은 이축 압출성형기를 이용한 다당류의 제조방법에 관한 것이다. 좀 더 구체적으로, 본 발명은 단시간 고온 처리에 의한 가열 효과뿐 만 아니라, 고압 및 강한 전단력(sheer force)을 수반하는 압출성형 공정에 의하여, 사과박, 감귤류 껍질, 해조류 등으로부터 식물 세포벽을 형성하는 펙틴(pectin), 알지네이트(alginate), 카라기난(carrageenan) 등의 다당류 성분을 수용화함으로써 다당류를 제조하는 방법에 관한 것이다. 본 발명의 압출성형기를 이용한 다당류의 제조방법에 의하면, 사과박, 감귤류 껍질, 해조류 등을 L/D비(length:diameter ratio) 20 내지 40의 이축압출성형기를 이용하여 스크류속도 150 내지 400 rpm, 시료투입속도 20 내지 50 kg/hr, 수분함량 15 내지 40%으로 유지하면서 압출시키는 공정; 압출성형된 원료를 증류수에 1 내지 10%(w/v)의 비율로 넣고 40 내지 80분간 교반한 후, 6,000 내지 9,000×g에서 5 내지 15분간 원심분리하여 상등액을 취하여 여과하는 공정; 전기 여과액에 3 내지 5배 부피의 이소프로판올을 넣고 3 내지 5시간 동안 방치하여 얻은 침전물을 이소프로판올과 아세톤으로 세척하고 상온에서 건조시키는 공정을 포함하는 제조방법에 의하여 다당류를 제조한다. 본 발명에 의하면 사과박, 감귤류 껍질, 해조류 등의 구성 다당류인 펙틴, 알긴산, 카라기난등을 수용화함으로써, 종래의 산 및 알칼리에 의한 화학적인 추출법이 갖는 많은 문제점을 해결할 수 있는 다당류의 제조방법을 제공한다.The present invention relates to a method for producing a polysaccharide using a twin screw extrusion machine. More specifically, the present invention provides a method for forming plant cell walls from apple peel, citrus peel, algae, and the like by an extrusion process involving high pressure and strong shear force as well as heating effect by a short time high temperature treatment. The present invention relates to a method for producing a polysaccharide by solubilizing a polysaccharide component such as pectin, alginate, carrageenan, and the like. According to the production method of the polysaccharide using the extruder of the present invention, the apple speed, citrus peel, seaweed and the like using a biaxial extrusion molding machine having a L / D ratio (length: diameter ratio) of 20 to 40 screw speed of 150 to 400 rpm, Extruding while maintaining at a sample feeding rate of 20 to 50 kg / hr and a water content of 15 to 40%; Adding the extruded raw material to distilled water at a rate of 1 to 10% (w / v), stirring for 40 to 80 minutes, and centrifuging at 6,000 to 9,000 × g for 5 to 15 minutes to take a supernatant and filter it; 3 to 5 times the volume of isopropanol in the filtrate and the precipitate obtained by leaving for 3 to 5 hours to prepare a polysaccharide by a method comprising the step of washing with isopropanol and acetone and drying at room temperature. According to the present invention, by accepting pectin, alginic acid, carrageenan, etc., which are constituent polysaccharides such as apple peel, citrus peel, seaweed, and the like, a method of preparing a polysaccharide capable of solving many problems of the conventional chemical extraction by acid and alkali is provided. to provide.

Description

압출성형기를 이용한 다당류 생산기술{Production of Polysaccharides by the Extrusion Process}Production technology of polysaccharides using extrusion machine {Production of Polysaccharides by the Extrusion Process}

본 발명은 압출성형기를 이용한 다당류의 제조방법에 관한 것이다. 좀더 구체적으로, 본 발명은 단시간 고온 처리에 의한 가열 효과뿐만 아니라, 고압 및 강한 전단력(sheer force)을 수반하는 압출성형 공정에 의하여, 사과박, 감귤류 껍질, 해조류 등으로부터 식물 세포벽을 형성하는 펙틴(pectin), 알지네이트 (alginate), 카라기난(carrageenan)등의 다당류 성분을 수용화하므로써 다당류을 제조하는 방법에 관한 것이다The present invention relates to a method for producing a polysaccharide using an extrusion molding machine. More specifically, the present invention provides a pectin for forming a plant cell wall from apple foil, citrus peel, algae, etc. by an extrusion process involving high pressure and strong shear force, as well as heating effect by a short time high temperature treatment. The present invention relates to a method for preparing polysaccharides by accepting polysaccharide components such as pectin, alginate, and carrageenan.

