KR20020080110A - Manufacturing method for water-soluble chitosan having high molecular weight - Google Patents

Manufacturing method for water-soluble chitosan having high molecular weight Download PDF

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KR20020080110A
KR20020080110A KR1020010019303A KR20010019303A KR20020080110A KR 20020080110 A KR20020080110 A KR 20020080110A KR 1020010019303 A KR1020010019303 A KR 1020010019303A KR 20010019303 A KR20010019303 A KR 20010019303A KR 20020080110 A KR20020080110 A KR 20020080110A
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chitosan
molecular weight
high molecular
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soluble
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임우진
임수길
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임우진
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    • 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
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
    • C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof

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Abstract

PURPOSE: Provided is a method capable of preparing a high molecular, water soluble chitosan which has deacetylation degree of 90% or more, and from which astringency is removed. CONSTITUTION: The method comprises the steps of (i) adding chitosan to aqueous mixture solution of sodium chloride and ascorbic acid and applying an ultrasound to the solution; (ii) centrifuging the resulting product from the step(i) to removing the supernatant; and (iii) washing the resulting product from the step(ii) with 95% or more of ethanol and drying the washed product. The method further comprises the step of washing chitosan with hydrogen peroxide prior to the step(i). The concentrations of sodium chloride and ascorbic acid in the aqueous mixture solution are 0.05-0.15 and 0.05-0.015 moles, respectively.

Description

고분자량 수용성 키토산 제조방법{Manufacturing method for water-soluble chitosan having high molecular weight}Manufacturing method for water-soluble chitosan having high molecular weight

본 발명은 키토산 제조방법에 관한 것으로서, 보다 상세하게는 고분자량의 수용성 키토산, 더욱 상세하게는 탈아세틸화도가 90%이상이며, 떫은 맛이 제거된 고분자량의 수용성 키토산을 고품질로 제조하는 방법에 관한 것이다.The present invention relates to a method for producing chitosan, and more particularly, to a high-quality water-soluble chitosan having a high molecular weight, more specifically, a deacetylation degree of 90% or more, and a method for producing high-molecular weight water-soluble chitosan from which astringent taste is removed. It is about.

1980년대 중반부터 산업분야에서 키토산의 다양한 용도가 밝혀지기 시작하면서 특정용도 및 응용분야에 부합되는 고유한 물성을 갖는 키토산 원료와 그 유도체의 개발이 활기를 띠기 시작하였다.Since the various uses of chitosan have been found in the industrial field since the mid-1980s, the development of chitosan raw materials and their derivatives, which have inherent properties corresponding to specific uses and applications, has been vigorous.

1980년대 초부터 1980년대 후반에 해당하는 기간 동안에 밝혀진 키토산의 용도는 대략 폐수처리 응용분야, 농업 응용분야, 식품과 음료 응용분야, 화장품 응용분야, 보건 위생 응용분야, 섬유관련 응용분야, 의약품 응용분야 등으로 대별될 수있다. 그러나 앞에 제시된 고유한 응용분야에서 최적의 효능이 발휘되려면 사용되는 키토산 자체가 엄격히 차별화되어야만 한다는 사실이 밝혀진 것은 최근의 일이다. 키토산이 유래되는 갑각의 종류(게, 새우, 갑오징어, 곤충의 갑각), 키토산의 분자량과 결정화도, 키토산의 순도, 키토산의 탈아세틸화도의 차이로부터 키토산의 차별화가 이루어질 수있다.The use of chitosan found during the period from the early 1980s to the late 1980s is largely in terms of wastewater treatment applications, agricultural applications, food and beverage applications, cosmetic applications, health and hygiene applications, textile applications, and pharmaceutical applications. Etc. can be divided into. However, it is only recently that the chitosan used must be strictly differentiated in order to achieve optimal efficacy in the unique applications presented above. Differentiation of chitosan can be made from the difference in the type of crust from which chitosan is derived (crab, shrimp, cuttlefish, insect crustacean), molecular weight and crystallinity of chitosan, purity of chitosan, and deacetylation of chitosan.

