KR20120076901A - Method of manufacture high concentration collagen extract using duck and extract from thereof - Google Patents
Method of manufacture high concentration collagen extract using duck and extract from thereof Download PDFInfo
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- KR20120076901A KR20120076901A KR1020100138667A KR20100138667A KR20120076901A KR 20120076901 A KR20120076901 A KR 20120076901A KR 1020100138667 A KR1020100138667 A KR 1020100138667A KR 20100138667 A KR20100138667 A KR 20100138667A KR 20120076901 A KR20120076901 A KR 20120076901A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/275—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of animal origin, e.g. chitin
- A23L29/281—Proteins, e.g. gelatin or collagen
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
- A23L3/42—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution with addition of chemicals before or during drying
Abstract
Description
본 발명은 오리 날개와 오리발로부터 화장용 원료 및 식품 원료로 사용할 수 있는 콜라겐 함유량이 높은 콜라겐 추출물을 생산하기 위한 오리 콜라겐 제조방법에 관한 것으로, 본 발명에 의해 생산된 오리 콜라겐은 내과, 안과, 외과, 이비인후과 등의 의약용 소재는 물론이고, 피부미용과 관련된 화장용 분야, 관절 및 피부미용과 관련된 건강기능식품분야 등의 다양한 분야에 효과적으로 사용될 수 있는 원료를 공급할 수 있는 소재를 공급하기 위한 발명이라 할 수 있다.The present invention relates to a duck collagen production method for producing a collagen extract with a high collagen content that can be used as a cosmetic raw material and food raw material from duck wings and flippers, the duck collagen produced by the present invention is internal medicine, ophthalmology, surgery It is an invention for supplying raw materials that can effectively be used in various fields, such as medical materials such as otolaryngology, cosmetic fields related to skin beauty, and health functional food fields related to joint and skin beauty. can do.
콜라겐은 포유동물을 비롯한 수산동물, 설치류와 조류 등의 껍질, 연골, 뼈, 인대, 혈관, 근막 등 생체조직 전반에 걸쳐 분포되어 있는 조직의 구조를 형성하는 근간이 되는 구조 단백질이다. 콜라겐의 생체 내 기능 중 가장 중요한 것은 뮤코다당체로서 콘드로이틴황산과 함께 고분자 매트릭스를 구성하여 각 기관의 특정구조를 유지 구성하는 것인데 다른 뮤코다당과 함께 분자량이나 함량 등에서는 차이가 있지만 포유동물의 동일 조직에서는 동일한 형태 및 비율로 존재한다.Collagen is a structural protein that forms the structure of tissues distributed throughout biological tissues, such as shells, cartilage, bones, ligaments, blood vessels, and fascia of marine animals, including mammals, rodents, and birds. The most important function of collagen in vivo is the mucopolysaccharide, which forms a polymer matrix with chondroitin sulfate to maintain the specific structure of each organ. In the same form and proportion.
특히 우리 몸속에는 단백질이 약 20% 포함되어 있는데 이중 콜라겐이 30%를 차지하는 물질이다(L.C.Junqueira and J.carneiro1983). 콜라겐은 크게 3가지로 구분될 수 있는데, 조직의 종류에 따라 섬유상 특성을 나타내는 선형 콜라겐(Type I, II, III), 비선형 콜라겐(Type IV), 미세 콜라겐(Type V, VI, VII, IX, X)등으로 구분할 수 있다. 지금까지 알려진 바에 의하면, 도계 부산물의 경우 닭발, 날개끝, 무릎연골, 가슴연골, 껍질 등에는 주로 선형 콜라겐이 많으며, Type I은 피부, 건, 뼈, 혈관 등에, Type II는 연골조직에, Type III 콜라겐은 Type I과 같으나 뼈에는 존재하지 않는 것으로 알려져 있다.In particular, our body contains about 20% protein, of which 30% is collagen (L.C. Junqueira and J.carneiro1983). Collagen can be largely classified into three types: linear collagen (Type I, II, III), nonlinear collagen (Type IV), fine collagen (Type V, VI, VII, IX, X) can be divided. So far, known by-products of chicken meat, wing tip, knee cartilage, breast cartilage, shell, etc. are mainly a lot of linear collagen, Type I is skin, tendon, bone, blood vessel, Type II is cartilage tissue, Type Collagen III is the same as Type I but is not present in bone.
