KR102084950B1 - Method for producing liquid product having high content of water-soluble tannin of astringent persimmon and persimmon peel by complex treatment of ultra high pressure extraction and enzyme - Google Patents
Method for producing liquid product having high content of water-soluble tannin of astringent persimmon and persimmon peel by complex treatment of ultra high pressure extraction and enzyme Download PDFInfo
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- KR102084950B1 KR102084950B1 KR1020170154644A KR20170154644A KR102084950B1 KR 102084950 B1 KR102084950 B1 KR 102084950B1 KR 1020170154644 A KR1020170154644 A KR 1020170154644A KR 20170154644 A KR20170154644 A KR 20170154644A KR 102084950 B1 KR102084950 B1 KR 102084950B1
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- persimmon
- enzyme
- ultra
- water
- high pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
- B01D35/02—Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B5/00—Other centrifuges
- B04B5/10—Centrifuges combined with other apparatus, e.g. electrostatic separators; Sets or systems of several centrifuges
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- Chemical & Material Sciences (AREA)
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Abstract
본 발명은 (a) 떫은 감 또는 감 껍질을 건조한 후 분쇄하여 감 분말을 제조하는 단계; (b) 상기 (a)단계의 제조한 감 분말에 물을 첨가한 혼합물을 초고압 추출하는 단계; (c) 상기 (b)단계의 초고압 추출한 추출물에 효소를 첨가한 후 가수분해하는 단계; 및 (d) 상기 (c)단계의 가수분해한 추출물을 가열한 후 원심분리한 상등액을 살균 및 여과하는 단계를 포함하여 제조하는 것을 특징으로 하는 수용성 탄닌을 고농도로 함유하는 감 추출물의 제조방법 및 상기 방법으로 제조된 수용성 탄닌을 고농도로 함유하는 감 추출물에 관한 것이다.The present invention comprises the steps of (a) drying persimmon persimmon or persimmon peel to produce persimmon powder; (b) ultra-high pressure extraction of the mixture of water added to the persimmon powder prepared in step (a); (c) hydrolyzing the enzyme after adding the enzyme to the ultra-high pressure extract of step (b); And (d) heating the hydrolyzed extract of step (c), and then sterilizing and filtering the supernatant obtained by centrifugation, and producing a persimmon extract containing a high concentration of water-soluble tannins. It relates to a persimmon extract containing a high concentration of water-soluble tannin prepared by the above method.
Description
본 발명은 떫은 감 또는 감 껍질의 초고압 추출 및 효소의 복합 처리에 의한 감 수용성 탄닌을 고농도로 함유하는 감 추출물의 제조방법 및 상기 방법으로 제조된 감 수용성 탄닌을 고농도로 함유하는 감 추출물에 관한 것이다.The present invention relates to a method for producing persimmon extracts containing a high concentration of persimmon water-soluble tannins by ultra-high pressure extraction of persimmon or persimmon peel and complex treatment of enzymes, and to persimmon extracts containing a high concentration of persimmon water-soluble tannins prepared by the above method. .
감은 우리나라에서 재배 면적으로나 생산량으로 볼 때 매우 중요한 위치를 차지하고 있는 과실로서 재배에 큰 어려움 없이 생산 농가의 소득에 일조하고 있는 작목이다. 감은 포도당, 과당 등의 당류와 비타민이 풍부한 알칼리성 식품으로 장의 수축과 장 분비를 촉진하고 기침을 멎게 하는 효능 등이 알려져 있으며, 약리작용에 대한 효능은 동의보감과 본초강목 등의 여러 고문헌에도 언급되고 있으며 고혈압, 동맥경화, 심장 및 신장병 등의 순환기 질환에 효능과 비타민 A, C, D 및 엽록소를 풍부하게 함유하고 그 외 B1, 판토텐산, 엽산의 함유량도 많아 위궤양, 십이지장 및 당뇨병 등의 만성질환과 암 예방 효과가 있다고 알려있다.Persimmon is a fruit that occupies a very important position in terms of cultivation area and output in Korea. Persimmon is an alkaline food rich in sugars such as glucose and fructose and vitamins. It is known to promote intestinal contraction, intestinal secretion, and cough-stopping effect. It is effective in circulatory diseases such as hypertension, arteriosclerosis, heart and kidney disease, and it is rich in vitamins A, C, D, and chlorophyll, and also contains a lot of B 1 , pantothenic acid, and folic acid, which can cause chronic diseases such as gastric ulcer, duodenum and diabetes. It is said to be effective in preventing cancer.
국내에서 생산되는 감은 크게 단감과 떫은 감으로 구별되며, 감 과실을 이용한 대표적인 식품으로는 곶감, 연시, 수정과, 건과, 감식초 등이 생산되고 있으나, 대부분이 곶감 생산에 사용되고 있다. 떫은 감의 생산량 중 곶감으로 활용되는 양은 약 117,506 톤 이상으로 예상되며, 감 껍질 중량은 16%로 곶감을 만들 때 버려지는 감 껍질의 양은 연간 약 18,800 톤 이상으로 추정된다. 특히 우리나라 감 주산지에서 감 과수의 증산으로 감 수확량이 증가하고 있고 이에 따른 곶감과 감말랭이 등 감 가공품의 증가와 더불어 폐기되는 감 껍질의 양도 증가하고 있다. 불량 감과 감가공품을 제조한 후 많은 양의 감 껍질의 상당량이 폐기되고 있는 실정으로 길가에 방치되어 환경오염 및 악취를 발생시키고 있다.Persimmons produced in Korea are largely divided into sweet persimmon and persimmon persimmon. Representative foods using persimmon fruit are dried persimmon, yeast, fertilized fruit, dried fruit and persimmon vinegar, but most of them are used for producing persimmon. The amount of persimmon produced in persimmon is estimated to be more than 117,506 tons, and the persimmon shell weight is 16%. In particular, persimmon yield is increasing due to the increase in persimmon fruit production in persimmon production in Korea. As a result, persimmon skins such as dried persimmons and persimmons are increasing. After manufacturing the defective persimmon and processed products, a large amount of persimmon peel is discarded and is left by the roadside to generate environmental pollution and odor.
감의 껍질 중에는 비타민 A 활성을 나타내는 카로티노이드 성분과 과육 중의 폴리페놀 성분, 펙틴을 비롯한 식이섬유 등의 천연 항노화, 항산화, 항암 작용 등의 다양한 생리활성 성분들이 다량 존재하며, 감 껍질에는 총 폴리페놀의 함량이 44.07~196.98 mg%이며, 그 중 플라보노이드 함량이 36.71~60.79 mg% 함유되어 있고 또한 카로티노이드 등의 색소 성분과 탄닌 등의 폴리페놀 및 식이섬유소가 풍부하여 활용가치가 높다. 감에는 카테킨(catechin), 에피카테킨(epicatechin), 에피카테킨갈레이트(epicatechingallate), 에피갈로카테킨(epigallocatechin), 에피갈로카테킨갈레이트(epigallocatechingallate), 에투린닌산(etulinin acid) 등과 같은 기능성 페놀화합물이 다량 함유되어 있으며, 이들 물질은 항산화기능, 노화방지, 심혈관계 질환 예방 및 항암효과가 있다고 보고됐다. 최근 떫은 감의 떫은맛을 내는 탄닌은 수렴성이나 지혈작용 등의 약리적 효과와 더불어 항산화능, 아질산염 제거능 및 항균효과가 뚜렷하고 항종양작용 및 중금속 제거능과 같은 생리활성이 보고되었다.The persimmon peel contains a large amount of various physiologically active ingredients such as carotenoids, which show vitamin A activity, polyphenols in the flesh, pectin, and other natural anti-aging, antioxidant, and anticancer activities. The content of is 44.07 ~ 196.98 mg%, among which flavonoid content is 36.71 ~ 60.79 mg% and also rich in pigment components, such as carotenoids and polyphenols and dietary fiber, such as tannins, high utilization value. Persimmon contains functional phenolic compounds such as catechin, epicatechin, epicatechin gallate, epigallocatechin, epigalallocatechingallate, and etulinin acid. High in content, these substances have been reported to have antioxidant, anti-aging, cardiovascular and anti-cancer effects. In recent years, tannins, which have astringent taste, have significant anti-oxidative, nitrite-removing, and antimicrobial effects, as well as pharmacological effects such as astringent and hemostatic effects, and physiological activities such as anti-tumor and heavy metal removal.
탄닌은 탄수화물과 단백질을 강하게 결합하는 비교적 높은 분자량을 가진 페놀성 대사산물의 독특한 그룹으로, 탄닌의 화학 구조식 또는 탄닌의 용해도나 추출능으로 구별한다. 탄닌의 구조는 매우 복잡하며, 갈산(gallic acid)이나 엘라직산(ellagic acid) 등으로 된 가수분해형 탄닌과 중합하여 물에 불용성인 플로바펜(plobaphene)을 형성하는 축합형 탄닌으로 분류된다. 가수분해형 탄닌에는 갈산(gallic acid)과 당이 결합하여 이루어진 갈로탄닌(gallotannin)이나 엘라직산(ellagic acid)과 당이 결합한 헥사하드로시디페닉산(hexahydroxydiphenic acid)으로 이루어진 엘라직탄닌(ellagitannin)이 있다. 감에 함유되는 탄닌은 에피카테킨(epicatechin), 카테킨-3-갈레이트(catechin-3-gallate), 에피갈로카테킨( epigallocatechin), 갈로카테킨(gallocatechin-3-gallate)이 1:1:2:2의 비로 결합한 고분자 화합물로 과실 내 탄닌 세포에 대량 함유되어 있다. 감의 탈삽은 탄닌물질의 중합에 의한 불용화에 기인하는 것으로 조직 내에 집적하는 아세트알데히드(acetaldehyde)의 작용에 의한 것이라고 짐작된다. 떫은 감을 에탄올 처리하면 조직 내 알코올 탈수소 효소의 작용에 의해 쉽게 아세트알데히드가 생성하여 탄닌이 불용화하여 탈삽된다. 프로안토시아니딘(Proanthocyanidins)은 프로시아니딘(procyanidin), 프로델피니딘(prodelphinidin), 프로퍼라고니딘(propelargonidin)이 있고, 프로시아니딘(procyanidin) 형태로 가장 많이 존재하고 산성 상태에서 열을 가하면 시아니딘(cyanidin)과 (-)-에피카테킨(epicatechin)으로 가수분해된다. 또한, 프로안토시아니딘(proanthocyanidins)은 높은 항산화능을 나타내고 유리기의 제거 특성은 심장혈관계 질병과 암, 혈액응고를 감소하는 효과와 요로감염증의 보호능이 있다. 현재 탄닌을 분리하는 방법으로는 유기용매와 유기산을 혼합하여 분리하는 방법과, 유기용매와 초음파 처리를 통한 탄닌 분리 방법이 알려져 있다. 이들 감 탄닌은 강장 작용, 피부보호 작용, 항암 작용뿐만 아니라 지질의 과산화를 방지하는 항산화 성분, 소취, 피부미용 효과 및 항균 작용 등의 효과가 알려짐으로써 관련한 천연물 내 탄닌의 분리와 관련제품 생산이 요구되고 있다.Tannins are a unique group of relatively high molecular weight phenolic metabolites that strongly bind carbohydrates and proteins and are distinguished by their chemical structural formula or their solubility or extractability. The structure of tannins is very complex and is classified as condensed tannins, which are polymerized with hydrolyzed tannins, such as gallic acid or ellagic acid, to form insoluble in water plobaphene. Hydrolyzed tannins include gallotannin, which consists of gallic acid and sugar, or ellagitannin, which consists of hexahydroxydiphenic acid, which combines ellagic acid and sugar. There is this. Tannins contained in persimmon are epicatechin, catechin-3-gallate, epigallocatechin, and gallocatechin-3-gallate 1: 1: 2: 2 It is a high molecular compound bound by the ratio of and is contained in large quantities in fruit tannin cells. Persimmon desorption is due to insolubilization by polymerization of tannins and is believed to be due to the action of acetaldehyde that accumulates in the tissues. Ethanol treatment of young persimmon is easily produced by acetaldehyde by the action of alcohol dehydrogenase in tissues, insolubilized and de-tanned. Proanthocyanidins are procyanidin, prodelphinidin, and propelargonidin, which are most present in the form of procyanidin, and cyanidin when heated in an acidic state. ) And (-)-epicatechin. In addition, proanthocyanidins have a high antioxidant activity and free radical scavenging properties reduce cardiovascular disease, cancer and blood coagulation and protect urinary tract infections. Currently, as a method of separating tannins, a method of mixing and separating an organic solvent and an organic acid and a method of separating tannins through an organic solvent and ultrasonication are known. These mutant tannins are known for their tonic, skin-protective and anti-cancer effects, as well as antioxidants that prevent peroxidation of lipids, deodorant, skin care and antimicrobial effects. It is becoming.