특히, 키토산은 천연물 중 유일하게 아미노기(NH2 +) 이온을 가지고 있어 화학적으로 음이온과 결합하기 쉬운 성질을 가지고 있어서 체내에서 유해한 중금속, 세균, 바이러스, 다이옥신 등과 같은 음이온을 배출시키는 역할을 할 수 있다. 이러한 역할을 증진시키기 위해서는 아미노기를 더욱 많이 가질 수 있는 고분자량의 키토산이 필요하다. 또한, 키토산이 수용성이면 식품과 음료 응용분야, 화장품 응용분야, 보건 위생 응용분야, 의약품 응용분야 등에서는 사용하기가 용이한 것으로 평가되고 있다.In particular, chitosan has the only amino group (NH 2 + ) ions among natural products, and has a property of being easily combined with anions chemically, which can play a role in releasing harmful anions such as heavy metals, bacteria, viruses, and dioxins in the body. . In order to enhance this role, a high molecular weight chitosan that can have more amino groups is required. In addition, if chitosan is water-soluble, it is evaluated to be easy to use in food and beverage applications, cosmetic applications, health and hygiene applications, and pharmaceutical applications.

상술한 바와 같이 고분자량이면서 수용성인 키토산의 필요성이 증대하고 있으면서도 현재까지 이러한 키토산의 제조방법은 알려진 바가 없다.As described above, while the necessity of high molecular weight and water-soluble chitosan is increasing, there is no known method for producing such chitosan.

따라서, 본 발명이 이루고자 하는 기술적 과제는 고분자량의 수용성인 키토산, 더욱 상세하게는 탈아세틸화도가 90% 이상이며, 떫은 맛이 제거된 고분자량의 수용성 키토산을 제조할 수 있는 방법을 제공하는 것이다.Accordingly, the technical problem to be achieved by the present invention is to provide a method for producing a high molecular weight water-soluble chitosan, more specifically a high molecular weight water-soluble chitosan having a deacetylation degree of 90% or more, and astringent taste is removed. .

도 1은 본 발명의 일실시예에 따라 제조된 키토산(실선으로 표시됨)과 기존의 키토산(점선으로 표시됨)에 대하여 FT-IR로 분석한 그래프로서,1 is a graph analyzed by FT-IR for chitosan (indicated by a solid line) and conventional chitosan (indicated by a dotted line) prepared according to an embodiment of the present invention.

도 2는 본 발명의 일실시예에 따라 제조된 키토산에 대하여 GPC로 분석한 그래프이다.Figure 2 is a graph analyzed by GPC for chitosan prepared according to an embodiment of the present invention.

상술한 기술적 과제를 달성하기 위하여, 본 발명은In order to achieve the above technical problem, the present invention

(a) 염화나트륨과 아스코르빈산 혼합 수용액에 키토산을 넣고 초음파를 가하는 단계;(a) adding chitosan to an aqueous solution of sodium chloride and ascorbic acid and applying ultrasonic waves;

(b) 상기 (a) 단계의 결과물을 원심분리하여 상등액을 제거하는 단계; 및(b) centrifuging the resultant of step (a) to remove the supernatant; And

(c) 상기 (b) 단계의 결과물을 95% 이상의 에탄올로 세척하고 건조하는 단계를 포함하는 것을 고분자량의 수용성 키토산 제조방법을 제공한다.(c) providing a method for producing a high molecular weight water-soluble chitosan comprising the step of washing and drying the resultant of step (b) with 95% or more of ethanol.

상술한 바와 같은 본 발명에 따른 제조방법은 상기 (a) 단계 이전에, 키토산을 과산화수소수로 세척하는 단계를 더 포함하는 것이 바람직하다.The manufacturing method according to the present invention as described above preferably further comprises the step of washing the chitosan with hydrogen peroxide before step (a).