생체의 연령 변화에 따라 콜라겐의 구성비가 변화하는데, 연령이 증가함에 따라 결국 그 함량이 감소한다고 알려져 있다. 즉 사람이 나이가 들면서 겪는 피부의 탄력 저하나 관절의 유연성 감소 등 이른바 노화현상은 피부를 구성하는 세포의 수분대사 감소와 결합조직 중 기초물질로서 보수력이 뛰어난 콜라겐이 감소하기 때문인 것으로 알려져 있다. 고령화에 따른 콜라겐 감소는 세포의 신진대사인 수분대사 조절에 영향을 주어 노화의 진행이 빨라지고, 각 조직 중의 수분함량을 감소시켜 결합조직의 원활함과 피부의 탄력도 없어진다. 이러한 상황에서 콜라겐을 섭취하여 보충해 주면 노화가 저지되고 피부에 윤기와 탄력을 주게 된다.The composition ratio of collagen changes with age of the living body, and it is known that the content decreases with age. In other words, the so-called aging phenomenon, such as a decrease in elasticity of the skin and a decrease in the flexibility of joints, which are experienced as a person ages, is known to be due to a decrease in water metabolism of cells constituting the skin and a decrease in collagen, which is excellent in water retention as a basic substance in connective tissues. Collagen reduction due to aging affects the regulation of water metabolism, which is a metabolism of cells, and accelerates the aging process, and decreases the water content in each tissue, thereby reducing the smoothness of connective tissue and skin elasticity. In these situations, supplementing with collagen will slow aging and give your skin shine and elasticity.
이런 상황에서 콜라겐을 의약품, 화장품, 건강기능성 식품 등의 형태로 인체 내부로 섭취하거나 또는 신체에 공급해 주면 노화가 억제되고 피부에 윤기와 탄력을 주게 되는 피부미용 효과를 얻을 수 있을 것이다.In this situation, if collagen is ingested or supplied to the human body in the form of medicines, cosmetics, health functional foods, etc., aging may be suppressed and skin beauty effect may be given to the skin with shine and elasticity.
본 발명은 매년 증가하고 있는 오리 소비량과 함께 불용자재로 허비되고 있는 오리 부산물, 즉 오리발과 오리날개 중에 함유되어 있는 오리 콜라겐을 생산하는 방법을 발명함으로서 국내 부존자원의 확보는 물론이고 대부분 수입에 의존하는 기능성 소재의 수입대체효과를 거둘 수 있는 높은 산업적 가치를 획득하기 위하여 실시하였다. The present invention invents a method of producing duck by-products, i.e., duck collagen contained in flippers and duck wings, which are consumed with increasing duck consumption every year. This study was conducted to obtain high industrial value that can achieve the import substitution effect of functional materials.
이에 본 발명자들은 광우병, 구제역 및 대장균 등의 오염으로부터 안정성이 보장되고 고부가가치를 창출하여 축산농가의 소득 증대에 기여할 수 있는 기능성 소재인 콜라겐을 생산하는 방법을 발명함으로써 매년 막대한 양이 폐기되고 있는 오리 날개와 오리발로부터 콜라겐을 추출하는 것으로 본 발명을 완성하였다. 따라서 본 발명의 목적은 부산물로부터 콜라겐을 추출하는 방법을 제공하는 데 있다.Therefore, the inventors have invented a method of producing collagen, a functional material that can guarantee stability from contamination of mad cow disease, foot-and-mouth disease and E. coli, and create high added value, thereby contributing to raising the income of livestock farmers. The present invention was completed by extracting collagen from wings and flippers. It is therefore an object of the present invention to provide a method for extracting collagen from by-products.
상기 목적을 달성하기 위한 본 발명은 날개 및 발의 뼈를 제거한 후, 껍질과 함께 각각 작은 크기로 세절한 후 -20℃이하에 급냉시키는 원료 전처리 단계와, 이를 수산화나트륨을 이용하여 표백 및 과도한 지방을 제거하는 단계와, 산 및 염화나트륨을 이용하여 가용성 콜라겐 추출물을 제조하는 단계와, 추출에 사용한 염을 제거하는 탈염단계와, 이를 농축 건조하여 콜라겐 함유 건조물을 얻는 건조공정으로 구성되는 것을 특징으로 하고 있다. 구제적으로는 하기와 같다.The present invention for achieving the above object is a raw material pretreatment step of removing the bones of the wings and feet, and then shred into small sizes with shells, and then quenched below -20 ℃, using bleaching and excess fat using sodium hydroxide Removing, preparing a soluble collagen extract using acid and sodium chloride, desalting to remove salt used for extraction, and drying to obtain collagen-containing dried product by concentrated drying. . Specifically, it is as follows.