감 말랭이 및 곶감 등 감 가공품을 생산하는 과정에서 생성되는 감 껍질은 사용되는 감의 20%에 달하며 대부분 폐기되고 있는 실정이며, 현재로서는 활용방안 및 관련기술의 개발이 미흡한 상황이다. 감 껍질은 표면의 왁스층과 카로티노이드 성분으로 결합되어 있는 지용성 과피 조직과 폴리페놀 등의 탄닌과 펙틴 등의 식이섬유 및 당질로 구성되어 있는 과육 부분이 강하게 결합되어 있는 이형질적인 소재로서 특히 발효 제품이나 식품 소재 등으로 활용하는데 걸림돌이 되므로 이의 제품 활용과 기술개발이 많지 않다. 따라서 떫은 불량 감 및 감 가공 현장에서 대량으로 발행하는 감 껍질을 소재화하기 위하여 농가나 단위 농협 등에서 쉽게 활용할 수 있는 감 껍질 중의 유용 조직 및 성분을 효율적으로 분리하는 전처리 기술이 필요하지만 현재까지 기술 개발이 미흡한 실정이다.Persimmon skin produced in the process of producing persimmon dried products such as persimmon dried persimmon and dried persimmon is 20% of the persimmon used, and most of them are discarded. Currently, there is insufficient development of utilization methods and related technologies. Persimmon peel is a heterogeneous material with strong bonding of fat-soluble skin tissue combined with surface wax layer and carotenoid component, and pulp part composed of dietary fiber and sugar such as tannin such as polyphenol and pectin. There is not much use of product and technology development because it is an obstacle to use as material. Therefore, in order to materialize persimmon shells that are issued in large quantities at persimmons and persimmon processing sites, pretreatment technology is required to efficiently separate useful tissues and components in persimmon shells that can be easily used by farmers or unit agricultural cooperatives. This is insufficient.
감 탄닌에 관한 선행 기술로서는 한국등록특허 제10-0758236호는 감으로부터 탄닌의 분리방법에 관한 것으로, 감에 알코올류의 유기용매와 유기산을 이용하여 탄닌을 분리하는 기술과 분리시 추가적으로 초음파를 처리하는 방법에 관한 기술을 개시하였고, 한국등록특허 제10-1475328호에서는 축합형 탄닌을 함유하는 천연염료 제조방법에 관한 것으로, 축합형 탄닌을 함유하는 염료를 제조하는 방법과 천연염료 조성물 및 분말화 과정에 관한 것을 개시하였으나, 본 발명은 감과 감 껍질 등에서 탄닌 성분을 별도로 분리하여 탄닌 성분만을 특정 짓고자 한 것이 아니라, 본 발명에서 제시하는 별도의 처리를 통하여 불용성 탄닌을 최대한 제거하고 수용성 탄닌 성분이 고농도로 함유되어 제조되는 액상의 제품에 관한 발명이다. 이에 본 발명에서는 감을 초고압 처리 및 효소 등으로 복합 처리하여 수용성 및 불용성 탄닌을 분리하고 수용성 탄닌을 고농도로 함유하는 액상의 관련 제품을 생산하고자 하는 발명으로서 이에 대한 기술은 고지된 바 없다.As a prior art relating to persimmon tannins, Korean Patent No. 10-0758236 relates to a method for separating tannins from persimmon, and a technique for separating tannins using an organic solvent and an organic acid of alcohol in persimmon and additionally treating ultrasonic waves during separation. Disclosed is a technique relating to the method, Korean Patent No. 10-1475328 relates to a method for producing a natural dye containing a condensed tannin, a method for producing a dye containing a condensed tannin and a natural dye composition and powdered Although the disclosure relates to the process, the present invention is not intended to specify only tannin components by separately separating tannin components from persimmon and persimmon peel, and by removing the insoluble tannins as much as possible by the separate treatment proposed in the present invention. The present invention relates to a liquid product that is contained and manufactured at a high concentration. Therefore, in the present invention, the invention is intended to produce a liquid-related product containing a high concentration of water-soluble tannins by separating the water-soluble and insoluble tannins by complex treatment of persimmon with ultra-high pressure treatment and enzymes and the like has not been disclosed.
본 발명은 상기와 같은 요구에 의해 안출된 것으로서, 본 발명의 목적은 떫은 감 또는 감 껍질 분말을 초고압 및 효소 복합 처리를 이용하여 감 추출물을 제조함으로써, 수용성 탄닌 및 갈산을 고농도로 포함하는 감 추출물의 제조방법을 제공하는 데 있다.The present invention has been made in accordance with the requirements as described above, the object of the present invention by producing a persimmon extract using a thin persimmon or persimmon peel powder using ultra-high pressure and enzyme complex treatment, persimmon extract containing a high concentration of water-soluble tannin and gallic acid It is to provide a method of manufacturing.
상기 과제를 해결하기 위해, 본 발명은 (a) 떫은 감 또는 감 껍질을 건조한 후 분쇄하여 감 분말을 제조하는 단계; (b) 상기 (a)단계의 제조한 감 분말에 물을 첨가한 혼합물을 초고압 추출하는 단계; (c) 상기 (b)단계의 초고압 추출한 추출물에 효소를 첨가한 후 가수분해하는 단계; 및 (d) 상기 (c)단계의 가수분해한 추출물을 가열한 후 원심분리한 상등액을 살균 및 여과하는 단계를 포함하여 제조하는 것을 특징으로 하는 수용성 탄닌을 고농도로 함유하는 감 추출물의 제조방법을 제공한다.In order to solve the above problems, the present invention comprises the steps of (a) producing a persimmon powder by drying and milling persimmon persimmon or persimmon peel; (b) ultra-high pressure extraction of the mixture of water added to the persimmon powder prepared in step (a); (c) hydrolyzing the enzyme after adding the enzyme to the ultra-high pressure extract of step (b); And (d) heating the hydrolyzed extract of step (c), and then sterilizing and filtering the supernatant obtained by centrifugation to prepare a persimmon extract containing a high concentration of water-soluble tannin. to provide.
또한, 본 발명은 상기 방법으로 제조된 수용성 탄닌을 고농도로 함유하는 감 추출물을 제공한다.The present invention also provides a persimmon extract containing a high concentration of water-soluble tannin prepared by the above method.
본 발명은 떫은 불량 감과 감 껍질의 분말을 초고압 처리 및 최적의 효소로 적절한 조건으로 복합 처리하여 수용성 및 불용성 탄닌을 분리하여 수용성 탄닌을 고농도로 함유하는 액상의 제품을 제조할 수 있다. 본 발명에서 획득되는 고농도의 수용성 탄닌 함유 액상 제품은 일상적으로 소취제, 항균제, 살균제, 화장제, 피부보호제, 가죽보호제 및 가구도포제 등의 다양한 용도로 활용할 수 있는 효과가 있다.The present invention can prepare a liquid product containing a high concentration of water-soluble tannins by separating the water-soluble and insoluble tannins by a combination of fine and poor persimmon and persimmon peel powder under ultra-high pressure treatment and the optimum enzyme in the appropriate conditions. The high concentration of water-soluble tannin-containing liquid products obtained in the present invention is effective in various applications such as deodorants, antibacterial agents, fungicides, cosmetics, skin protectors, leather protectants and furniture coatings.
도 1은 본 발명의 제조예 1 및 2의 떫은 감 및 감 껍질을 이용한 수용성 탄닌을 고농도로 함유하는 감 추출물의 제조공정을 보여준다.
도 2는 초고압 추출한 떫은 불량 감에 펙티넥스 울트라 SP-L(Pectinex ultra SP-L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 떫은 불량 감 효소분해물의 수용성 탄닌 함량을 4차원 반응표면분석 결과를 보여준다(수용성 탄닌 함량: 600-700-800 mg/100 g).
도 3은 초고압 추출한 떫은 불량 감에 펙티넥스 울트라 SP-L(Pectinex ultra SP-L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 떫은 불량 감 효소분해물의 불용성 탄닌 함량을 4차원 반응표면분석 결과를 보여준다(불용성 탄닌 함량: 120-150-180 mg/100 g).
도 4는 초고압 추출한 떫은 불량 감에 펙티넥스 울트라 SP-L(Pectinex ultra SP-L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 떫은 불량 감 효소분해물의 갈산 함량을 4차원 반응표면분석 결과를 보여준다(갈산 함량: 20-21-22 mg/100 g).
도 5는 초고압 추출한 떫은 불량 감에 펙티넥스 울트라 SP-L(Pectinex ultra SP-L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 떫은 불량 감 효소분해물의 수용성 탄닌 및 갈산 함량 최적화를 위한 슈퍼임포징(superimposing)된 반응표면분석 결과를 보여준다.
