KR100341284B1 - Potato vinegar and process for preparation thereof - Google Patents
Potato vinegar and process for preparation thereof Download PDFInfo
- Publication number
- KR100341284B1 KR100341284B1 KR1019990055979A KR19990055979A KR100341284B1 KR 100341284 B1 KR100341284 B1 KR 100341284B1 KR 1019990055979 A KR1019990055979 A KR 1019990055979A KR 19990055979 A KR19990055979 A KR 19990055979A KR 100341284 B1 KR100341284 B1 KR 100341284B1
- Authority
- KR
- South Korea
- Prior art keywords
- fermentation
- potato
- vinegar
- acetic acid
- alcohol
- Prior art date
Links
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Abstract
본 발명은 감자식초 및 그 제조방법에 관한 것으로 파쇄한 감자에 가수하고 누룩, 정제효소, 조효소제 또는 액체효소 등의 혼합효소를 첨가하여 당화시킨 후 1단계로 주모를 첨가하여 알콜발효시키고 2단계로 종초를 첨가하여 초산발효시키므로써 실험실 규모에서 감자식초를 제조하고 상기 실험실 규모의 감자식초 제조방법에 기초하여 공장 규모로 보존성이 우수한 감자식초를 제조하는 뛰어난 효과가 있다.The present invention relates to potato vinegar and a method for producing the same, which is hydrolyzed to shredded potatoes and saccharified by the addition of mixed enzymes, such as yeast, tablet enzyme, coenzyme or liquid enzyme, and then fermented by alcohol in two steps. Potassium vinegar is prepared by adding fermented vinegar to fermentation of acetic acid to produce potato vinegar on a laboratory scale and to produce potato vinegar with excellent shelf life on a plant scale based on the laboratory-scale potato vinegar production method.
Description
본 발명은 감자식초 및 그 제조방법에 관한 것이다. 더욱 상세하게는, 본 발명은 파쇄한 감자를 발효시켜 얻은 감자식초 및 그 제조방법에 관한 것이다.The present invention relates to potato vinegar and a manufacturing method thereof. More specifically, the present invention relates to potato vinegar obtained by fermenting crushed potatoes and a method for producing the same.
저온성 작물인 감자는 생육기간이 짧고 단위 면적당 생산량이 많으며 토질에 대한 적응성이 커서 전세계적으로 재배되고 있다. 감자는 칼륨, 인, 마그네슘 등의 무기질과 비타민 B군 및 C의 함량이 높은 알카리성 식품으로서 서양의 식생활에서는 주된 탄수화물 급원 식품으로 다양한 형태로 이용되어 왔다. 국내에서 감자는 강원도를 중심으로 생산되고 있으며 근년에는 수입개방과 동시에 불균형한 과다생산에 의해서 원활한 소비가 되지 못해 가격폭락 양상을 보이고 있다. 또한 감자에 함유된 수분함량이 높아서 저장이 어렵고 또한 중량 80g 이하의 상품성이 없는 불량 감자가 약 30% 정도 발생되어 재배 농가에 경제적 손실이 초래되고 있다. 현재 감자를 이용한 가공식품으로는 냉동프렌치프라이, 건조감자(감자칩), 감자가루 등이 있으나, 불량감자의 이용이 어렵고 지속적인 대량 가공에도 한계가 있으며 경제성 역시 매우 낮다. 따라서 감자의 상품성에 제약되지 않고, 고부가가치를 창출할 수 있는 대량 가공품의 개발이 시급한 실정이다.Potatoes, a low-temperature crop, are grown worldwide because of their short growing period, high yields per unit area, and adaptability to soil. Potatoes are alkaline foods with high minerals such as potassium, phosphorus and magnesium, and high levels of vitamins B and C, and have been used in various forms as a major carbohydrate source in Western diets. In Korea, potatoes are produced mainly in Gangwon-do, and in recent years, the price has been falling due to unbalanced overproduction due to import opening and unbalanced overproduction. In addition, the high moisture content of the potato is difficult to store and about 30% of bad potatoes without commerciality less than 80g in weight is generated, causing economic losses to growers. Currently, processed foods using potatoes include frozen French fries, dried potatoes (potato chips), and potato powder. However, the use of defective potatoes is difficult, and there is a limit to continuous mass processing, and the economic efficiency is also very low. Therefore, there is an urgent need to develop mass processed products that can create high value without limiting the commerciality of potatoes.