1) 원료의 전처리 단계1) Pretreatment Step of Raw Material
오리발, 오리날개를 흐르는 물로 깨끗이 수세하는 방법으로 이물질을 제거하였다. 오리발은 피부를 절개한 후, 내부의 발가락뼈 중 단단한 뼈 부분을 모두 제거한 후 이를 원료로 사용하였으며, 날개도 오리발과 동일한 방법으로 분쇄가 되지 않을 굵은 뼈만 제거한 후 이를 사용하였다. 전술한 원료를 세절한 후 -20℃이하의 급냉실에서 동결시켰으며, 완전히 동결된 원료에 4℃이하 냉수를 첨가한 후 원료의 육괘가 보이지 않을 정도로 세절하였고, 이를 원심분리하여 상층액과 지방층 물질들을 아스피레이터로 제거하는 것으로 원료육의 전처리를 완성하였다.The foreign substances were removed by washing the flippers and duck wings with running water. After the incision of the flippers, all the hard bones of the inner toe bone were removed and then used as raw materials. The wings were also used after removing the coarse bones that would not be crushed in the same way as the flippers. The raw materials were chopped and frozen in a quenching chamber at -20 ° C. or lower, and cold water at 4 ° C. or lower was added to the completely frozen raw material, and the raw material was sliced so that the grains of the raw material were not visible. The pretreatment of the raw meat was completed by removing the substances with an aspirator.
2) 지방 제거단계2) fat removal step
상기 1)에서 수득한 침전물에 염기성 용액(수산화나트륨, 수산화칼륨, 수산화칼슘, 수산화마그네슘, 소듐하이포클로라이트 등)을 첨가하여 12-48hr 냉장실에서 교반하였다. 교반이 끝난 수산화나트륨 용액을 원심분리하여 비콜라겐 물질인 상등액과 상층부의 지방 등의 부유물을 제거하였다. 이러한 수산화나트륨을 이용한 세척을 2회 반복 실시하였다. 이러한 비 콜라겐 물질의 제거는 콜라겐 제품 순도를 증가시킬 수 있으며 악취나 부패의 원인을 제거하여 안정성이 향상된 제품을 만들 수 있게 된다.A basic solution (sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, sodium hypochlorite, etc.) was added to the precipitate obtained in 1), followed by stirring in a 12-48hr refrigerator compartment. The stirred sodium hydroxide solution was centrifuged to remove suspended substances such as supernatant, a non-collagen substance, and fats in the upper layer. This washing with sodium hydroxide was repeated twice. Removal of these non-collagen substances can increase the purity of collagen products and eliminate the cause of odor or rot to make products with improved stability.
3) 콜라겐 추출단계3) Collagen Extraction Step
상기 2)의 잔사를 잔사 표면의 물기가 없어질 때 까지 감압 건조시킨 후, 4℃로 냉각시켜 둔 0.1~2M 농도의 산성 용액(초산, 포름산, 구연산 등)을 가하여 24~48hr 냉장실(4℃)에서 교반하며 콜라겐을 추출하였다. 콜라겐이 추출된 용액을 원심분리하였으며, 상층액을 분취하여 최종농도 5-20%(v/w)가 되도록 염화나트륨을 첨가한 후 10-120분간 실온에 정치하였다. 이 용액을 원심분리 하였으며, 상등액을 제거하고 침전물을 콜라겐 농축물로 수득하였다. The residue of 2) was dried under reduced pressure until the moisture on the surface of the residue disappeared, and then an acid solution (acetic acid, formic acid, citric acid, etc.) of 0.1-2 M concentration, cooled to 4 ° C., was added to the refrigerator for 24 to 48 hours (4 ° C.). The collagen was extracted with stirring. The collagen extracted solution was centrifuged, the supernatant was aliquoted, and sodium chloride was added to a final concentration of 5-20% (v / w), and then allowed to stand at room temperature for 10-120 minutes. This solution was centrifuged, the supernatant was removed and the precipitate was obtained as a collagen concentrate.