도 6은 초고압 추출한 감 껍질에 비스코자임 L(Viscozyme L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 감 껍질 효소분해물의 수용성 탄닌 함량을 4차원 반응표면분석 결과를 보여준다(수용성 탄닌 함량: 530-570-610 mg/100 g).
도 7은 초고압 추출한 감 껍질에 비스코자임 L(Viscozyme L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 감 껍질 효소분해물의 불용성 탄닌 함량을 4차원 반응표면분석 결과를 보여준다(불용성 탄닌 함량: 300-320-340 mg/100 g).
도 8은 초고압 추출한 감 껍질에 비스코자임 L(Viscozyme L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 감 껍질 효소분해물의 갈산 함량을 4차원 반응표면분석 결과를 보여준다(갈산 함량: 14-16-18 mg/100 g).
도 9는 초고압 추출한 감 껍질에 비스코자임 L(Viscozyme L) 효소 가수분해 조건(효소농도, 반응온도, 반응시간)에 따른 감 껍질 효소분해물의 수용성 탄닌 및 갈산 함량 최적화를 위한 슈퍼임포징(superimposing)된 반응표면분석 결과를 보여준다.Figure 1 shows the manufacturing process of persimmon extract containing a high concentration of water-soluble tannins using a thin persimmon and persimmon peel of Preparation Examples 1 and 2 of the present invention.
Figure 2 is a four-dimensional water-soluble tannin content of the poorly degraded enzyme decomposed according to Pectinex ultra SP-L enzyme hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) in ultra-high pressure extracted poor sense Results of response surface analysis are shown (soluble tannin content: 600-700-800 mg / 100 g).
Figure 3 is a four-dimensional insoluble tannin content of a thin poor sense enzyme decomposed according to Pectinex ultra SP-L enzyme hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) in ultra-high pressure extracted poor quality sense Results of response surface analysis are shown (insoluble tannin content: 120-150-180 mg / 100 g).
Figure 4 is a four-dimensional reaction of the gallic acid content of the poor deficient enzyme decomposed according to the Pectinex ultra SP-L enzyme hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) in the ultra-high pressure extracted poor sense Results of surface analysis are shown (gallic acid content: 20-21-22 mg / 100 g).
FIG. 5 is a water-soluble tannin and gallic acid content optimization of a thin poor persimmon degrading product according to Pectinex ultra SP-L enzymatic hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) The results of superimposed response surface analysis are shown.
6 shows the results of 4D reaction surface analysis on the water-soluble tannin content of persimmon peel enzymatic digestion according to Viscozyme L enzymatic hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) in ultra-high pressure extracted persimmon peel (water solubility) Tannin content: 530-570-610 mg / 100 g).
7 shows the results of 4D reaction surface analysis on the insoluble tannin content of persimmon peel enzyme degraded according to the Viscozyme L enzyme hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) in ultra-high pressure extracted persimmon peel (insoluble) Tannin content: 300-320-340 mg / 100 g).
FIG. 8 shows the results of four-dimensional reaction surface analysis of gallic acid content of persimmon hull enzymatic hydrolyzate according to Viscozyme L enzyme hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) in ultra-high pressure extracted persimmon husk (gallic acid content) : 14-16-18 mg / 100 g).
FIG. 9 is a superimposing method for optimizing the water-soluble tannin and gallic acid content of persimmon hull enzymatic hydrolysates according to Viscozyme L enzyme hydrolysis conditions (enzyme concentration, reaction temperature, reaction time) Shows the result of the response surface analysis.
본 발명의 목적을 달성하기 위하여, 본 발명은In order to achieve the object of the present invention, the present invention
(a) 떫은 감 또는 감 껍질을 건조한 후 분쇄하여 감 분말을 제조하는 단계;(a) drying the dried persimmon or persimmon peel and then grinding to produce persimmon powder;
(b) 상기 (a)단계의 제조한 감 분말에 물을 첨가한 혼합물을 초고압 추출하는 단계;(b) ultra-high pressure extraction of the mixture of water added to the persimmon powder prepared in step (a);
(c) 상기 (b)단계의 초고압 추출한 추출물에 효소를 첨가한 후 가수분해하는 단계; 및(c) hydrolyzing the enzyme after adding the enzyme to the ultra-high pressure extract of step (b); And
(d) 상기 (c)단계의 가수분해한 추출물을 가열한 후 원심분리한 상등액을 살균 및 여과하는 단계를 포함하여 제조하는 것을 특징으로 하는 수용성 탄닌을 고농도로 함유하는 감 추출물의 제조방법을 제공한다.(d) heating the hydrolyzed extract of step (c), and then sterilizing and filtering the supernatant obtained by centrifugation to provide a method for preparing persimmon extract containing a high concentration of water-soluble tannins. do.
본 발명의 감 추출물의 제조방법에서, 상기 (a)단계의 감 분말은 바람직하게는 떫은 감 또는 감 껍질을 45~55℃에서 44~52시간 동안 건조한 후 분쇄하여 제조할 수 있으며, 더욱 바람직하게는 떫은 감 또는 감 껍질을 50℃에서 48시간 동안 건조한 후 분쇄하여 제조할 수 있다. 상기와 같은 조건으로 감 분말을 제조하여 이후 단계인 초고압 추출에 적합한 상태로 감을 전처리할 수 있었다.In the production method of the persimmon extract of the present invention, the persimmon powder of step (a) is preferably dried and pulverized after 44 to 52 hours at 45 ~ 55 ℃ persimmon persimmon peel or persimmon, more preferably The dried persimmon or persimmon peel can be prepared by drying after drying for 48 hours at 50 ℃. Persimmon powders were prepared under the same conditions as described above, and thus the persimmon powder was pretreated in a state suitable for ultra-high pressure extraction.
또한, 본 발명의 감 추출물의 제조방법에서, 상기 (b)단계는 바람직하게는 감 분말에 물을 8~12배량(v/w) 첨가한 혼합물을 80~120 MPa 및 45~55℃에서 3~7시간 동안 초고압 추출할 수 있으며, 더욱 바람직하게는 감 분말에 물을 10배량(v/w) 첨가한 혼합물을 100 MPa 및 50℃에서 5시간 동안 초고압 추출할 수 있다. 상기와 같은 조건으로 초고압 처리함으로써, 추출물의 추출 수율 및 탄닌 함량을 더욱 향상시킬 수 있었다. 또한, 본 발명자는 예비실험 시, 효소 처리한 후 초고압 추출한 감 추출물에 비해 초고압 추출한 후 효소를 처리하는 것이 제조된 감 추출물 내 수용성 탄닌 함량을 더욱 증진시킬 수 있음을 확인할 수 있었다.In addition, in the preparation method of the persimmon extract of the present invention, the step (b) is preferably a mixture of 80 to 120 MPa and 45 ~ 55 ℃ 3 to 8 to 12 times the amount of water (v / w) added to the persimmon powder Ultra high pressure extraction can be performed for ˜7 hours, and more preferably, a mixture obtained by adding 10 times (v / w) of water to the persimmon powder may be ultra high pressure extraction at 100 MPa and 50 ° C. for 5 hours. By ultra-high pressure treatment under the above conditions, it was possible to further improve the extraction yield and tannin content of the extract. In addition, the inventors were able to confirm that the pre-experimental treatment, the enzyme treatment after the ultra-high pressure extraction after the enzyme treatment to enhance the water-soluble tannin content in the produced persimmon extract compared to the ultra-high pressure extraction persimmon extract.
또한, 본 발명의 감 추출물의 제조방법에서, 상기 (c)단계의 효소는 바람직하게는 비스코자임(Viscozyme) 또는 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)일 수 있다. 상기 비스코자임은 Novozyme사의 복합효소제로서 아라바나아제(arabanase), 셀룰라아제(cellulase), β-글루카나아제(β-glucanase), 헤미셀룰라아제(hemicellulase) 및 자일라나아제(xylanase)를 함유하는 효소를 의미한다.In addition, in the preparation method of persimmon extract of the present invention, the enzyme of step (c) may preferably be Biscozyme (Viscozyme) or Pectinex ultra SP-L (Pectinex ultra SP-L). The biskozyme refers to an enzyme containing arabanase, a cellulase, β-glucanase, hemicellulase and xylanase as a complex enzyme of Novozyme. do.
또한, 상기 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)는 아스퍼질러스 아쿨레아투스(Aspergillus aculeatus) 유래 효소로, 폴리갈락투로나아제(polygalacturonase) 및 엔도-β-1,4-갈락타나아제(endo-β-1,4-galactanase)의 특성을 갖는 효소를 의미한다.In addition, the Pectinex ultra SP-L (Pectinex ultra SP-L) is Aspergillus Aculeathus ( Aspergillus aculeatus ) -derived enzymes, which refer to enzymes having properties of polygalacturonase and endo-β-1,4-galactanase.
또한, 본 발명의 감 추출물의 제조방법에서, 상기 (c)단계의 효소 처리는 떫은 감을 초고압 추출한 추출물일 경우, 바람직하게는 추출물에 18,000~30,000 PG/ml 농도의 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)을 추출물 부피대비 2.4~2.8% 첨가한 후 50~60℃에서 7~9시간 동안 가수분해할 수 있으며, 더욱 바람직하게는 추출물에 26,000 PG/ml 농도의 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)을 추출물 부피대비 2.6% 첨가한 후 55℃에서 8시간 동안 가수분해할 수 있다. 또한, 감 껍질을 초고압 추출한 추출물일 경우 효소 처리조건은, 바람직하게는 추출물에 80~120 FBG/ml 농도의 비스코자임(Viscozyme)을 추출물 부피대비 2.5~2.7% 첨가한 후 50~60℃에서 8~9시간 동안 가수분해할 수 있으며, 더욱 바람직하게는 추출물에 100 FBG/ml 농도의 비스코자임(Viscozyme)을 추출물 부피대비 2.6% 첨가한 후 54℃에서 8.5시간 동안 가수분해할 수 있다. 상기와 같은 조건으로 감 초고압 추출물을 효소 처리하는 것이 감의 수용성 탄닌을 더욱 효과적으로 분리할 수 있었다.In addition, in the preparation method of the persimmon extract of the present invention, the enzyme treatment of the step (c) is an ultra-high pressure extract of persimmon persimmon extract, preferably Pectinex Ultra SP-L (Pectinex) of 18,000 ~ 30,000 PG / ml concentration in the extract ultra SP-L) can be hydrolyzed for 7-9 hours at 50-60 ℃ after adding 2.4 ~ 2.8% to the volume of the extract, more preferably Pectex Ultra SP-L of 26,000 PG / ml concentration in the extract (Pectinex ultra SP-L) can be hydrolyzed at 55 ° C. for 8 hours after adding 2.6% of the extract volume. In addition, in the case of extract extracted from persimmon peel with ultra-high pressure, the enzyme treatment condition is preferably 80 to 120 FBG / ml of biscozyme (Viscozyme) to the extract after adding 2.5 to 2.7% to the volume of the extract, and then at 8 to 50 to 60 ° C. The hydrolysis may be hydrolyzed for ˜9 hours, and more preferably, after adding 2.6% of Viscozyme at a concentration of 100 FBG / ml to the extract, it may be hydrolyzed at 54 ° C. for 8.5 hours. Treatment of persimmon ultra high pressure extract under the same conditions as described above could more effectively separate the water-soluble tannins of persimmon.