펙틴, 알지네이트, 카라기난 등의 다당류는 물에 용해되어 콜로이드(colloid)성질을 갖는 물질로서, 식품, 화장품, 약품 등에서 증점제(thickening agent), 겔화제(gelling agent), 안정화제(stabilizing agent)로서 광범위하게 사용하는 생고분자(biopolymer)이다. 이들은 과채류 및 해조류의 세포벽을 구성하며 자연적으로는 성분간에 강하게 결합되어 있어 불용성 상태로 존재한다(참조:한국영양식량학회지, 23(2):358-370(1994)). 따라서 이들은 고온하에서 산용액이나 알칼리 용액을 가하여 수용화하여 추출하여 왔다. 이와 같은 화학적인 추출방법은, 수율을 높이는 데는 유용하나, 화학적 처리에 따른 폐수의 다량 발생, 용기의 부식, 생산고분자 물질의 분해에 따른 기능성 저하, 추출잔사의 재활용 불가능 등 여러 가지 산업적 문제점을 노출 시켜 왔다.Polysaccharides such as pectin, alginate, and carrageenan are colloidal substances that are dissolved in water, and are widely used as thickening agents, gelling agents, and stabilizing agents in food, cosmetics, and pharmaceuticals. Biopolymer is used. They constitute the cell walls of fruit and seaweeds and are naturally insoluble because of their strong binding between components (see Korean Journal of Nutrition and Nutrition, 23 (2): 358-370 (1994)). Therefore, they have been extracted by solubilizing by adding an acid solution or an alkaline solution at high temperature. Such chemical extraction methods are useful for increasing yields, but they expose various industrial problems such as the generation of large amounts of wastewater by chemical treatment, corrosion of containers, deterioration of functionality due to decomposition of production polymer materials, and the inability to recycle the extraction residues. Has been made.

한편, 압출성형기는 혼합, 가압, 성형, 건조, 살균, 냉각 등의 여러 단위 공정을 단일 기종에 의하여 수행할 수 있는 장치로서, 작동과정에서 고온, 고압 및 고전단력을 수반하여 각종 식품 및 고분자물질의 가공에 많이 사용되고 있다. 특히, 전술한 고전단력은 식물 세포벽을 구성하고 있는 다당류성분들의 수용화에 매우 효율적으로 사용될 수 있다. 지금까지 압출성형기는 제면, 시리얼류 등의 가공식품이나 동물사료의 제조에는 많이 사용되어 왔으나, 불용성 식물 세포벽의 수용화 기능을 이용한 다당류 소재의 생산에는 적용되지 않았다.On the other hand, the extrusion molding machine is a device that can perform several unit processes such as mixing, pressurization, molding, drying, sterilization, cooling, etc. by a single model, and various food and polymer materials with high temperature, high pressure, and high shear force during operation. It is used a lot in the processing. In particular, the aforementioned high shear force can be used very efficiently for the reception of polysaccharide components constituting the plant cell wall. Extruders have been widely used in the manufacture of processed foods and animal feeds such as noodle and cereals, but have not been applied to the production of polysaccharide materials using the water solubility of insoluble plant cell walls.

이에, 본 발명자들은 압출성형기를 이용하여, 펙틴, 알지네이트, 카라기난 등의 다당류를 식물세포의 세포벽으로부터 추출함으로써 기존의 화학적 추출방법을 대체할 수 있음을 확인하고, 본 발명을 완성하게 되었다.Thus, the present inventors have confirmed that it is possible to replace the existing chemical extraction method by extracting polysaccharides such as pectin, alginate, carrageenan, etc. from the cell walls of plant cells using an extruder, and completed the present invention.

결국, 본 발명의 주된 목적은 압출성형기를 이용하여 사과박, 감귤류 껍질, 해조류 등의 식물로부터 펙틴, 알지네이트, 카라기난 등의 다당류를 간편하고도 경제적으로 추출하는 방법을 제공하는 것이다.After all, the main object of the present invention is to provide a simple and economical method for extracting polysaccharides such as pectin, alginate, carrageenan from plants such as apple peel, citrus peel, algae, etc. using an extruder.

본 발명의 압출성형 공정에 의한 다당류의 제조방법을 제조공정별로 설명하면 다음과 같다.The manufacturing method of the polysaccharide by the extrusion molding process of the present invention will be described as follows.