4) 탈염 및 농축 단계4) Desalting and Concentrating Steps
상기 3)에서 수득한 침전물에 증류수를 첨가하여 잘 분산시킨 후, 셀룰로오스 한외여과막(Cellu sep, 분자량 3,500)에 충진시킨 후, 48시간 이상 증류수를 이용하여 4℃에서 투석하였다. 투석외액은 1일 2회 이상 교환하였으며, 투석이 완료된 콜라겐 용액은 동결건조의 방법으로 콜라겐 분말을 수득하였다. After distilled water was added to the precipitate obtained in 3) to disperse well, the cellulose ultrafiltration membrane (Cellu sep, molecular weight 3,500) was filled, and dialyzed at 4 ° C. using distilled water for 48 hours or more. The dialysis solution was exchanged at least twice a day, and the collagen solution after dialysis was obtained by lyophilization to obtain collagen powder.
본 발명에 따르면, 국내 오리 시장에서 폐기되고 있는 오리발 및 오리날개로부터 기능성 소재인 동물성 콜라겐을 효율적으로 생산하여 이를 산업 전반에 활용하고자 하는 것으로, 이는 폐기되고 있는 동물성 소재의 발굴에 따른 부존자원의 개발적 효과, 오리 산업에 고부가가치 원료를 생산할 수 있다는 경제적 효과, 전처리-탈지방-추출-농축이라는 단순한 생산 공정 및 생산 수율의 증가에서 오는 산업적 효과를 기대할 수 있으며, 이를 내과, 외과, 안과, 이비인후과 등의 의약분야 및 화장품산업분야에 범용적으로 사용할 수 있는 안전한 기능성 물질을 공급할 수 있는 기반을 조성해 줄 수 있는 효과를 거둘 수 있으리라 생각한다. According to the present invention, to efficiently produce animal collagen, which is a functional material, from the flippers and duck wings that are discarded in the domestic duck market, and to utilize them throughout the industry, which is the development of abundant resources according to the discovery of the discarded animal material Economic effects, the economic effect of producing high value-added raw materials for the duck industry, the simple production process of pretreatment-defatting-extraction-concentration and the increase in production yield can be expected, which can be used in internal medicine, surgery, ophthalmology and otolaryngology. I think it will be able to create a foundation to supply safe functional materials that can be used universally in the pharmaceutical and cosmetic industries.
도 1은 실시예 6에 따라 나타나는 전기영동도이다.
도 2는 콜라겐 추출물의 용해도 측정결과이다
도 3은 콜라겐 추출물의 탁도 측정결과이다1 is an electrophoretic diagram shown according to Example 6.
2 is a result of measuring the solubility of collagen extract
3 is a turbidity measurement result of the collagen extract
이하에서 실시예를 통하여 본 발명을 보다 상세히 설명할 것이다. 그러나, 이하의 실시예는 단지 예시를 위한 것이므로, 본 발명의 범위를 국한시키는 것으로 이해되어서는 안 될 것이다.Hereinafter, the present invention will be described in more detail with reference to Examples. However, the following examples are for illustration only and should not be understood as limiting the scope of the invention.