또한, 본 발명의 감 추출물의 제조방법에서, 상기 (d)단계는 바람직하게는 가수분해한 추출물을 80~90℃에서 10~20분 동안 가열한 후 7,000~9,000 rpm으로 원심분리한 상등액을 60~100℃에서 10~60분 동안 살균한 후 여과할 수 있으며, 더욱 바람직하게는 가수분해한 추출물을 85℃에서 15분 동안 가열한 후 8,000 rpm으로 원심분리한 상등액을 80℃에서 30분 동안 살균한 후 여과할 수 있다. 상기와 같은 처리공정을 통해 효소를 불활성화 시키고, 불용성 탄닌을 분리하고 수용성 탄닌을 고농도로 함유하는 추출물로 제조할 수 있었다.In addition, in the preparation method of persimmon extract of the present invention, the step (d) is preferably a supernatant 60 centrifuged at 7,000 ~ 9,000 rpm after heating the hydrolyzed extract at 80 ~ 90 ℃ for 10-20 minutes After sterilization for 10 ~ 60 minutes at ~ 100 ℃ can be filtered, more preferably, the hydrolyzed extract is heated for 15 minutes at 85 ℃ and then the supernatant centrifuged at 8,000 rpm for 30 minutes at 80 ℃ And then filtered. Through the above treatment process, the enzyme was inactivated, the insoluble tannins were separated, and a extract containing high concentration of water-soluble tannins could be prepared.
본 발명의 감 껍질을 이용한 감 추출물의 제조방법은, 보다 구체적으로는The production method of persimmon extract using the persimmon peel of the present invention, more specifically
(a) 감 껍질을 45~55℃에서 44~52시간 동안 건조한 후 분쇄하여 감 분말을 제조하는 단계;(a) drying the persimmon peel at 45-55 ° C. for 44-52 hours and then grinding to produce persimmon powder;
(b) 상기 (a)단계의 제조한 감 분말에 물을 8~12배량(v/w) 첨가한 혼합물을 80~120 MPa 및 45~55℃에서 3~7시간 동안 초고압 추출하는 단계;(b) ultra-high pressure extraction of the mixture of 8-12 times water (v / w) added to the persimmon powder prepared in step (a) at 80-120 MPa and 45-55 ° C. for 3-7 hours;
(c) 상기 (b)단계의 초고압 추출한 추출물에 80~120 FBG/ml 농도의 비스코자임(Viscozyme)을 추출물 부피대비 2.5~2.7% 첨가한 후 50~60℃에서 8~9시간 동안 가수분해하는 단계; 및(c) adding the Viscozyme of 80-120 FBG / ml concentration to the extract of the ultra-high pressure extract of step (b) 2.5 to 2.7% of the volume of the extract and then hydrolyzing at 50 to 60 ℃ for 8 to 9 hours. step; And
(d) 상기 (c)단계의 가수분해한 추출물을 80~90℃에서 10~20분 동안 가열한 후 7,000~9,000 rpm으로 원심분리한 상등액을 60~100℃에서 10~60분 동안 살균한 후 여과하는 단계를 포함할 수 있으며,(d) the hydrolyzed extract of step (c) was heated at 80-90 ° C. for 10-20 minutes, and then the supernatant centrifuged at 7,000-9,000 rpm was sterilized at 60-100 ° C. for 10-60 minutes. It may include the step of filtering,
더욱 구체적으로는More specifically
(a) 감 껍질을 50℃에서 48시간 동안 건조한 후 분쇄하여 감 분말을 제조하는 단계;(a) drying the persimmon peel at 50 ° C. for 48 hours and then grinding to prepare persimmon powder;
(b) 상기 (a)단계의 제조한 감 분말에 물을 10배량(v/w) 첨가한 혼합물을 100 MPa 및 50℃에서 5시간 동안 초고압 추출하는 단계;(b) ultra-high pressure extraction of the mixture of 10 times (v / w) of water to the persimmon powder prepared in step (a) at 100 MPa and 50 ° C. for 5 hours;
(c) 상기 (b)단계의 초고압 추출한 추출물에 100 FBG/ml 농도의 비스코자임(Viscozyme)을 추출물 부피대비 2.6% 첨가한 후 54℃에서 8.5시간 동안 가수분해하는 단계; 및(c) adding 2.6% of biscozyme (Viscozyme) at a concentration of 100 FBG / ml to the ultra-high pressure extracted extract of step (b) and hydrolyzing at 54 ° C. for 8.5 hours; And
(d) 상기 (c)단계의 가수분해한 추출물을 85℃에서 15분 동안 가열한 후 8,000 rpm으로 원심분리한 상등액을 80℃에서 30분 동안 살균한 후 여과하는 단계를 포함할 수 있다.(d) heating the hydrolyzed extract of step (c) for 15 minutes at 85 ° C. and then sterilizing the supernatant centrifuged at 8,000 rpm for 30 minutes at 80 ° C. and then filtering.
본 발명의 떫은 감을 이용한 감 추출물의 제조방법은, 보다 구체적으로는The production method of persimmon extract using a thin persimmon of the present invention, more specifically
(a) 떫은 감을 45~55℃에서 44~52시간 동안 건조한 후 분쇄하여 감 분말을 제조하는 단계;(a) drying the persimmon persimmon at 45-55 ° C. for 44-52 hours and then grinding to prepare persimmon powder;
(b) 상기 (a)단계의 제조한 감 분말에 물을 8~12배량(v/w) 첨가한 혼합물을 80~120 MPa 및 45~55℃에서 3~7시간 동안 초고압 추출하는 단계;(b) ultra-high pressure extraction of the mixture of 8-12 times water (v / w) added to the persimmon powder prepared in step (a) at 80-120 MPa and 45-55 ° C. for 3-7 hours;
(c) 상기 (b)단계의 초고압 추출한 추출물에 18,000~30,000 PG/ml 농도의 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)을 추출물 부피대비 2.4~2.8% 첨가한 후 50~60℃에서 7~9시간 동안 가수분해하는 단계; 및(c) Pectinex ultra SP-L (Pectinex ultra SP-L) of 18,000 ~ 30,000 PG / ml concentration to the ultra-high pressure extraction of step (b) after adding 2.4 ~ 2.8% of the volume of the extract at 50 ~ 60 ℃ Hydrolysis for 7-9 hours; And
(d) 상기 (c)단계의 가수분해한 추출물을 80~90℃에서 10~20분 동안 가열한 후 7,000~9,000 rpm으로 원심분리한 상등액을 60~100℃에서 10~60분 동안 살균한 후 여과하는 단계를 포함할 수 있으며,(d) the hydrolyzed extract of step (c) was heated at 80-90 ° C. for 10-20 minutes, and then the supernatant centrifuged at 7,000-9,000 rpm was sterilized at 60-100 ° C. for 10-60 minutes. It may include the step of filtering,
더욱 구체적으로는More specifically
(a) 떫은 감을 50℃에서 48시간 동안 건조한 후 분쇄하여 감 분말을 제조하는 단계;(a) drying the persimmon persimmon at 50 ° C. for 48 hours and then grinding to prepare persimmon powder;
(b) 상기 (a)단계의 제조한 감 분말에 물을 10배량(v/w) 첨가한 혼합물을 100 MPa 및 50℃에서 5시간 동안 초고압 추출하는 단계;(b) ultra-high pressure extraction of the mixture of 10 times (v / w) of water to the persimmon powder prepared in step (a) at 100 MPa and 50 ° C. for 5 hours;
(c) 상기 (b)단계의 초고압 추출한 추출물에 26,000 PG/ml 농도의 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)을 추출물 부피대비 2.6% 첨가한 후 55℃에서 8시간 동안 가수분해하는 단계; 및(c) Pectinex ultra SP-L (Pectinex ultra SP-L) of 26,000 PG / ml concentration to the ultra-high pressure extracted extract of step (b) after adding 2.6% of the volume of the extract and hydrolyzed at 55 ℃ for 8 hours step; And
(d) 상기 (c)단계의 가수분해한 추출물을 85℃에서 15분 동안 가열한 후 8,000 rpm으로 원심분리한 상등액을 80℃에서 30분 동안 살균한 후 여과하는 단계를 포함할 수 있다.(d) heating the hydrolyzed extract of step (c) for 15 minutes at 85 ° C. and then sterilizing the supernatant centrifuged at 8,000 rpm for 30 minutes at 80 ° C. and then filtering.
본 발명자는 예비실험에서, 효소 처리한 후 초고압 추출한 감 추출물에 비해 초고압 추출한 후 효소 처리한 감 추출물이 수용성 탄닌 함량을 더욱 고농도로 함유하고 있음을 확인하였다.In the preliminary experiments, the inventors confirmed that the persimmon extract subjected to the ultra high pressure extraction and the enzyme-treated persimmon extract contained the water-soluble tannin content at a higher concentration than the persimmon extract obtained after the enzyme treatment.
본 발명은 또한, 상기 방법으로 제조된 수용성 탄닌을 고농도로 함유하는 감 추출물을 제공한다.
The present invention also provides a persimmon extract containing a high concentration of water-soluble tannin prepared by the above method.
이하, 본 발명의 제조예 및 실시예를 들어 상세히 설명한다. 단, 하기 제조예 및 실시예는 본 발명을 예시하는 것일 뿐, 본 발명의 내용이 하기 제조예 및 실시예에 한정되는 것은 아니다.
Hereinafter, the production examples and examples of the present invention will be described in detail. However, the following Preparation Examples and Examples are merely to illustrate the present invention, the contents of the present invention is not limited to the following Preparation Examples and Examples.
제조예Production Example 1. 떫은 불량 감을 이용한 고농도 수용성 1. High concentration water solubility 탄닌Tannins 함유 감 추출물 Persimmon extract
(a) 세척한 후 이물질을 제거한 떫은 불량 감(부위: 과육+껍질, 품종: 청도산 반시)을 건조기(OF-12GW, JEIO TECH, Korea)를 이용하여 50℃에서 48시간 동안 건조한 후 분쇄기(SMX-30WS, Shinil, Korea)로 분쇄하여 감 분말을 제조하였다.(a) After washing, remove the debris and remove the foreign matter (site: pulp + skin, varieties: Qingdao Banshi) using a dryer (OF-12GW, JEIO TECH, Korea) for 48 hours at 50 ℃ and then grinder ( SMX-30WS, Shinil, Korea) was prepared by grinding the persimmon powder.