상술한 바와 같은 본 발명에 따른 제조방법에 있어서, 상기 염화나트륨과 아스코르빈산 혼합 수용액 중에서 염화나트륨의 농도가 0.05 내지 0.15 몰농도이고, 아스코르빈산의 농도가 0.05 내지 0.015몰농도인 것이 바람직하다.In the production method according to the present invention as described above, it is preferable that the concentration of sodium chloride is 0.05 to 0.15 molar concentration, and the concentration of ascorbic acid is 0.05 to 0.015 molar concentration in the mixed solution of sodium chloride and ascorbic acid.

상술한 바와 같은 본 발명에 따른 제조방법은,The manufacturing method according to the present invention as described above,

(d) 상기 (c) 단계의 결과물을 물에 용해시키는 단계;(d) dissolving the result of step (c) in water;

(e) 상기 수용액을 공극 크기가 25 내지 50㎛인 필터로 여과하는 단계; 및(e) filtering the aqueous solution with a filter having a pore size of 25 to 50 μm; And

(f) 상기 여과물을 동결건조하는 단계를 더 포함하는 것이 바람직하다.(f) preferably lyophilizing the filtrate.

상술한 바와 같은 본 발명에 있어서, 상기 키토산은 1200cps 이상의 점도를 갖는 것을 출발물질로 사용하는 것이 바람직하다.In the present invention as described above, the chitosan is preferably used as a starting material having a viscosity of 1200cps or more.

이하, 본 발명을 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in detail.

본 발명에서는 기존의 키토산을 출발물질로 하여 고분자량의 수용성 키토산을 제조한다. 이 때의 출발물질이 되는 키토산은 그 점도가 1200cps 이상인 것을 사용하는 것이 바람직하다. 그 이유는 점도가 1200cps 미만인 것을 사용할 경우에 최종 생성물에서 저분자량의 키토산의 함량이 높아지는 문제점이 발생하기 때문이다.In the present invention, a high molecular weight water-soluble chitosan is prepared using the existing chitosan as a starting material. It is preferable to use the chitosan used as a starting material at this time whose viscosity is 1200 cps or more. The reason for this is that when a viscosity of less than 1200 cps is used, a problem arises in that the content of low molecular weight chitosan in the final product is increased.

먼저, 본 발명에서는 기존의 키토산을 염화나트륨과 아스코르빈산 혼합 수용액에 가한 다음 초음파 처리하여 고분자량으로 분획하고 수용성을 가질 수 있도록 한다.First, in the present invention, the existing chitosan is added to a mixed aqueous solution of sodium chloride and ascorbic acid and then ultrasonicated to fractionate into high molecular weight and have water solubility.

상기 염화나트륨과 아스코르빈산 혼합 수용액 중에서 염화나트륨의 농도가 0.05 내지 0.15몰농도이고, 아스코르빈산의 농도가 0.05 내지 0.015몰농도인 것이 바람직하며, 또한, 상기 염화나트륨과 아스코르빈산 혼합 수용액 1ℓ에 대하여 키토산 약 100g 정도를 부가하는 것이 좋다.It is preferable that the concentration of sodium chloride is 0.05 to 0.15 molar concentration, and the concentration of ascorbic acid is 0.05 to 0.015 molar concentration in the sodium chloride and ascorbic acid mixed aqueous solution, and chitosan per 1 L of the mixed sodium chloride and ascorbic acid aqueous solution. It is good to add about 100g.

그리고, 상기 초음파의 범위는 일반적인 초음파 발생기에서 발생되는 초음파 정도의 범위이면 충분하다.In addition, the range of the ultrasonic wave is sufficient to be the range of the ultrasonic level generated in a general ultrasonic generator.