실시예Example 1) 전처리 단계 1) Pretreatment Step
오리발(발목주위를 절단하고 남은 발가락 부위), 오리날개(날개의 가장 끝 부분에서 관절부위를 절단한 날개)를 흐르는 물로 깨끗이 수세하는 방법으로 이물질을 제거하였다. 오리발은 피부를 절개한 후, 내부의 발가락뼈 중 단단한 뼈 부분을 모두 제거한 후 이를 원료로 사용하였으며, 날개도 오리발과 동일한 방법으로 분쇄가 되지 않을 굵은 뼈만 제거한 후 이를 사용하였다. 전술한 원료를 2cm 이하의 크기로 세절한 후 -20℃이하의 급냉실에서 동결시켰으며, 완전히 동결된 원료에 10배수(v/v)의 4℃이하 냉수를 첨가한 후 15,000rpm 이상/3min(IKA-T 18 B 균질기)간 원료의 육괘가 보이지 않을 정도로 세절하였으며, 이를 10,000xg/30분(4℃)간 원심분리하여 상층액과 지방층 물질들을 아스피레이터로 제거하는 것으로 원료육의 전처리를 완성하였다.The foreign body was removed by washing the flippers (cut off the ankle and the remaining toe) and the wing of the duck (wings cut at the end of the wing) with running water. After the incision of the flippers, all the hard bones of the inner toe bone were removed and then used as raw materials. The wings were also used after removing the coarse bones that would not be crushed in the same way as the flippers. The above-mentioned raw materials were chopped to a size of 2 cm or less and then frozen in a quenching chamber at -20 ° C. or lower. After adding 10 times (v / v) cold water at 4 ° C. or lower to a completely frozen raw material, 15,000 rpm or more / 3 min. (IKA-T 18 B Homogenizer) The raw material was chopped so as not to be seen, and it was centrifuged at 10,000xg / 30 minutes (4 ℃) to remove supernatant and fatty layer materials with aspirator. To complete.
실시예Example 2) 지방 제거단계 2) fat removal step
상기 실시예 1)에서 수득한 침전물에 1~10배(w/v)량의 4℃ 0.01~2M 염기성 용액(수산화나트륨, 수산화칼륨, 수산화칼슘, 수산화마그네슘, 소듐하이포클로라이트 등)을 첨가하여 12-48hr 냉장실에서 교반하였다. 본 발명에서는 발명의 조건을 단순화시키기 위하여 1M수산화나트륨을 10배수(w/v) 첨가하여 24시간 교반하는 것으로 하였다. 교반이 끝난 수산화나트륨 용액을 10,000xg/30분(4℃)간 원심분리하여 비콜라겐 물질인 상등액과 상층부의 지방 등의 부유물을 제거하였다. 이러한 수산화나트륨을 이용한 세척을 2회 반복 실시하였다. 이러한 비 콜라겐 물질의 제거는 콜라겐 제품 순도를 증가시킬 수 있으며 악취나 부패의 원인을 제거하여 안정성이 향상된 제품을 만들 수 있게 된다.To the precipitate obtained in Example 1) was added 1-10 times (w / v) of 4 ℃ 0.01 ~ 2M basic solution (sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, sodium hypochlorite, etc.) Stir in a -48 hr refrigerator. In the present invention, in order to simplify the conditions of the present invention, 10 times (w / v) of 1 M sodium hydroxide was added, followed by stirring for 24 hours. The stirred sodium hydroxide solution was centrifuged at 10,000 × g / 30 minutes (4 ° C.) to remove supernatants, which are non-collagen substances, and suspended solids such as fat in the upper layer. This washing with sodium hydroxide was repeated twice. Removal of these non-collagen substances can increase the purity of collagen products and eliminate the cause of odor or rot to make products with improved stability.
실시예Example 3) 콜라겐 추출단계 3) Collagen Extraction Step
상기 실시예 2)의 잔사를 로타리에바포레이터(HAHNSHIN[HS-2005S], 한국)를 이용하여 잔사 표면의 물기가 없어질 때까지 감압 건조시킨 후, 4℃로 냉각시켜 둔 0.1~2M 농도의 산성 용액(초산, 포름산, 구연산 등)을 1~20배(w/v)량을 가하여 24~48hr 냉장실(4℃)에서 교반하며 콜라겐을 추출하였다. 본 발명에서는 1M 초산용액을 10배수(w/v)첨가하여 24시간 냉장실에서 교반하는 것으로 가용화시켰다. 콜라겐이 추출된 용액을 10,000xg/10분(4℃)간 원심분리하였으며, 상층액을 분취하여 최종농도 5-20%(v/w)가 되도록 염화나트륨을 첨가한 후 10-120분간 실온에 정치하였다. 본 발명에서는 10% 염화나트륨을 첨가한 후 60분간 정치하는 것으로 하였다. 이 용액을 30,000xg/20분(4℃)간 원심분리 하였으며, 상등액을 제거하고 침전물을 콜라겐 농축물로 수득하였다. The residue of Example 2) was dried under reduced pressure using a rotary evaporator (HAHNSHIN [HS-2005S], Korea) until the moisture on the surface of the residue disappeared, and then cooled to 4 ° C. at a concentration of 0.1 to 2 M. 1 to 20 times (w / v) of an acidic solution (acetic acid, formic acid, citric acid, etc.) was added, and the collagen was extracted with stirring in a 24-48 hr refrigerator (4 ° C). In the present invention, 1M acetic acid solution was solubilized by adding 10-fold water (w / v) and stirring in the refrigerator for 24 hours. The collagen extracted solution was centrifuged at 10,000 × g / 10 min (4 ° C.), the supernatant was aliquoted, and sodium chloride was added to a final concentration of 5-20% (v / w), followed by standing at room temperature for 10-120 min. It was. In the present invention, the mixture was allowed to stand for 60 minutes after adding 10% sodium chloride. This solution was centrifuged for 30,000 × g / 20 min (4 ° C.), the supernatant was removed and the precipitate was obtained as a collagen concentrate.