식초는 동서양을 막론하고 음식의 조미료 등으로 널리 이용되고 있는 대표적인 발효 식품으로 전분질과 알콜을 초산발효시켜 생산하는 양조식초와 빙초산, 향신료 및 착색료 등으로 제조되는 합성식초로 구별된다. 최근에는 합성식초의 유해성이 대두되면서 건강에 대한 인식전환으로 천연소재의 전통 양조식초의 소비가 상대적으로 증가되고 있다. 또한 경제성장과 더불어 식생활문화가 향상되면서 조미용, 음료용 및 식초음료까지 개발되어 식초의 용도도 다양화되고 있다. 국내 시장규모는 매년 7% 이상 안정적인 성장추세에 있으며 2000년대에는 2000억원대의 매출로 고급화, 다양화 양상이 기대된다. 초산이 주성분인 식초는 TCA cycle에 관여하여 혈액의 산성화와 젖산의 발생에 기인하는 피로를 감소시킨다. 일반적으로 혈액의 pH는 약알카리인 7.2 ∼ 7.5인데 과다한 업무, 불균형한 식사로 인한 피로는 혈액 산성화의 원인이 된다. 이는 생체내의 에너지가 해당과정을 거쳐 소비될 때 과도한 양의 젖산이 발생하기 때문이며, 생성된 젖산이 혈관과 근육에 축적되게 되면 혈액의 산성화를 유발하여 근육을 경직하게 하고 통증을 유발한다. 따라서 식초는 다량의 유기산과 아미노산이 함유되어 신진대사를 원할하게 하여 과격한 운동으로 생성되는 젖산을 빠르게 분해시키므로 피로회복에 좋고 동맥경화 및 고혈압 예방등의 효과를 지니고 있다. 이러한 식초의 특성은 천연원료를 이용한 양조식초에서 새로운 연구분야가 되고 있으며, 일본에서는 오래전부터 기능성 식초에 대한 연구가 진행되어 왔다. 국내에서는 사과식초, 현미식초 이외에 감식초, 포도식초, 레몬식초, 유자식초 등이 상품화되어 농가소득증대 및 국민건강에 기여하고 있다. 현재 감자에 관한 연구로 품종별 전분 특성, 저장조건, 감자 튀김유 및 마이크로파를 이용한 감자전분의 이화학적 특성 등이 보고되었으나 상품성이 저하된 불량감자를 대량으로 활용할 수 있는 가공방법에 관한 연구는 미비한 실정이다. 특히 알카리성 감자식초 개발은 고부가가치의 창출 및 식초시장의 고급화 등이 기대되지만, 이에 관한 연구는 국내·외적으로 전무하다.Vinegar is a representative fermented food that is widely used as food seasoning in both East and West, and is divided into vinegar produced by acetic acid fermentation of starch and alcohol and synthetic vinegar produced by glacial acetic acid, spices and coloring. In recent years, as the danger of synthetic vinegar has emerged, the consumption of traditional brewed vinegar of natural materials has been relatively increased due to a change in awareness of health. In addition, with economic growth and improved food culture, seasonings, beverages, and vinegar beverages have been developed. The domestic market is growing at a stable growth rate of more than 7% annually. In the 2000s, the market is expected to expand and diversify to 200 billion won. Vinegar, the main component of acetic acid, participates in the TCA cycle and reduces fatigue due to acidification of blood and the generation of lactic acid. In general, the pH of the blood is 7.2 to 7.5, which is a weak alkali. Excessive work and unbalanced dietary fatigue cause blood acidification. This is because excessive amounts of lactic acid are generated when energy in the body is consumed through glycolysis, and when the generated lactic acid accumulates in blood vessels and muscles, it causes acidification of blood, causing muscle stiffness and pain. Therefore, vinegar contains a large amount of organic acid and amino acid, which makes metabolism smooth, and rapidly decomposes lactic acid produced by intense exercise, so it is good for fatigue recovery and prevents arteriosclerosis and hypertension. Such vinegar has become a new field of research in brewing vinegar using natural raw materials, and research on functional vinegar has been in progress for a long time in Japan. In Korea, in addition to apple vinegar and brown rice vinegar, persimmon vinegar, grape vinegar, lemon vinegar and citron vinegar are commercialized, contributing to the increase of farm household income and national health. The current research on potatoes has reported starch characteristics, storage conditions, and physicochemical properties of potato starch using french fries and microwaves. However, there are insufficient studies on processing methods that can utilize defective potatoes with reduced marketability. to be. In particular, the development of alkaline potato vinegar is expected to create high value-added and high-grade vinegar market, but there are no studies on this at home and abroad.