이어서, 초음파 처리 결과물을 원심분리하여 상등액은 제거하고 하부에 가라앉은 것을 취하여 95%이상의 에탄올을 세척하고 이를 건조하면 본 발명에 따른 고분자량의 수용성 키토산을 제조할 수 있다. 원심분리 단계 및 에탄올 세척 단계를 거치는 이유는 초음파 처리 단계에서 키토산의 표면에 붙어 있는 불순물이나 수분 등을 제거하기 위한 것이다. 이와 같은 제조방법을 통하여 제조되는 키토산은 그 중량평균분자량이 약 600,000정도이며, 물에 거의 100% 녹을 수 있다.Subsequently, the supernatant is removed by centrifugation, and the supernatant is removed. The supernatant is submerged to wash 95% or more of ethanol and to dry it, thereby preparing a high molecular weight water-soluble chitosan according to the present invention. The reason for going through the centrifugation step and the ethanol washing step is to remove impurities, moisture, etc. on the surface of the chitosan in the sonication step. Chitosan produced through such a manufacturing method has a weight average molecular weight of about 600,000, and can be dissolved in water almost 100%.

상술한 바와 같은 과정을 통하여 본 발명에서 목적하는 바인 고분자량의 수용성인 키토산의 제조가 가능하지만, 제조되는 키토산의 색상을 백색으로 하고, 살균 등을 통하여 안전성을 높이기 위하여, 초음파 처리 단계 전에 과량의 과산화수소수로 세척하는 과정을 거치는 것이 바람직하다.It is possible to produce a high molecular weight water-soluble chitosan, which is the object of the present invention through the above-described process, but in order to make the color of the chitosan produced white and to increase the safety through sterilization, It is preferable to go through the process of washing with hydrogen peroxide.

또한, 고분자량의 수용성인 키토산을 탈아세틸화도가 90% 이상이며, 떫은 맛이 제거될 수 있도록, 상술한 제조방법 중에서 원심분리한 결과물을 물에 용해시키고 이를 여과하고 동결건조하는 단계를 수행하는 것이 바람직하다.In addition, the deacetylation degree of the high molecular weight water-soluble chitosan is 90% or more, so that the astringent taste can be removed, the resultant centrifuged in the above-described manufacturing method dissolved in water, filtered and lyophilized It is preferable.

상기 여과시 필터의 공극 크기는 25 내지 50㎛인 것이 좋으며, 이러한 여과 단계를 통하여 수용액 중의 불순물로 포함되어 있는 이온, 먼지 등을 제거되어 떫은 맛이 제거될 수 있다.The pore size of the filter at the time of filtration is preferably 25 to 50㎛, through the filtration step, ions, dust and the like contained in the aqueous solution may be removed to remove the astringent taste.

또한, 상기 동결건조 단계는 일반적인 동결건조기를 이용하여 약 -70℃에서 급속 냉동하여 수행되며, 이러한 동결건조 단계를 통하여 수분이 거의 완전히 제거되어 탈아세틸화도가 90% 이상으로 높아지게 되는 것이다.In addition, the freeze-drying step is carried out by rapid freezing at about -70 ℃ using a common lyophilizer, the water is almost completely removed through this freeze-drying step to increase the deacetylation degree to more than 90%.

이러한 탈아세틸화도를 높이는 단계에서는 출발물질로 사용되는 키토산의 탈아세틸화도가 80% 이상인 것을 사용하는 것이 바람직하다.In the step of increasing the degree of deacetylation, it is preferable to use a deacetylation degree of chitosan used as a starting material of 80% or more.

이하, 본 발명을 하기의 실시예에 의거하여 상세하게 설명하기로 한다. 하기의 실시예에 의해 본 발명이 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail based on the following examples. The present invention is not limited by the following examples.

(실시예 1)(Example 1)

본 실시예에서는 키토산의 농도가 1중량%가 되도록 초산에 키토산을 녹인 다음 25℃에서 B형 점도계로 측정하여 점도가 약 1200cps가 되는 키토산을 출발물질로 사용하였다.In this example, chitosan was dissolved in acetic acid so that the concentration of chitosan was 1% by weight, and the chitosan having a viscosity of about 1200 cps was used as a starting material by measuring with a type B viscometer at 25 ° C.