실시예Example 4) 4) 탈염Desalination 및 농축 단계 And concentration step
상기 실시예 3)에서 수득한 침전물에 증류수를 첨가하여 잘 분산시킨 후, 셀룰로오스 한외여과막(Cellu sep, 분자량 3,500)에 충진시킨 후, 48시간 이상 증류수를 이용하여 4℃에서 투석하였다. 투석외액은 1일 2회 이상 교환하였으며, 투석이 완료된 콜라겐 용액은 동결건조의 방법으로 콜라겐 분말을 수득하였다. After distilled water was added to the precipitate obtained in Example 3) to disperse well, the cellulose ultrafiltration membrane (Cellu sep, molecular weight 3,500) was filled and dialyzed at 4 ° C. using distilled water for 48 hours or more. The dialysis solution was exchanged at least twice a day, and the collagen solution after dialysis was obtained by lyophilization to obtain collagen powder.
실시예Example 5) 부위별 콜라겐의 생산량 5) Production amount of collagen by site
콜라겐함량 분석은 Kurt Kolar의 방법(1990, J. Assoc. Off. Anal. Chem.)에 따라 Erlemyer flask에 시료 4g에 300ml H2SO4를 첨가하고 뚜껑을 닫은 후 105℃ drying oven에서 16시간 동안 가열하였다. 500ml 플라스크에 넣고 희석한 후 100ml 원심분리 튜브에 용액을 여과하였다. 여과액 5ml를 넣고 100ml로 희석한 후 시험관에 희석액 2ml을 넣고 Oxidant 용액 1ml를 더 첨가하고 교반하여 20분간 상온에서 정치하였다. 각 시험관에 발색시약을 첨가하고 혼합한 다음 60℃의 water bath에서 15분간 침지 후 냉각하였다. 시험관을 건조시킨 후 558nm에서 흡광도를 측정하였다. 오리발 및 오리날개를 상기 실시예 1-4의 방법으로 각각 생산한 결과, 표 1과 같은 회수량을 보였다.Collagen content analysis was performed by adding Kurt Kolar's method (1990, J. Assoc. Off.Anal. Chem.) To the Erlemyer flask, adding 300 ml H 2 SO 4 to 4 g of the sample and closing the lid for 16 hours in a 105 ° C drying oven. Heated. After dilution in a 500 ml flask, the solution was filtered through a 100 ml centrifuge tube. 5 ml of the filtrate was diluted to 100 ml, 2 ml of the diluted solution was added to the test tube, and 1 ml of the Oxidant solution was further added and stirred to stand at room temperature for 20 minutes. Color test reagents were added to each test tube, mixed, and then cooled in a water bath at 60 ° C. for 15 minutes. After drying the test tube, the absorbance was measured at 558 nm. The flippers and the wings were produced by the method of Example 1-4, respectively, and showed the recovery amount shown in Table 1.
오리발의 경우 오리 날개에 비해 3.70배 많이 회수되었으며, 이는 오리발에서 수율이 높다는 사실을 알 수 있다.The flippers were recovered 3.70 times higher than the duck wings, which indicates that the flippers have a high yield.