(b) 상기 (a)단계의 제조한 감 분말에 물을 10배량(v/w) 첨가한 혼합물을 비닐 팩에 넣어 공기가 들어가지 않도록 밀봉과 동시에 초고압 추출장치(TFS-SL, TOYO KOTASU Co., LTD., Japan)를 이용하여 100 MPa 및 50℃에서 5시간 동안 초고압 추출하였다.(b) a mixture of 10 times (v / w) of water added to the persimmon powder prepared in step (a) in a plastic pack and sealed to prevent air from entering and at the same time an ultra-high pressure extraction device (TFS-SL, TOYO KOTASU Co , LTD., Japan) was extracted at 100 MPa and 50 ℃ for 5 hours.
(c) 상기 (b)단계의 초고압 추출한 추출물에 26,000 PG(Polygalacturonase Units)/ml 농도의 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)을 추출물 부피대비 2.6% 첨가한 후 55℃에서 8시간 동안 가수분해하였다.(c) Pectinex ultra SP-L (Pectinex ultra SP-L) of 26,000 PG (Polygalacturonase Units) / ml concentration to the ultra-high pressure extract of step (b) after adding 2.6% of the extract volume for 8 hours at 55 ℃ During hydrolysis.
(d) 상기 (c)단계의 가수분해한 추출물을 85℃에서 15분 동안 가열하여 효소를 불활성화하고, 8,000 rpm으로 원심분리한 상등액을 80℃에서 30분 동안 살균한 후 1.0 마이크로 필터기를 통과시켜 여과하였다.
(d) the hydrolyzed extract of step (c) was heated at 85 ° C. for 15 minutes to inactivate the enzyme, and the supernatant centrifuged at 8,000 rpm for 30 minutes at 80 ° C. and then passed through a 1.0 micro filter. And filtered.
제조예Production Example 2. 감 껍질을 이용한 고농도 수용성 2. High concentration water soluble using persimmon peel 탄닌Tannins 함유 감 추출물 Persimmon extract
(a) 세척한 후 이물질을 제거한 감 껍질(품종: 청도산 반시)을 건조기(OF-12GW, JEIO TECH, Korea)를 이용하여 50℃에서 48시간 동안 건조한 후 분쇄기(SMX-30WS, Shinil, Korea)로 분쇄하여 감 분말을 제조하였다.(a) After washing, the persimmon peel (variety: Qingdao Banshee) from which foreign matters were removed was dried at 50 ° C for 48 hours using a dryer (OF-12GW, JEIO TECH, Korea), followed by a grinder (SMX-30WS, Shinil, Korea). Persimmon powder was prepared.
(b) 상기 (a)단계의 제조한 감 분말에 물을 10배량(v/w) 첨가한 혼합물을 비닐 팩에 넣어 공기가 들어가지 않도록 밀봉과 동시에 초고압 추출장치(TFS-SL, TOYO KOTASU Co., LTD., Japan)를 이용하여 100 MPa 및 50℃에서 5시간 동안 초고압 추출하였다.(b) a mixture of 10 times (v / w) of water added to the persimmon powder prepared in step (a) in a plastic pack and sealed to prevent air from entering and at the same time an ultra-high pressure extraction device (TFS-SL, TOYO KOTASU Co , LTD., Japan) was extracted at 100 MPa and 50 ℃ for 5 hours.
(c) 상기 (b)단계의 초고압 추출한 추출물에 100 FBG(Fungal Beta-Glucanase Units)/ml 농도의 비스코자임(Viscozyme L.)을 추출물 부피대비 2.6% 첨가한 후 54℃에서 8.5시간 동안 가수분해하였다.(c) 100% FBG (Fungal Beta-Glucanase Units) / ml concentration of biscozyme (Viscozyme L.) was added to the ultra-high pressure extracted extract of step (b), followed by hydrolysis at 54 ° C. for 8.5 hours. It was.
(d) 상기 (c)단계의 가수분해한 추출물을 85℃에서 15분 동안 가열하여 효소를 불활성화하고, 8,000 rpm으로 원심분리한 상등액을 80℃에서 30분 동안 살균한 후 1.0 마이크로 필터기를 통과시켜 여과하였다.
(d) the hydrolyzed extract of step (c) was heated at 85 ° C. for 15 minutes to inactivate the enzyme, and the supernatant centrifuged at 8,000 rpm for 30 minutes at 80 ° C. and then passed through a 1.0 micro filter. And filtered.
비교예Comparative example 1. One. 무처리No treatment 감 분말 Persimmon powder
세척한 후 이물질을 제거한 떫은 불량 감 또는 감 껍질을 건조기(OF-12GW, JEIO TECH, Korea)를 이용하여 50℃에서 48시간 동안 건조한 후 분쇄기(SMX-30WS, Shinil, Korea)로 분쇄하여 떫은 감 분말 또는 감 껍질 분말을 제조하였다.
After cleaning, remove the debris and remove the deteriorated persimmon or persimmon peel with a dryer (OF-12GW, JEIO TECH, Korea) for 48 hours at 50 ℃, and then crush it with a grinder (SMX-30WS, Shinil, Korea). Powder or persimmon peel powder was prepared.
실험예Experimental Example 1. One. 탄닌Tannins 함량 및 통계처리 Content and Statistical Processing
1) 탄닌 함량1) Tannin Content
시료 0.5 mL에 1% K3F3(CN)6 1 mL와 1% FeCl3 1 mL를 첨가하여 혼합한 후 실온에서 5분 동안 반응시킨 후 720 nm에서 흡광도 값을 측정하였다. 탄닌산(tannic acid, Sigma Chemical Co. USA)을 이용하여 표준 검량 곡선을 작성한 후, 탄닌산 등가물(mg TE/100 g)로 나타내었다. 갈산(Gallic acid) 함량은 시료 용액을 0.45 ㎛ 막여과지(membrane filter)로 여과한 후, HPLC(Alliance e2695, Waters Co., Milford, MA, USA)로 분석하였고, 분석조건은 표 1에 나타내었다. 표준품은 갈산(gallic acid, Sigma Chemical Co.)을 이용하여 표준 검량선을 작성한 후 각각의 함량을 계산하였다.
1 mL of 1% K 3 F 3 (CN) 6 and 1 mL of 1% FeCl 3 were added to 0.5 mL of the sample, followed by reaction at room temperature for 5 minutes, and then absorbance at 720 nm was measured. Standard calibration curves were prepared using tannic acid (Snicma Chemical Co. USA) and expressed as tannic acid equivalents (mg TE / 100 g). The gallic acid content was analyzed by HPLC (Alliance e2695, Waters Co., Milford, MA, USA) after filtering the sample solution with 0.45 ㎛ membrane filter, the analysis conditions are shown in Table 1 . As a standard, gallic acid (Sigma Chemical Co.) was used to prepare a standard calibration curve, and the contents of each were calculated.
2) 통계처리 2) Statistical Processing
모든 시험은 3 반복하여 평균값과 표준편차로 결과값을 나타내었으며, 결과의 통계는 SAS(statistical analysis system, Version 9.3) 프로그램을 이용하여 반응표면분석(response surface methodology, RSM)으로 실시하였다. 또한, 매스매티카 프로그램(Mathematica program)을 이용하여 4차원 반응표면분석을 해석하였다. 각 실험군에 대한 유의차 검정은 분산분석한 후 p<0.05 수준에서 Duncans multiple test에 따라 분석하여 비교하였다.
All the tests were repeated three times and the results were expressed as mean values and standard deviations. The statistics of the results were performed by response surface methodology (RSM) using a statistical analysis system (Version 9.3) program. In addition, four-dimensional response surface analysis was analyzed using the Mathematica program. Significant difference test for each experimental group was analyzed according to Duncans multiple test at p <0.05 level after variance analysis.
실시예Example 1. 떫은 감의 초고압 추출 처리에 의한 1. Ultra high pressure extraction process of thin persimmon 탄닌Tannins 함량 비교 Content comparison
비교예 1의 무처리 떫은 감 분말 및 감 껍질 분말과, 비교예 1의 무처리 감 분말에 제조예 1 및 2의 (b)단계의 조건으로 초고압 처리한 시료의 탄닌 함량을 측정하여 그 결과를 표 2에 나타내었다. 떫은 불량 감의 경우, 수용성 탄닌 함량은 비교예 1의 258.66±6.03 mg/100 g에 비하여 초고압 처리 시료는 353.29±5.26 mg/100 g으로 36.6% 이상 높았고, 불용성 탄닌 함량도 비교예 1의 78.01±0.48 mg/100 g에 비하여 초고압 처리 시료 97.17±0.48 mg/100 g으로 24.6% 이상 높게 나타났다.The tannin content of the untreated persimmon powder and the persimmon peel powder of Comparative Example 1 and the untreated persimmon powder of Comparative Example 1 and ultra-high pressure treated samples under the conditions of steps (b) of Preparation Examples 1 and 2 were measured and the results were measured. Table 2 shows. In the case of a poor sense of water, the water-soluble tannin content was 353.29 ± 5.26 mg / 100 g compared to 258.66 ± 6.03 mg / 100 g in Comparative Example 1, which was 36.6% higher, and the insoluble tannin content was 78.01 ± in Comparative Example 1. Compared to 0.48 mg / 100 g, the ultrahigh pressure treated sample was 97.17 ± 0.48 mg / 100 g, which was higher than 24.6%.
또한, 감 껍질의 경우, 수용성 탄닌 함량은 비교예 1의 356.06±5.53 mg/100 g에 비하여 초고압 처리 시료는 457.15±3.19 mg/100 g으로 28.4% 이상 높게 나타났고, 불용성 탄닌 함량도 비교예 1의 153.38±1.82 mg/100 g에 비하여 초고압 처리 시료 194.64±0.42 mg/100 g으로 26.9% 이상 높게 나타나 초고압 처리가 탄닌의 함량을 증대시키는 것으로 나타났다.In the case of persimmon peel, the water-soluble tannin content was higher than 356.06 ± 5.53 mg / 100 g of Comparative Example 1, and the high-pressure treated sample was 457.15 ± 3.19 mg / 100 g, which was 28.4% or more higher, and the insoluble tannin content was also Comparative Example 1 Compared to 153.38 ± 1.82 mg / 100 g of, the ultra high pressure sample 194.64 ± 0.42 mg / 100 g was higher than 26.9%, indicating that the ultra high pressure treatment increases the content of tannin.