염화나트륨과 아스코르빈산을 그 농도가 각각 0.1몰이 되도록 물에 용해시킨 혼합 수용액 2ℓ를 초음파 추출기(미국에 소재하는 프로 라도(Pro Lado)에서 만든 모델명 Sox Wave 100)에 넣은 다음, 이어서 상기 키토산 200g을 상기 혼합 수용액에 부가하고 30℃에서 20분간 파장이 15Å인 초음파를 가하여 반응시켰다.2 liters of a mixed aqueous solution in which sodium chloride and ascorbic acid were dissolved in water so that their concentration was 0.1 mole each were placed in an ultrasonic extractor (Model Sox Wave 100, manufactured by Pro Lado, USA), followed by 200 g of the chitosan. It was added to the mixed aqueous solution and reacted by adding ultrasonic waves having a wavelength of 15 Hz at 20C for 20 minutes.

이어서, 상기 반응 결과물을 7,000rpm에서 15분간 원심분리기(비전과학에서 제조한 모델명 VS-21SMTN)를 통하여 원심분리한 다음 상등액은 제거하고, 이어서 과량의 95% 에탄올로 30분간 세척하였다.Subsequently, the reaction product was centrifuged at 7,000 rpm for 15 minutes through a centrifuge (Model VS-21SMTN manufactured by Vision Science), and then the supernatant was removed and then washed with excess 95% ethanol for 30 minutes.

마지막으로 세척한 결과물을 자연건조하여 고분자량의 수용성 키토산 180g(수율 90%)을 제조하였다.Finally, the resultant washed naturally dried to prepare a high molecular weight water-soluble chitosan 180g (90% yield).

(실시예 2)(Example 2)

초음파 추출기에 부가하기 전에 과량의 0.01N 과산화수소수로 세척하는 단계를 더 거친 것을 제외하고는 상기 실시예1과 동일한 제조방법을 고분자량의 수용성 키토산 180g(수율 90%)을 제조하였다.180 g (yield 90%) of high molecular weight water-soluble chitosan was prepared in the same manner as in Example 1, except that the washing step was performed with an excess amount of 0.01 N hydrogen peroxide before adding to the ultrasonic extractor.

본 실시예 2를 통해서 백색이면서 안전성이 높은 키토산을 제조할 수 있었다.In Example 2, chitosan, which was white and highly stable, could be produced.

(실시예 3)(Example 3)

본 실시예에서는 키토산의 농도가 1중량%가 되도록 초산에 키토산을 녹인 다음 25℃에서 B형 점도계로 측정하여 점도가 약 1200cps가 되며, 탈아세틸화도가 80% 이상인 키토산을 출발물질로 사용하였다.In this example, chitosan was dissolved in acetic acid so that the concentration of chitosan was 1% by weight, and the resultant was measured at 25 ° C. using a B-type viscometer to obtain a viscosity of about 1200 cps.

염화나트륨과 아스코르빈산을 그 농도가 각각 0.1몰이 되도록 물에 용해시킨혼합 수용액 2ℓ를 초음파 추출기(미국에 소재하는 프로 라도(Pro Lado)에서 만든 모델명 Sox Wave 100)에 넣은 다음, 이어서 상기 키토산 200g을 상기 혼합 수용액에 부가하고 30℃에서 20분간 파장이 15Å인 초음파를 가하여 반응시켰다.2 L of a mixed aqueous solution in which sodium chloride and ascorbic acid were dissolved in water at a concentration of 0.1 mol each was placed in an ultrasonic extractor (Model Sox Wave 100, manufactured by Pro Lado, USA), and then 200 g of the chitosan was added thereto. It was added to the mixed aqueous solution and reacted by adding ultrasonic waves having a wavelength of 15 Hz at 20C for 20 minutes.

이어서, 상기 반응 결과물을 12,000rpm에서 30분간 원심분리기(비전과학에서 제조한 모델명 VS-21SMTN)를 통하여 원심분리한 다음 상등액은 제거하였다.Subsequently, the reaction product was centrifuged at 12,000 rpm for 30 minutes through a centrifuge (Model VS-21SMTN manufactured by Vision Science), and then the supernatant was removed.