실시예Example 6) 부위별 콜라겐의 조성 6) Composition of collagen by site
SDS-PAGE는 Laemmli(1970, Nature)의 방법을 준용하여 실시하였다. 도면 1에서 확인된 바와 같이, 분자량 200, 140, 120 kDa의Type I형의 콜라겐이 대부분이었으며, Type III 콜라겐도 다량으로 함유되어 있는 전형적인 동물성 콜라겐인 것으로 확인되었다(도 1. 표준물질의 분자량(맨 왼쪽) : 위로부터 170, 130, 95, 72, 55, 43, 34, 26 kDa). SDS-PAGE에 의한 오리 부산물의 콜라겐 조성과 닭의 날개 및 연골의 콜라겐 조성은 유사한 경향을 나타내었으며(농림부, GA0350-0225), 주요 콜라겐이 Type I인 것으로 나타났다. 본 발명의 분석 결과, 본 발명에 의한 제조방법은 오리 부산물의 콜라겐을 효율적으로 추출할 수 있는 것이며, 동물성 콜라겐의 주요 성분인 Type I 및 III형 콜라겐을 다량으로 생산하여 산업적으로 활용할 수 있는 발명을 개발하였다고 확신한다.SDS-PAGE was carried out by applying the method of Laemmli (1970, Nature ). As confirmed in FIG. 1, most of Type I collagen having a molecular weight of 200, 140, and 120 kDa, and was found to be typical animal collagen containing a large amount of Type III collagen (Fig. 1. Leftmost): 170, 130, 95, 72, 55, 43, 34, 26 kDa) from above). Collagen composition of duck by-products and collagen composition of chicken wings and cartilage by SDS-PAGE showed similar trends (Ministry of Agriculture, GA0350-0225), and the main collagen was Type I. As a result of the analysis of the present invention, the production method according to the present invention is capable of efficiently extracting the collagen of the by-product of duck, and the invention that can be industrially produced by producing a large amount of type I and III collagen, which is a major component of animal collagen I am sure it has been developed.
실시예Example 7) 콜라겐 용해도 측정 7) Collagen Solubility Measurement
콜라겐 농도를 0-1%가 되도록 조절한 후 상온에서 2시간 교반하여 가용화하였으며, 그 후 10,000xg/30min 원심분리한 후 상층액 중의 단백질 농도를 정량(Markwell 등, Anal. Biochem., 1978)하여 전체 단백질에 대한 상층액 중의 단백질 함량을 백분율로 계산하여 용해도를 산출하였다. 즉, 용해도는 다음과 같이 계산하였다.After adjusting the collagen concentration to 0-1%, it was solubilized by stirring at room temperature for 2 hours. After centrifugation at 10,000xg / 30min, the protein concentration in the supernatant was quantified (Markwell et al., Anal. Biochem., 1978). Solubility was calculated by calculating the protein content in the supernatant relative to the total protein as a percentage. That is, the solubility was calculated as follows.
용해도(%) = (상층액의 단백질 농도/총 단백질 농도) X 100Solubility (%) = (protein concentration of supernatant / total protein concentration)
콜라겐 용해도의 경우, 콜라겐 농도 0.3% 이상이 될 경우, 서서히 용해도가 감소하기 시작하였으며, 콜라겐 농도 0.4% 이상에서는 용해도가 급격히 감소하는 경향을 나타내었다(도 2). 이러한 경향은 오리발과 오리날개가 유사한 경향을 나타내었으며, 용해도 또한 거의 차이가 없는 것으로 나타났다. 따라서 이후 본 발명의 콜라겐을 이용할 경우 액상 제품을 개발할 경우 콜라겐 농도 0.3-0.5% 사이에서 사용하는 것이 최적일 가능성이 제시되었다. 그러나, 본 발명에서는 순수한 증류수에 대한 용해도를 검증한 것으로서, 기타 용매를 사용하여 용해시킬 경우, 이러한 용해성은 더욱 증가시킬 수 있으리라 생각한다.In the case of collagen solubility, when the collagen concentration was 0.3% or more, the solubility began to decrease gradually, and at the collagen concentration 0.4% or more, the solubility tended to decrease rapidly (FIG. 2). This tendency showed similar trends between flippers and duck wings, and solubility also showed little difference. Therefore, when using the collagen of the present invention, when developing a liquid product, it was suggested that it is optimal to use between 0.3-0.5% of the collagen concentration. However, in the present invention, the solubility in pure distilled water is verified, and it is thought that this solubility can be further increased by dissolving using other solvents.