함량(mg/100 g)Insoluble Tannin
Content (mg / 100 g)
함량(mg/100 g)Water soluble tannin
Content (mg / 100 g)
함량(mg/100 g)Insoluble Tannin
Content (mg / 100 g)
(무처리 분말)Comparative Example 1
(Untreated powder)
실시예Example 2. 떫은 감의 효소 처리에 의한 2. By enzyme treatment of young persimmon 탄닌Tannins 함량 비교 Content comparison
불량 떫은 감과 감 껍질 분말을 초고압 처리하여 얻어진 추출물에 최적의 효소를 결정하게 위하여 시판용 상업 효소를 선별 시험하였다. 사용된 시판용 상업효소로서 노보자임사(Novo Nordisk Co.)의 셀루클라스트(Celluclast 1.5L), 비스코자임(Viscozyme L), 펙티넥스 울트라 SP-L(Pectinex Ultra SP-L), 펙티넥스 XXL(Pectinex XXL), 알카라아제(Alcalase 2.4 L), 플라보르자임(Flavourzyme 500 MG), 뉴트라제(Neutrase 0.8 L), 프로타멕스(Protamex)를 사용하였다. 효소처리는 초고압 추출 시료 100 mL에 상기의 상업효소를 각각 2%씩 첨가하여 50℃에서 6시간 동안 처리하였다. 처리가 끝난 즉시 효소처리 시료를 85℃에서 15분간 열처리하여 효소를 불활성화하고 원심분리한 후 상등액을 취하여 수용성 탄닌 함량을 측정하였으며, 잔여물에 1% 염산(HCl)이 포함된 80% 메탄올(methanol)을 가하여 충분히 혼합 후 실온에서 2시간 방치 후 원심분리하여 상징액을 불용성 탄닌 시험용액으로 사용하여 측정한 결과는 표 3과 같다.Commercially available commercial enzymes were screened to determine the optimal enzyme for extracts obtained by ultra high pressure treatment of persimmon and persimmon peel powder. Commercial commercial enzymes used were Novozydisk Co., Ltd. (Celluclast 1.5L), Viscozyme L, Pectinex Ultra SP-L, Pectinex XXL ( Pectinex XXL), Alcalase (Alcalase 2.4 L), Flavorzyme 500 MG, Neutrase (0.8 L), Protamex were used. Enzyme treatment was performed by adding 2% of each of the commercial enzymes to 100 mL of the ultra-high pressure extraction sample and treating it at 50 ° C. for 6 hours. Immediately after the treatment, the enzyme-treated samples were heat treated at 85 ° C. for 15 minutes to inactivate the enzyme, centrifuged, and the supernatant was taken to measure the water-soluble tannin content. The residue was treated with 80% methanol (1% hydrochloric acid (HCl)). After mixing sufficiently with methanol), the mixture was left at room temperature for 2 hours, centrifuged and the supernatant was used as an insoluble tannin test solution.
떫은 불량 감 분말을 초고압 처리하여 얻은 추출물에 효소를 처리하여 얻은 가수분해물의 수용성 탄닌 함량은 펙티넥스 울트라 SP-L(Pectinex Ultra SP-L)의 처리구에서 629.44±4.93 mg/100 g으로 가장 높은 함량을 나타내었으며 사용된 효소 간에 유의적인 차이를 보였다. 펙티넥스 울트라 SP-L 효소처리된 가수분해물의 수용성 탄닌 함량은 629.44±4.93 mg/100 g으로 무처리 떫은 감 분말(비교예 1)의 258.66±6.03 mg/100 g보다 약 243.3% 이상 증가하였고, 초고압 처리 시료의 353.29±5.26 mg/100 g보다 78.2% 이상 증가하였다. 불용성 탄닌 함량 또한 펙티넥스(Pectinex Ultra SP-L)의 처리구에서 다른 효소 처리구에 비해 유의적인 차이를 보이며 높은 함량을 나타내었다. 이상의 결과로 펙티넥스 울트라 SP-L(Pectinex Ultra SP-L)로 가수분해시킨 떫은 불량 감 가수분해물의 탄닌 함량이 높은 것으로 나타나 적절한 효소제라 것으로 판단되어 초고압 처리한 떫은 불량 감의 최적 효소제로 선정하여 최적 조건을 설정하기 위하여 다음 단계의 실시예에 사용하였다. The water-soluble tannin content of the hydrolyzate obtained by treating the extracts obtained by ultra high pressure treatment of thin persimmon powder was 629.44 ± 4.93 mg / 100 g in the treatment group of Pectinex Ultra SP-L. And significant difference between the enzymes used. The water-soluble tannin content of the Pectinex Ultra SP-L enzymatic hydrolysate was 629.44 ± 4.93 mg / 100 g, which was about 243.3% higher than 258.66 ± 6.03 mg / 100 g of the untreated persimmon powder (Comparative Example 1), 78.2% more than 353.29 ± 5.26 mg / 100 g of the ultra-high pressure treated sample. Insoluble tannin content was also significantly higher in Pectinex Ultra SP-L treatment than in other enzyme treatments. As a result, 시킨 hydrolyzed with Pectinex Ultra SP-L showed high tannin content of the defective persimmon hydrolyzate. It was used in the next step examples to set the optimum conditions.
또한, 초고압 처리된 감 껍질 추출물을 시판용 각 효소로 처리하여 얻은 가수분해물의 수용성 탄닌 함량은 비스코자임(Viscozyme L)의 처리구에서 595.69±6.14 mg/100 g으로 가장 높은 함량을 나타내었고 효소 종류 간의 유의적인 차이를 보였다. 불용성 탄닌 함량 또한, 비스코자임(Viscozyme L)의 처리구에서 다른 효소 처리구에 비해 유의적인 차이를 보이며 높은 함량을 나타내었다. 초고압 처리된 감껍질 추출물을 비스코자임(Viscozyme L) 효소처리된 가수분해물의 수용성 탄닌 함량은 595.69±6.14 mg/100 g으로 무처리 감 껍질 분말(비교예 1)의 356.06±5.53 mg/100 g 보다 약 67.3% 이상 증가하였고 초고압 처리 시료의 457.15±3.19 mg/100 g보다 30.3% 이상 증가하였다. 이상의 결과로 비스코자임(Viscozyme L)으로 가수분해시킨 감 껍질 가수분해물의 탄닌 함량이 높게 나타나 적절한 효소제로 판단되어 초고압 처리한 감 껍질의 최적 효소제로 선정하여 다음 단계의 실시예에 사용하였다. In addition, the water-soluble tannin content of the hydrolyzate obtained by treating the ultra-high pressure persimmon peel extract with each commercially available enzyme showed the highest content of 595.69 ± 6.14 mg / 100 g in the Viscozyme L treatment, Showed a difference. Insoluble tannin content also showed a significant difference in the treatment of Viscozyme L compared to the other enzyme treatment, and showed a high content. The water-soluble tannin content of Viscozyme L-enzymatic hydrolysates was 595.69 ± 6.14 mg / 100 g of ultrahigh-pressure persimmon peel extract than 356.06 ± 5.53 mg / 100 g of untreated persimmon peel powder (Comparative Example 1). It was increased by more than about 67.3% and increased by more than 30.3% than 457.15 ± 3.19 mg / 100 g of the ultra-high pressure treated sample. As a result, the tannin content of the persimmon peel hydrolyzed by Viscozyme L was high, which was judged to be an appropriate enzyme, and was selected as an optimal enzyme for ultra-high pressure treatment persimmon shell.
실시예Example 3. 반응표면분석법을 이용한 떫은 불량 감의 효소분해 최적화 3. Optimizing Enzymatic Degradation of Young Defects Using Response Surface Methodology
떫은 불량 감 분말을 초고압 처리하여 얻은 추출물에 펙티넥스 울트라 SP-L(Pectinex Ultra SP-L)의 최적 효소처리 조건을 설정하기 위해 효소농도, 반응온도 및 반응시간을 독립변수로 하여 중심합성계획에 의해 표 4와 같이 설계된 20구의 효소처리조건에서 얻어진 탄닌 함량은 표 5와 같다. 표 5의 각각의 결과를 이용하여 반응표면분석을 실시하고, 각 종속변수 즉, 수용성 탄닌, 불용성 탄닌, 갈산(gallic acid) 함량에 대한 회귀식을 얻었다(표 6). 또한, 변수별 최적 효소처리조건과 각 효소분해물의 특성 값을 예측하여 표 7에 나타내었으며, 이들의 4차원 반응표면을 효소농도, 반응온도 및 반응시간을 독립변수로 하여, 도 2~4에 나타내었다.In order to set the optimum enzyme treatment condition of Pectinex Ultra SP-L in extracts obtained from ultra-high pressure treatment of poor persimmon powder, the enzyme concentration, reaction temperature and reaction time were independent variables. Tannin content obtained under 20 enzyme treatment conditions designed as shown in Table 4 is shown in Table 5. Response surface analysis was performed using the results of Table 5, and a regression equation was obtained for each dependent variable, that is, water soluble tannin, insoluble tannin, and gallic acid content (Table 6). In addition, the optimum enzymatic treatment conditions for each variable and the characteristic values of each enzymatic degradation product were predicted and shown in Table 7. The four-dimensional reaction surface of these variables was shown in Figs. Indicated.
1)중심합성계획에 의한 실험조건 번호
1) Test condition number by central synthesis plan
그 결과, 떫은 불량 감을 초고압 처리 후 펙티넥스 울트라 SP-L(Pectinex Ultra SP-L)의 효소처리 조건에 따른 효소분해물의 수용성 탄닌 함량은 308.41~720.67 mg/100 g의 범위로 나타났으며(표 5), 이를 바탕으로 한 수용성 탄닌 함량의 회귀식은 표 6와 같고 R2 값은 0.9272으로 1% 이내의 수준에서 유의성이 확인되었다. 효소처리 조건에 따라 반응표면모델로 예측된 회귀분석결과 임계점이 안장점으로 나타났으며, 능선분석을 하여 최적점을 산출한 결과 최대값은 809.10 mg/100 g이며, 이때의 효소처리 조건은 효소농도 2.37 g/100 mL, 반응온도 59.02℃ 및 반응시간 6.87시간으로 나타났다(표 7). 4차원 반응표면을 통한 효소분해 조건에 따른 불량 감 효소분해물의 수용성 탄닌 함량의 변화는 도 2와 같이 반응 온도가 높을수록 증가하는 것으로 나타났다. 효소분해 처리조건에 대한 영향은 표 8에서와 같이 반응온도의 영향이 가장 크며, 반응시간, 효소농도 순으로 영향을 받는 것으로 나타났다.As a result, the water-soluble tannin content of the enzymatic degradation products according to the enzyme treatment conditions of Pectinex Ultra SP-L after ultra high pressure treatment of the poor defect was in the range of 308.41 ~ 720.67 mg / 100 g (Table 5) Based on this, the regression formula of water-soluble tannin content is shown in Table 6 and the R 2 value was 0.9272, which was found to be significant at a level within 1%. The regression analysis predicted by the response surface model according to the enzyme treatment condition showed the critical point as the saddle point, and the maximum value obtained by the ridge analysis was 809.10 mg / 100 g, and the enzyme treatment condition was enzyme The concentration was 2.37 g / 100 mL, the reaction temperature was 59.02 ° C. and the reaction time was 6.87 hours (Table 7). The change in the water-soluble tannin content of the poor persimmon enzymatic degradation product according to the enzymatic degradation conditions through the four-dimensional reaction surface was increased as the reaction temperature was increased as shown in FIG. 2. As shown in Table 8, the effect on the enzymatic digestion conditions was the most affected by reaction temperature, followed by reaction time and enzyme concentration.