이어서, 원심분리한 결과물을 물에 용해시켜 약 2중량% 수용액을 만든 다음에 진공펌프를 이용하여 공극의 크기가 30㎛인 필터로 강제여과하였다.Subsequently, the resultant obtained by centrifugation was dissolved in water to form an aqueous solution of about 2% by weight, and then filtered by a filter having a pore size of 30 μm using a vacuum pump.

이어서, 상기 여과 잔류물을 동결건조기에 넣고 -70℃에서 냉동한 후 건조한 다음 분쇄하여 고분자량의 수용성 키토산 120g(수율 60%)을 제조하였다.Subsequently, the filtration residue was placed in a lyophilizer, frozen at −70 ° C., dried, and ground to prepare 120 g (yield 60%) of high molecular weight aqueous chitosan.

본 실시예 3에서 제조한 키토산은 탈아세틸화도가 90%이상이며, 떫은 맛이 제거된 키토산이 제조된다.Chitosan prepared in Example 3 has a degree of deacetylation of 90% or more, and chitosan from which astringent taste is removed is prepared.

(실험예)Experimental Example

상기 실시예 1에서 제조한 키토산과 기존 키토산을 FT-IR로 분석하여 그 결과를 도 1에 나타냈다.The chitosan prepared in Example 1 and the existing chitosan were analyzed by FT-IR and the results are shown in FIG. 1.

도 1를 보면 본 발명의 실시예 1에 따라 제조된 키토산 피크와 기존 키트산 피크가 동일한 것으로 나타났으므로 본 발명에 따라 제조된 것이 키토산인 것을 확인할 수 있었다.1 shows that the chitosan peak prepared according to Example 1 of the present invention and the existing kit acid peak were the same, and thus, the chitosan prepared according to the present invention was confirmed.

또한, 실시예 1에서 제조한 키토산을 GPC로 분석하여 그 결과를 도 2에 나타냈으며, 도 2의 결과를 보면 본 발명에 따라 제조된 키토산의 중량평균분자량 약 600,000인 것을 알 수 있었다.In addition, the chitosan prepared in Example 1 was analyzed by GPC, and the results are shown in FIG. 2, and the results of FIG. 2 showed that the weight average molecular weight of the chitosan prepared according to the present invention was about 600,000.

상술한 바와 같은 본 발명에 따른 제조방법은 고분자량의 수용성 키토산 또는 탈아세틸화도가 90% 이상이며, 떫은 맛이 제거된 고분자량의 수용성 키토산을 고품질이면서도 고수율로 제조할 수 있는 장점이 있다.The production method according to the present invention as described above has the advantage that the high molecular weight water-soluble chitosan or deacetylation degree of 90% or more, the high-molecular weight water-soluble chitosan from which the astringent taste is removed can be produced with high quality and high yield.

Claims (8)