사과박, 감귤류 껍질, 해조류 등을 L/D비(length:diameter ratio) 20 내지 40의 이축 압출반응기(twin screw extruder: Buhler Brothers Co. DNDL-40, Swltzerland)에 투입한 후, 스크류속도 150 내지 400 rpm, 시료투입속도 20 내지 50 kg/hr, 수분함량 15 내지 40%로 유지하면서 압출성형시킨다.Apple peel, citrus peel, algae, etc. are introduced into a twin screw extruder (Buller Brothers Co. DNDL-40, Swltzerland) having a length / diameter ratio of 20 to 40, and then the screw speed is 150 to Extrusion is performed while maintaining at 400 rpm, a sample feeding rate of 20 to 50 kg / hr, and a water content of 15 to 40%.

압출성형된 원료를 증류수에 1 내지 10%(w/v)의 비율로 넣고 40 내지 80분간 교반한 후, 6,000 내지 9,000×g에서 5 내지 15분간 원심분리하여 상등액을 취하여 여과한다. 상등액을 여과한 후 여과액의 3 내지 5배 부피의 이소프로판올(isopropanol)을 넣고 3 내지 5시간 동안 방치하여 얻은 침전물을 이소프로판올과 아세톤(acetone)으로 세척한 후 상온에서 건조시켜 다당류를 제조한다.The extruded raw material is put in distilled water at a rate of 1 to 10% (w / v), stirred for 40 to 80 minutes, centrifuged at 6,000 to 9,000 × g for 5 to 15 minutes, and the supernatant is collected and filtered. After filtering the supernatant, 3 to 5 times the volume of isopropanol (isopropanol) of the filtrate was added and left for 3 to 5 hours to wash the precipitate obtained with isopropanol and acetone (acetone) and dried at room temperature to prepare a polysaccharide.

이하, 본 발명을 실시예에 의해 상세히 설명하고자 한다. 이들 실시예는 오로지 본 발명을 설명하기 위한 것으로, 이들 실시예에 의하여 본 발명의 범위가 한정되자 않는다는 것은 본 발명이 속하는 분야에서 통상의 지식을 가진 자들에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in detail by way of examples. These examples are only for illustrating the present invention, it will be apparent to those skilled in the art that the scope of the present invention is not limited by these examples.

실시예 1Example 1

건조 사과박 L/D비(length:diameter ratio) 20의 이축 압출반응기(twin screw extruder: Buhler Brothers Co. DNDL-40, Swltzerland)에 투입한 후, 스크류 속도 250 rpm, 시료투입속도 40 kg/hr, 수분함량 25%로 유지하면서 압출성형시켰다. 압출성형된 사과박 50 g을 증류수 1 L에 넣고 1시간 동안 교반한 후, 6,500×g에서 10분간 원심분리하였다. 그런 다음 상등액을 여과한 후 여과액에 4 L의 이소프로판올(isoproprnol)을 넣고 4시간 동안 방치하여 얻은 침전물을 이소판올과 아세톤(acetone)으로 세척한 후 상온에서 건조시켰다. 이 건조물의 압출성형 사과박에 대한 중량비로 펙틴 생산수율을 측정한 결과, 14.0%로 나타났으며, 분자량을 겔여과 크로마토그래피(gel permeation chromatography)로 측정한 결과 181,000으로 나타났다. 따라서, 압출성형에 의하여 사과박으로부터 펙틴의 추출이 성공적으로 이루질 수 있음을 알 수 있었다.After feeding into a twin screw extruder (twin screw extruder: Buhler Brothers Co. DNDL-40, Swltzerland) with a dry apple foil L / D ratio of 20, a screw speed of 250 rpm and a sample feeding rate of 40 kg / hr The extrusion was carried out while maintaining the moisture content at 25%. 50 g of extruded apple foil was put in 1 L of distilled water, stirred for 1 hour, and centrifuged at 6,500 × g for 10 minutes. Then, after filtering the supernatant, 4 L isopropanol (isoproprnol) was added to the filtrate, and the precipitate obtained by standing for 4 hours was washed with isopanol and acetone (acetone) and dried at room temperature. As a result of measuring the yield of the pectin by weight ratio of the dried apple filament of the dried product, it was found to be 14.0%, and the molecular weight was determined to be 181,000 by gel permeation chromatography. Therefore, it can be seen that extraction of pectin from apple foil can be successfully achieved by extrusion molding.