떫은 불량 감을 초고압 처리 후 펙티넥스 울트라 SP-L(Pectinex Ultra SP-L)의 효소를 사용하여 조건별로 처리된 효소분해물의 불용성 탄닌 함량은 65.63~181.50 mg/100 g의 범위로 나타났으며(표 5), 이를 바탕으로 한 회귀식은 표 6와 같다. 불용성 탄닌 함량에 대한 R2값은 0.9515으로 높은 신뢰도를 보였으며, p값은 1% 이내 유의수준을 보였다. 효소처리 조건에 대한 영향에서 불용성 탄닌 함량의 경우 효소처리 온도와 시간에 영향을 크게 받는 것으로 나타났으나, 설정된 범위 내에서 효소농도에 대한 영향은 거의 나타나지 않았다(표 8). 효소처리에 따라 반응표면모델로 예측된 회귀분석 결과 정상점이 안장점으로 나타났으며, 최적점을 산출한 결과 불용성 탄닌 함량의 최대값은 209.23 mg/100 g이고 이때의 발효조건은 효소농도 1.98 g/100 mL, 반응온도 58.18℃ 및 반응시간 8.29시간으로 나타났다(표 7). 실험조건에 따라 얻은 효소분해물의 불용성 탄닌 함량에 대한 반응표면은 도 3에 나타내었으며, 반응온도가 높고, 반응시간이 길수록 증가하는 것으로 나타났다. Insoluble tannin content of enzyme decomposed by the conditions of Pectinex Ultra SP-L after treatment with ultra high pressure was found to be in the range of 65.63 ~ 181.50 mg / 100 g. 5), The regression formula based on this is shown in Table 6. The R 2 value for the insoluble tannin content was 0.9515, showing high reliability, and the p value showed a significant level within 1%. Insoluble tannin content was significantly affected by enzyme treatment temperature and time, but little effect on enzyme concentration within the set range (Table 8). The regression analysis predicted by the reaction surface model according to the enzyme treatment showed that the normal point was the saddle point. The optimum point was calculated and the maximum value of insoluble tannin content was 209.23 mg / 100 g and the fermentation condition was 1.98 g. / 100 mL, the reaction temperature was 58.18 ℃ and the reaction time was 8.29 hours (Table 7). The reaction surface of the insoluble tannin content of the enzymatically obtained product according to the experimental conditions is shown in FIG. 3, and the reaction temperature was increased as the reaction temperature was higher and the reaction time was longer.
떫은 불량 감을 초고압 처리 후 펙티넥스 울트라 SP-L(Pectinex Ultra SP-L)의 효소를 사용하여 처리 조건에 따른 불량 감 효소분해물의 갈산(gallic acid) 함량은 18.51~23.75 ㎍/mL의 범위로 나타났으며(표 5), 이를 바탕으로 한 회귀식은 표 6과 같으며, 이 모델에 대한 회귀식의 R2 값은 0.8858로 1% 이내의 유의성이 인정되었다. 갈산의 함량은 효소농도, 반응시간, 반응온도의 효소처리조건 모두에서 영향을 받고 있는 것으로 나타났으며, 효소농도와 반응온도가 높고, 효소처리 시간이 길어질수록 갈산 함량이 증가하는 것으로 나타났다(표 8). 표 7과 같이 갈산 함량의 예측된 정상점은 최대점으로 최대값이 22.65 ㎍/mL이었고, 이때 효소농도 2.73 g/100 mL, 반응온도 56.71℃ 및 반응시간 6.54시간이었다. 효소분해물의 불용성 탄닌 함량의 효소처리 조건에 따른 4차원 반응표면에서 볼 때 효소농도와 반응온도가 높고 반응시간이 길어질수록 함량이 증가하는 것으로 나타났다(도 4).The gallic acid content of the decomposing enzyme decomposed according to the treatment conditions using the enzyme of Pectinex Ultra SP-L after ultra high pressure treatment of the deficient persimmon was found to be in the range of 18.51 ~ 23.75 ㎍ / mL. (Table 5), and the regression equation based on this is shown in Table 6, and the R 2 value of the regression equation for this model was 0.8858, indicating a significance within 1%. The content of gallic acid was affected by the enzyme concentration, reaction time, and enzyme treatment conditions of the reaction temperature. The content of gallic acid increased as the enzyme concentration, reaction temperature and enzyme treatment time increased. 8). As shown in Table 7, the predicted peak of the gallic acid content was the maximum and the maximum value was 22.65 ㎍ / mL, wherein the enzyme concentration was 2.73 g / 100 mL, the reaction temperature was 56.71 ° C, and the reaction time was 6.54 hours. The insoluble tannin content of the enzymatic degradation product was found to increase as the enzyme concentration and reaction temperature were higher and the reaction time was longer according to the enzymatic treatment conditions (FIG. 4).
(mg/100 g)Water Soluble Tannin Content
(mg / 100 g)
(mg/100 g)Insoluble Tannin Content
(mg / 100 g)
(㎍/mL)Gallic acid content
(Μg / mL)
(℃)Reaction temperature
(℃)
Saddle
Saddle
Max
Reactant
*유의성 10% 이내; **유의성 5% 이내; ***유의성 1% 이내
* Significance within 10%; ** within 5% of significance; *** Significance within 1%
떫은 불량 감을 초고압 처리 후 펙티넥스 울트라 SP-L 최적 효소 처리조건을 설정하기 위하여 수용성 탄닌, 갈산 함량 모두 만족시켜주는 최적 효소 처리조건을 얻고자 각 반응표면을 슈퍼임포징(superimposing)하여 도 5의 겹쳐진 부분으로 나타내었고 표 9에 최적 조건을 나타내었다. 불량 감 효소처리 최적 조건 범위는 효소농도 2.4~2.8 g/100 mL, 반응온도 50~60℃ 및 반응시간 7~8시간으로 나타났다.In order to set the pectinex ultra SP-L optimum enzyme treatment condition after ultra-high pressure treatment to obtain the optimum enzyme treatment condition that satisfies both water-soluble tannin and gallic acid content, superimposing each reaction surface is performed in FIG. The overlapped parts are shown and the optimum conditions are shown in Table 9. The optimum conditions for the treatment of defective persimmon enzyme were 2.4 ~ 2.8 g / 100 mL of enzyme concentration, 50 ~ 60 ℃ of reaction temperature and 7 ~ 8 hours of reaction time.
(최적점)Forecast condition range
(Optimal)
(2.6)2.4 ~ 2.8
(2.6)
(55)50-60
(55)
(8)7-8
(8)
따라서 이와 같은 예측 결과에 대한 모델식의 신뢰성을 확인하기 위하여 예측된 최적 조건 범위 내에서 임의의 조건 즉, 효소농도 2.6 g/100 mL, 반응온도 55℃ 및 반응시간 8시간을 대입하여 실제 효소 처리를 실시하고, 효소분해물의 탄닌 함량 및 갈산 함량을 측정한 결과 예측된 값들과 유사한 수준으로 비교되었다(표 10).Therefore, in order to confirm the reliability of the model equation for this prediction result, the actual enzyme treatment was performed by substituting any conditions within the predicted optimum conditions, that is, enzyme concentration of 2.6 g / 100 mL, reaction temperature of 55 ° C. and reaction time of 8 hours. The tannin content and the gallic acid content of the enzymatic degradation product were measured and compared with the predicted values at a similar level (Table 10).
(mg/100 g)Water Soluble Tannin Content
(mg / 100 g)
(mg/100 g)Insoluble Tannin Content
(mg / 100 g)
(㎍/mL)Gallic acid content
(Μg / mL)
1)반응표면 변화값에 대한 예측식으로 계산된 값 1) Value calculated by the equation for response surface change
2)독립변수의 최적조건: 효소농도 2.6 g/100 mL, 반응온도 55℃, 반응시간 8시간
2) Optimal conditions for independent variables: enzyme concentration 2.6 g / 100 mL,
실시예Example 4. 반응표면분석법을 이용한 감 껍질 효소분해 최적화 4. Optimization of Persimmon Shell Enzyme Degradation Using Response Surface Methodology
감 껍질을 초고압 처리하여 얻은 추출물에 비스코자임(Viscozyme L)의 최적 효소처리 조건을 설정하기 위해 효소농도, 반응온도 및 반응시간을 독립변수로 하여 표 4와 같이 중심합성계획에 의해 설계된 20구의 효소 처리조건에서 얻어진 탄닌 함량은 표 11과 같다. 표 11의 각각의 결과를 이용하여 반응표면분석을 실시하고, 각 종속변수 즉, 수용성 탄닌, 불용성 탄닌, 갈산(gallic acid) 함량에 대한 회귀식을 얻었다(표 12). 또한, 변수별 최적 효소처리조건과 각 효소분해물의 특성값을 예측하여 표 13에 나타내었으며, 이들의 4차원 반응표면을 효소농도, 반응온도 및 반응시간을 독립변수로 하여 도 6~8에 나타내었다.In order to set the optimum enzymatic treatment condition of Viscozyme L in extracts obtained from ultra-high pressure treatment of persimmon peel, 20 enzymes designed according to the central synthesis plan as shown in Table 4 with enzyme concentration, reaction temperature and reaction time as independent variables The tannin content obtained under the treatment conditions is shown in Table 11. Response surface analysis was performed using each result of Table 11, and a regression equation was obtained for each dependent variable, that is, water soluble tannin, insoluble tannin, and gallic acid content (Table 12). In addition, the optimum enzyme treatment conditions for each variable and the characteristic values of each enzyme decomposition product were predicted and shown in Table 13. The four-dimensional reaction surface is shown in FIGS. 6 to 8 using enzyme concentration, reaction temperature and reaction time as independent variables. It was.