(a) 염화나트륨과 아스코르빈산 혼합 수용액에 키토산을 넣고 초음파를 가하는 단계;(a) adding chitosan to an aqueous solution of sodium chloride and ascorbic acid and applying ultrasonic waves; (b) 상기 (a) 단계의 결과물을 원심분리하여 상등액을 제거하는 단계; 및(b) centrifuging the resultant of step (a) to remove the supernatant; And (c) 상기 (b) 단계의 결과물을 95% 이상의 에탄올로 세척하고 건조하는 단계를 포함하는 것을 특징으로 하는 고분자량의 수용성 키토산 제조방법.(C) a method of producing a high molecular weight water-soluble chitosan, characterized in that the step of washing (b) the resultant with 95% or more of ethanol and dried. 제 1항에 있어서,The method of claim 1, 상기 (a) 단계 이전에, 키토산을 과산화수소수로 세척하는 단계를 더 포함하는 것을 특징으로 하는 고분자량의 수용성 키토산 제조방법.Before the step (a), the method of producing a high molecular weight water-soluble chitosan, further comprising the step of washing chitosan with hydrogen peroxide water. 제 1항 또는 2항에 있어서,The method according to claim 1 or 2, 상기 염화나트륨과 아스코르빈산 혼합 수용액 중에서 염화나트륨의 농도가 0.05 내지 0.15 몰농도이고, 아스코르빈산의 농도가 0.05 내지 0.015몰농도인 것을 특징으로 하는 고분자량의 수용성 키토산 제조방법.A method for producing a high molecular weight water-soluble chitosan, wherein the concentration of sodium chloride is 0.05 to 0.15 molar concentration and the concentration of ascorbic acid is 0.05 to 0.015 molar concentration in the mixed sodium chloride and ascorbic acid aqueous solution. 제 1항 또는 2항에 있어서,The method according to claim 1 or 2, (d) 상기 (c) 단계의 결과물을 물에 용해시키는 단계;(d) dissolving the result of step (c) in water; (e) 상기 수용액을 공극 크기가 25 내지 50㎛인 필터로 여과하는 단계; 및(e) filtering the aqueous solution with a filter having a pore size of 25 to 50 μm; And (f) 상기 여과물을 동결건조하는 단계를 더 포함하는 것을 특징으로 하는 고분자량의 수용성 키토산 제조방법.(F) a method of producing a high molecular weight water-soluble chitosan, characterized in that further comprising the step of lyophilizing the filtrate. 제 1항에 있어서,The method of claim 1, 상기 키토산이 1200cps 이상의 점도를 갖는 것을 특징으로 하는 고분자량의 수용성 키토산 제조방법.Method for producing a high molecular weight water-soluble chitosan, characterized in that the chitosan has a viscosity of 1200cps or more. 상술한 바와 같은 제1항에 의해 제조되는 것을 특징으로 하는 고분자량의 수용성 키토산.A high molecular weight water soluble chitosan, which is prepared according to claim 1 as described above. 중량평균분자량이 약 600,000이고, 물에 녹는 키토산.Chitosan that has a weight average molecular weight of about 600,000 and is soluble in water. 제 7항에 있어서, 상기 키토산의 탈아세틸화도가 90%이상이며, 떫은 맛이 제거된 키토산.The chitosan according to claim 7, wherein the degree of deacetylation of the chitosan is 90% or more, and the astringent taste is removed.
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KR100506710B1 (en) * 2003-03-24 2005-08-05 주식회사 건풍바이오 Chitosan oligosaccharide ascorbic acid salt having anti-diabetic effect
CN103172758A (en) * 2013-03-14 2013-06-26 内蒙古医科大学 Method for extracting polysaccharides from fringed pinks

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KR950014473A (en) * 1993-11-25 1995-06-16 김무연 Pure cotton chlorite low temperature bleaching method
JPH0931105A (en) * 1995-07-24 1997-02-04 Kitosan Shokuhin Kogyo Kk Production of low-molecular chitosan and chitooligosaccharide
KR100200547B1 (en) * 1997-05-27 1999-06-15 유향자 Method of separation and purification for low molecular weight chitosan using multi-step membrane process
KR19990057607A (en) * 1997-12-30 1999-07-15 조정래 Chitosan Derivative Manufacturing Method
KR19990069029A (en) * 1998-02-04 1999-09-06 김공수 Water-soluble low molecular chitin, chitosan and oligosaccharides thereof
KR20000007967A (en) * 1998-07-09 2000-02-07 윤종용 Self-inspection method for base station testing equipment
KR20000012173A (en) * 1999-03-26 2000-03-06 김공수 Method of manufacturing polysaccharites having low molecular weight and oligosaccharites
KR20010025932A (en) * 1999-09-01 2001-04-06 문상돈 Preparation method by ultrasonication of microcrystalline chitosan

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KR100506710B1 (en) * 2003-03-24 2005-08-05 주식회사 건풍바이오 Chitosan oligosaccharide ascorbic acid salt having anti-diabetic effect
CN103172758A (en) * 2013-03-14 2013-06-26 内蒙古医科大学 Method for extracting polysaccharides from fringed pinks

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