실시예 2-19Example 2-19

상기 실시예 1과 동일한 사과박 원료와 기계장치를 사용하여, 온도, 스크류 속도, 수분함량 등을 조절하면서 시료를 조제한 후, 이에 따른 펙틴의 생산수율과 분자량을 확인하였다. 하기 표 1에서 나타난 바와 같이, 압출성형 조건에 따라 수율과 분자량의 조절이 가능한 것을 알 수 있었는데, 이는 결과적으로 압출성형 조건의 변화에 따라 다양한 종류의 제품생산이 가능한 것을 의미하였다.Using the same apple foil raw material and machinery as in Example 1, after preparing a sample while adjusting the temperature, screw speed, water content, and the like, the yield and molecular weight of the pectin was confirmed. As shown in Table 1, it was found that the yield and the molecular weight can be controlled according to the extrusion molding conditions, which means that it is possible to produce a variety of products in accordance with the change in the extrusion conditions.

(표 1)Table 1

실시예 20Example 20

건조 사과박을 L/D비 40의 이축 압출반응기에 투입한 후, 실시예 1과 동일한 건조하에서 압출성형한 결과, 펙틴의 수율이 19.5%로 크게 증가한 반면에, 분자량은 55,0000으로 감소하였다. 이는 L/D비의 증가에 따라 압출성형기내에서 사과박의 체류시간이 증가하였기 때문으로 추측되었다. 따라서, 반응조건 뿐만 아니라 L/D비의 변화에 의해서도, 수율과 분자량의 조절이 가능하다는 것을 알 수 있었다.The dried apple foil was put into a twin screw extruder with an L / D ratio of 40, and then extruded under the same drying as in Example 1, whereby the yield of pectin was greatly increased to 19.5%, while the molecular weight was reduced to 55,0000. . This was presumably because the residence time of apple foil in the extruder increased with increasing L / D ratio. Therefore, it was found that the yield and the molecular weight can be controlled not only by the reaction conditions but also by the change of the L / D ratio.

실시예 21Example 21

수분함량 80%의 함수 사과박을 L/D비l 40의 이축 압출반응기를 이용하여 온도 350℃, 스크류 속도 300rpm의 조건으로 압출성형하여 건조 사과박을 제조하였는데, 이때 생산된 펙틴의 수율과 분자량은 각각 14.2%, 118.000이였다. 이와 같은 결과는 사과가공 과정에서 발생하는 함수 사과박을 건조과정 없이 직접 압출성형한 경우에도 건조 사과박과 펙틴을 제조할 수 있다는 것을 의미한다.A dried apple foil was prepared by extruding an 80% water-containing apple foil at a temperature of 350 ° C. and a screw speed of 300 rpm using a biaxial extrusion reactor with an L / D ratio of 40. The yield and molecular weight of the produced pectin Were 14.2% and 118.000, respectively. This result means that even when the water-containing apple foil generated during the apple processing is directly extruded without a drying process, dried apple foil and pectin can be prepared.

실시예 22-31Example 22-31

건조 감귤류 껍질을 이용하여 상기 실시예 1과 동일한 압출성형기를 이용하여 시료를 조제한 후 이에 따른 펙틴의 생산수율을 확인하였다. 하기 표 2에 나타난 바와 같이, 감귤류 껍질의 경우에는 압출성형에 의하여 펙틴이 효율적으로 추출되는 것을 알 수 있다.Samples were prepared using the same extruder as in Example 1 using the dried citrus peel, and the yield of pectin was confirmed. As shown in Table 2, in the case of citrus peel, it can be seen that the pectin is efficiently extracted by extrusion molding.

(표 2)Table 2

실시예 32-40Example 32-40

갈조류의 일종인 미역(Undaria pinnatifide)을 상기 실시예 1과 동일한 기계장치를 사용하여, 온도, 스크류 속도, 수분함량등을 조절하면서 시료를 조제한 후, 이에 따른 알긴산의 생산수율을 확인하여, 하기 표 3에 나타내었다.The brown seaweed ( Undaria pinnatifide ), a kind of brown algae, was prepared by adjusting the temperature, screw speed, water content, etc. using the same machinery as in Example 1, and then confirming the production yield of alginic acid according to the following table. 3 is shown.