(mg/100 g)Water Soluble Tannin Content
(mg / 100 g)
(mg/100 g)Insoluble Tannin Content
(mg / 100 g)
(㎍/ml)Gallic acid content
(Μg / ml)
초고압처리된 감 껍질 추출물의 비스코자임(Viscozme L) 효소처리 조건에 따른 감 껍질 효소분해물의 수용성 탄닌 함량은 483.44~608.93 mg/100 g의 범위로 나타났으며(표 11), 이를 바탕으로 한 수용성 탄닌 함량의 회귀식은 표 12와 같고 R2 값은 0.8912으로 1% 이내의 수준에서 유의성이 확인되었다. 효소처리 조건에 따라 반응표면모델로 예측된 회귀분석결과 임계점이 최대점이 아닌 안장점으로 나타났으며, 능선분석을 하여 최적점을 산출한 결과 최대값은 631.19 mg/100 g이며, 이때의 효소처리 조건은 효소농도 2.67 g/100 mL, 반응온도 53.98℃ 및 반응시간 8.46시간으로 나타났다(표 13). 4차원 반응표면을 통한 효소분해 조건에 따른 떫은 감 효소분해물의 수용성 탄닌 함량의 변화는 도 6과 같이 효소농도와 반응온도가 높아질수록, 반응시간이 길어질수록 함량이 증가하는 경향을 나타내었다. 효소분해 처리조건에 대한 영향은 표 14에서와 같이 효소처리 조건 모두에서 영향을 받고 있는 것으로 나타났으며, 반응온도>반응시간>효소농도의 순으로 반응온도의 영향이 가장 크며, 효소농도의 영향이 가장 낮은 것으로 나타났다. The water-soluble tannin content of persimmon bark enzyme decomposed according to the Viscozme L enzyme treatment condition of ultra high pressure persimmon bark extract ranged from 483.44 to 608.93 mg / 100 g (Table 11). The regression equation of tannin content is shown in Table 12, and the R 2 value was 0.8912, and the significance was confirmed within 1%. The regression analysis predicted by the response surface model according to the enzyme treatment conditions showed that the critical point was the saddle point, not the maximum point, and the maximum value was 631.19 mg / 100 g as the result of the ridge analysis. The conditions were enzyme concentration 2.67 g / 100 mL, reaction temperature 53.98 ℃ and reaction time 8.46 hours (Table 13). The change in the water-soluble tannin content of the persimmon enzymatic degradation product according to the enzymatic degradation conditions through the four-dimensional reaction surface showed a tendency to increase as the enzyme concentration and the reaction temperature increased and the reaction time increased as shown in FIG. 6. As shown in Table 14, the effect on the enzymatic digestion condition was affected by all enzymatic conditions.The reaction temperature was the largest in the order of reaction temperature> reaction time> enzyme concentration. This was found to be the lowest.
감 껍질을 초고압 처리후 비스코자임 효소를 사용하여 조건별로 처리된 감 껍질 효소분해물의 불용성 탄닌 함량은 212.05~351.59 mg/100 g의 범위로 나타났으며(표 11), 이를 바탕으로 한 회귀식은 표 12와 같다. 불용성 탄닌 함량에 대한 R2값은 0.8952로 높은 신뢰도를 보였으며, p값은 1% 이내 유의수준을 보였다. 효소처리에 따라 반응표면모델로 예측된 회귀분석 결과 정상점이 최대점으로 나타났으며, 최적점을 산출한 결과 불용성 탄닌 함량의 최대값은 353.17 mg/100 g이고 이때의 발효조건은 효소농도 2.58 g/100 mL, 반응온도 52.35℃ 및 반응시간 9.10시간으로 나타났다(표 13). 효소처리 조건에 대한 영향에서 불용성 탄닌 함량의 경우 반응온도와 반응시간에 영향을 크게 받는 것으로 나타났다. 그러나 설정된 범위 내에서 효소농도의 영향은 거의 나타나지 않았다(표 14). 실험조건에 따라 얻은 효소분해물의 불용성 탄닌 함량에 대한 반응표면은 도 7에 나타내었다.The insoluble tannin content of persimmon skin degrading enzyme was treated in the range of 212.05 ~ 351.59 mg / 100 g after ultra high pressure treatment of biscozyme enzyme (Table 11). Same as 12. The R 2 value for the insoluble tannin content was 0.8952 with high reliability and the p value showed a significant level within 1%. The regression analysis predicted by the reaction surface model according to the enzyme treatment showed that the normal point was the maximum point. The optimum point was calculated and the maximum value of insoluble tannin content was 353.17 mg / 100 g and the fermentation condition was 2.58 g. / 100 mL, reaction temperature 52.35 ℃ and reaction time was 9.10 hours (Table 13). Insoluble tannin content was significantly affected by reaction temperature and reaction time. However, little effect of enzyme concentration was observed within the set range (Table 14). The reaction surface for the insoluble tannin content of the enzymatic digest obtained according to the experimental conditions is shown in FIG.
감 껍질을 초고압 처리 후 비스코자임(Viscozyme L) 효소를 사용하여 조건별로 처리된 감 껍질 효소분해물의 갈산의 함량은 13.28~18.66 ㎍/mL의 범위로 나타났으며(표 11), 이를 바탕으로 한 회귀식은 표 12와 같으며, 이 모델에 대한 회귀식의 R2 값은 0.9731로 1% 이내의 유의성이 인정되었다. 표 13과 같이 갈산 함량의 예측된 정상점은 최대점으로 최대값이 19.25 ㎍/mL이었고, 이때 효소농도 2.76 g/100 mL, 반응온도 50.56℃ 및 반응시간 8.57시간이었다. 갈산 함량은 효소농도, 반응시간, 반응온도의 효소 처리조건 모두에서 영향을 받고 있는 것으로 나타났다(표 14). 효소분해물의 불용성 탄닌 함량의 효소처리 조건에 따른 4차원 반응표면에서 볼 때 효소농도와 반응온도가 높고 반응시간이 길어질수록 함량이 증가하는 것으로 나타났다(도 8).The gallic acid content of persimmon hull degrading enzymes treated by conditions using Viscozyme L enzyme after ultra high pressure treatment ranged from 13.28 to 18.66 ㎍ / mL (Table 11). The regression equation is shown in Table 12, and the R 2 value of the regression equation for this model was 0.9731, indicating a significance within 1%. As shown in Table 13, the predicted peak of the gallic acid content was the maximum, the maximum value was 19.25 ㎍ / mL, wherein the enzyme concentration was 2.76 g / 100 mL, the reaction temperature 50.56 ℃ and the reaction time 8.57 hours. The gallic acid content was found to be affected by all enzyme treatment conditions such as enzyme concentration, reaction time and reaction temperature (Table 14). The insoluble tannin content of the enzymatic degradation product was found to increase as the enzyme concentration and reaction temperature were higher and the reaction time was longer according to the enzymatic treatment conditions (Fig. 8).
(℃)Reaction temperature
(℃)
*유의성 10% 이내; **유의성 5% 이내; ***유의성 1% 이내
* Significance within 10%; ** within 5% of significance; *** Significance within 1%
감 껍질의 최적 효소처리조건을 설정하기 위하여 수용성 탄닌, 갈산 함량 모두 만족시켜주는 최적 효소처리 조건을 얻고자 각 반응표면을 슈퍼임포징(superimposing)하여 도 9의 겹쳐진 부분으로써 표 15에 최적 조건을 나타내었다. 감 껍질 효소처리 최적 조건 범위는 효소농도 2.5~2.7 g/100 mL, 반응온도 51~56℃ 및 반응시간 8~9시간으로 나타났다. 따라서 이와 같은 예측 결과에 대한 모델식의 신뢰성을 확인하기 위하여 예측된 최적 조건 범위 내에서 임의의 조건 즉, 효소농도 2.6 g/100 mL, 반응온도 54℃ 및 반응시간 8.5시간을 대입하여 실제 효소 처리를 실시하고, 효소분해물의 탄닌 함량, 갈산 함량을 측정한 결과 예측된 값들과 유사한 수준으로 비교되었다(표 16).In order to set the optimum enzyme treatment condition of persimmon peel, superimposing each reaction surface to obtain the optimum enzyme treatment condition satisfying both the water-soluble tannin and gallic acid content. Indicated. The optimum condition of persimmon peel enzyme treatment ranged from enzyme concentration of 2.5-2.7 g / 100 mL, reaction temperature of 51-56 ℃ and reaction time of 8-9 hours. Therefore, in order to confirm the reliability of the model equation for this prediction result, the actual enzyme treatment was performed by substituting any conditions within the predicted optimum conditions, that is, enzyme concentration of 2.6 g / 100 mL, reaction temperature of 54 ° C. and reaction time of 8.5 hours. Was carried out, and the tannin content and the gallic acid content of the enzymatic degradation product were measured and compared with the predicted values (Table 16).
(2.6)2.5-2.7
(2.6)
(54)51-56
(54)
(8.5)8-9
(8.5)
(㎍/mL)Gallic acid content
(Μg / mL)
1)반응표면 변화값에 대한 예측식으로 계산된 값 1) Value calculated by the equation for response surface change
2)독립변수의 최적조건: 효소농도 2.6 g/100 mL, 반응온도 54℃, 반응시간 8.5시간 2) Optimal conditions for independent variables: enzyme concentration 2.6 g / 100 mL,
Claims (5)
(b) 상기 (a)단계의 제조한 감 분말에 물을 8~12배량(v/w) 첨가한 혼합물을 80~120 MPa 및 45~55℃에서 3~7시간 동안 초고압 추출하는 단계;
(c) 상기 (b)단계의 초고압 추출한 추출물에 18,000~30,000 PG/ml 농도의 펙티넥스 울트라 SP-L(Pectinex ultra SP-L)을 추출물 부피대비 2.4~2.8% 첨가한 후 50~60℃에서 7~9시간 동안 가수분해하는 단계; 및
(d) 상기 (c)단계의 가수분해한 추출물을 80~90℃에서 10~20분 동안 가열한 후 원심분리한 상등액을 60~100℃에서 10~60분 동안 살균한 후 여과하는 단계를 포함하여 제조하는 것을 특징으로 하는 수용성 탄닌을 고농도로 함유하는 감 추출물의 제조방법.(a) drying the pulp and skin of the persimmon persimmon at 45-55 ° C. for 44-52 hours and then grinding to prepare persimmon powder;
(b) ultra-high pressure extraction of the mixture of 8-12 times water (v / w) added to the persimmon powder prepared in step (a) at 80-120 MPa and 45-55 ° C. for 3-7 hours;
(c) Pectinex ultra SP-L (Pectinex ultra SP-L) of 18,000 ~ 30,000 PG / ml concentration to the ultra-high pressure extraction of step (b) after adding 2.4 ~ 2.8% of the volume of the extract at 50 ~ 60 ℃ Hydrolysis for 7-9 hours; And
(d) heating the hydrolyzed extract of step (c) at 80-90 ° C. for 10-20 minutes and then sterilizing the supernatant centrifuged at 60-100 ° C. for 10-60 minutes, followed by filtration. Method for producing persimmon extract containing a high concentration of water-soluble tannin, characterized in that the production.
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