실시예Example 8) 탁도 측정 8) Turbidity Measurement
탁도는 콜라겐 농도를 0-1%가 되도록 조절한 후 상온에서 2 시간동안 교반한 후 흡광도를 260nm에서 측정하였다. 그 결과, 0.2% 이상이 되면서 탁도가 증가하는 경향을 나타내었으며, 이후 급격한 증가 추세를 보였다(도 3). 이는 도 2의 결과에서 0.2-0.3% 이상에서 용해도가 급격히 감소하는 경향과 유사한 것으로 나타났다.
Turbidity was adjusted to a collagen concentration of 0-1%, and then stirred at room temperature for 2 hours, and then absorbance was measured at 260 nm. As a result, the turbidity increased as it became 0.2% or more, and then showed a sharp increase trend (FIG. 3). This is similar to the tendency of the solubility decreases more than 0.2-0.3% in the result of FIG.
Claims (2)
1) 오리발 또는 오리날개의 뼈를 제거한 후, 껍질과 함께 각각 작은 크기로 세절한 후 급냉시키는 원료 전처리 단계;
2) 염기성 물질을 이용하여 표백 및 과도한 지방을 제거하는 단계;
3) 산 및 염을 이용하여 가용성 콜라겐 추출물을 제조하는 단계;
4) 추출에 사용한 염을 제거하는 탈염단계; 및
5) 농축 건조하여 콜라겐 함유 건조물을 얻는 건조공정.Method for producing a duck collagen extract comprising the following steps, characterized in that the extraction and production of collagen using a flippers or duck wings:
1) the raw material pretreatment step of removing the bones of the flippers or duck wings, and then slicing them into small pieces with shells and quenching them;
2) removing bleach and excess fat using a basic substance;
3) preparing a soluble collagen extract using an acid and a salt;
4) desalting to remove salt used for extraction; And
5) A drying step of obtaining a collagen-containing dried product by concentrated drying.
A liquid product containing 0.3-0.5 mass% of duck collagen extract prepared by the method according to claim 1.
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| KR101336011B1 (en) * | 2013-02-22 | 2013-12-02 | 윤형묵 | Health supplementary food made of duck's feet and method thereof |
| KR101409205B1 (en) * | 2012-07-18 | 2014-06-20 | 영농조합법인 시.케이.푸드 | Making method of collagen food using duck feet |
| KR101489916B1 (en) * | 2013-04-10 | 2015-02-06 | 전북대학교산학협력단 | A method for extracting high purity collagen from animal byproducts |
| KR20180076478A (en) * | 2016-12-28 | 2018-07-06 | 전북대학교산학협력단 | PLGA/Hydroxyapatite hybrid bone graft containing duck's feet-derived collagen and a fabrication method of it |
| CN110384212A (en) * | 2018-04-19 | 2019-10-29 | 沈阳一合食品有限公司 | A kind of spicy duck wing product formula |
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| KR890001815B1 (en) * | 1986-11-28 | 1989-05-25 | 한국과학 기술원 | Process for collagen |
| AUPS242702A0 (en) * | 2002-05-21 | 2002-06-13 | Colltech Australia Limited | Improved method for the extraction and purification of collagen |
| KR100497666B1 (en) * | 2003-05-02 | 2005-07-01 | 주식회사 이에스바이오텍 | Extraction of edible or cosmetic collagen from the bone or horn of animals |
| KR100892605B1 (en) * | 2007-12-18 | 2009-04-08 | 주식회사 정풍 | Producing method of extract for condiment containing much collagen from chicken feet and the extract |
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| KR101409205B1 (en) * | 2012-07-18 | 2014-06-20 | 영농조합법인 시.케이.푸드 | Making method of collagen food using duck feet |
| KR101336011B1 (en) * | 2013-02-22 | 2013-12-02 | 윤형묵 | Health supplementary food made of duck's feet and method thereof |
| KR101489916B1 (en) * | 2013-04-10 | 2015-02-06 | 전북대학교산학협력단 | A method for extracting high purity collagen from animal byproducts |
| KR20180076478A (en) * | 2016-12-28 | 2018-07-06 | 전북대학교산학협력단 | PLGA/Hydroxyapatite hybrid bone graft containing duck's feet-derived collagen and a fabrication method of it |
| CN110384212A (en) * | 2018-04-19 | 2019-10-29 | 沈阳一合食品有限公司 | A kind of spicy duck wing product formula |
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