(표 3)Table 3

실시예 41-49Example 41-49

홍조류의 일종인 진두발(Chondrus crispus)로부터 실시에 1과 동일한 기계장치를 사용하여, 온도, 스크류속도, 수분함량 등을 조절하면서 시료를 조제하고, 이에 따른 카라기난의 생산수율을 확인하여 하기 표 4에 나타내었다.Using the same machinery as in Example 1 from Chondrus crispus , a type of red algae, samples were prepared while controlling temperature, screw speed, water content, and the like, and the yield of carrageenan was confirmed according to Table 4 below. Shown in

(표 4)Table 4

이상에서 상세히 설명하고 입증하였듯이, 본 발명은 압출성형을 이용하여 사과박, 감귤류 껍질, 해조류 등의 구성 다당류인 펙틴, 알긴산, 카라기난 등을 수용화하므로써, 종래의 산 및 알칼리에 의한 화학적인 추출법이 갖는 많은 문제점을 해결할 수 있는 다당류의 제조방법을 제공한다.As described and demonstrated in detail above, the present invention is a conventional chemical extraction method by acid and alkali by accepting pectin, alginic acid, carrageenan, etc., constituent polysaccharides such as apple peel, citrus peel, seaweed using extrusion molding It provides a method for producing a polysaccharide that can solve many problems having.

Claims (3)

사과박, 감귤류 껍질 또는 해조류를 L/D비(length diameter ratio) 20 내지 40의 이축 압출반응기에 투입한 후 스크류속도 150 내지 400 rpm, 시료투입속도 20 내지 50 kg/hr, 수분함량 15 내지 40%로 유지하면서 압출성형시키므로써 다당류를 생산하는 기술.Apple peel, citrus peel or algae is introduced into a twin screw extruder with a length diameter ratio of 20 to 40, and then the screw speed is 150 to 400 rpm, the sample feeding speed is 20 to 50 kg / hr, and the water content is 15 to 40. A technique for producing polysaccharides by extruding while maintaining the percentage. 제 1항에 있어 건조 사과박, 비건조 함수 사과박 및 감귤류 껍질을 이축 압출성형시키고 증류수를 넣어 교반한 다음, 원심분리하여 상등액을 취하여 상등액을 여과한 여과액에 이소프로판올을 넣고 방치하여 얻은 침전물을, 이소프로판올과 아세톤으로 세척한 후 상온에서 건조시켜 제조된 펙틴.The dried apple foil, undried apple citrus fruit and citrus peel are biaxially extruded, stirred with distilled water, centrifuged to obtain a supernatant, and the precipitate obtained by placing isopropanol in the filtrate filtered supernatant is left. , Pectin prepared by washing with isopropanol and acetone and drying at room temperature. 미역, 진두발 등의 해조류를 이축 압출성형기로 압출성형시키고 증류수를 넣어 교반한 다음, 원심분리하여 상등액을 취하여 상등액을 여과한 여과액에 이소프로판올을 넣고 방치하여 얻은 침전물을, 이소프로판올과 아세톤으로 세척한 후 상온에서 건조시켜 제조된 알지네이트와 카라기난.Seaweeds such as wakame and jindubal were extruded with a twin-screw extruder, stirred with distilled water, centrifuged, and the supernatant was taken. Alginate and carrageenan prepared by drying at room temperature.
KR1019990016100A 1999-05-04 1999-05-04 Production of Polysaccharides by the Extrusion Process KR19990064740A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010112817A (en) * 2000-06-15 2001-12-22 황재관 Method for isolating physiologically active materials from green tea
KR100367716B1 (en) * 2000-03-29 2003-01-14 윤의구 Manufacture of water soluble low-molecular alginate by autoclaving pretreatment and hot water extraction
KR20210027756A (en) * 2019-09-03 2021-03-11 (주)태초생활건강 Manufacturing method of fucoidan having high purity and low molecular

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5736949A (en) * 1980-08-12 1982-02-27 Nitto Electric Ind Co Ltd Preparation of pectin
JPS59179502A (en) * 1983-03-30 1984-10-12 Mitsubishi Acetate Co Ltd Preparation of carrageenan

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5736949A (en) * 1980-08-12 1982-02-27 Nitto Electric Ind Co Ltd Preparation of pectin
JPS59179502A (en) * 1983-03-30 1984-10-12 Mitsubishi Acetate Co Ltd Preparation of carrageenan

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100367716B1 (en) * 2000-03-29 2003-01-14 윤의구 Manufacture of water soluble low-molecular alginate by autoclaving pretreatment and hot water extraction
KR20010112817A (en) * 2000-06-15 2001-12-22 황재관 Method for isolating physiologically active materials from green tea
KR20210027756A (en) * 2019-09-03 2021-03-11 (주)태초생활건강 Manufacturing method of fucoidan having high purity and low molecular

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