본 발명자들은 과잉생산 및 저장성이 떨어지는 감자의 효율적 활용을 위하여 감자식초의 제조방법을 최적화함과 동시에 규모확대(scale up)에 따른 공정의 최적화와 제품의 표준화로 대량생산을 이루고자 여러 종류의 발효제를 사용하여 감자식초를 제조한 후 성분을 분석하여 최적의 조건으로 품질이 우수한 감자식초를 제조한 다음 규모를 확대하여 대량으로 감자식초를 제조하므로써 본 발명을 완성하였다.The inventors of the present invention optimized the production method of potato vinegar for efficient use of potatoes with low overproduction and low shelf life, and at the same time, various kinds of fermenting agents to achieve mass production by optimizing the process according to scale up and standardizing products. The potato vinegar was prepared using potato vinegar after analyzing the components to prepare the vinegar with excellent quality under optimum conditions and then expanding the scale to produce potato vinegar in large quantities.
따라서, 본 발명의 목적은 감자를 발효시켜 제조한 감자식초를 제공함에 있다. 본 발명의 다른 목적은 상기 감자식초의 제조방법을 제공함에 있다.Accordingly, it is an object of the present invention to provide potato vinegar prepared by fermenting potatoes. Another object of the present invention to provide a method for producing the potato vinegar.
본 발명의 상기 목적은 파쇄한 감자에 물 및 혼합효소를 첨가하여 당화시킨후 1단계로 주모를 첨가하여 알콜발효시키고 2단계로 종초를 첨가하여 초산발효시켜 감자식초를 제조하였다. 이때, 상기 알콜발효 조건과 초산발효 조건을 변화시키면서 감자식초를 제조하고 이들 감자식초들의 알콜, 총산, 아미노태질소, 총페놀성 물질, 유기산, 유리당, 유리아미노산 함량을 조사하고 색상, 갈색도, 탁도를 조사하여 최적의 알콜발효 조건과 초산발효 조건을 확립하고 이어서, 상기 알콜발효 조건과 초산발효 조건에 기초하여 대규모로 감자식초를 제조한 후 시간경과에 따른 감자식초의 보존성을 조사하므로써 달성하였다.The object of the present invention was to saccharified by adding water and mixed enzyme to the crushed potato, and then fermented by acetic acid by adding jujum in one step, and adding vinegar in two steps to prepare potato vinegar. At this time, the potato vinegar is prepared by changing the alcohol fermentation conditions and acetic acid fermentation conditions, and the content of alcohol, total acid, amino nitrogen, total phenolic substance, organic acid, free sugar, free amino acid, and color, brownness, Turbidity was investigated by establishing optimal alcoholic and acetic acid fermentation conditions, and then preparing potato vinegar on a large scale based on the alcoholic and acetic acid fermentation conditions, and then examining the preservation of potato vinegar over time. .
이하, 본 발명의 구성 및 작용을 설명한다.Hereinafter, the configuration and operation of the present invention.
도 1은 본 발명 감자식초 제조에 사용되는 원료감자를 나타낸 사진도이다.1 is a photograph showing the raw potatoes used in the production of potato vinegar of the present invention.
도 2는 파쇄한 감자에 첨가하는 발효제의 종류에 따라 당화력의 차이를 나타낸 그래프이다.Figure 2 is a graph showing the difference in glycation power according to the type of fermentation agent added to the crushed potatoes.
도 3은 파쇄한 감자에 첨가하는 가수량의 차이에 따라 당화력의 차이를 나타낸 그래프이다.3 is a graph showing the difference in glycation power according to the difference in the amount of hydrolyzate added to the crushed potatoes.
도 4는 파쇄한 감자에 첨가하는 복합발효제의 종류에 따라 당화력의 차이를 나타낸 그래프이다.Figure 4 is a graph showing the difference in glycation power according to the type of complex fermentation agent added to the crushed potatoes.
도 5는 감자의 알콜발효시 첨가되는 주모의 종류에 따라 알콜생성량의 차이를 나타낸 그래프이다.Figure 5 is a graph showing the difference in the amount of alcohol production according to the type of hair added during the alcoholic fermentation of potatoes.
도 6은 감자의 초산발효시 첨가되는 종초의 종류에 따라 산생성량의 차이를 나타낸 그래프이다.Figure 6 is a graph showing the difference in the amount of acid production according to the type of seed that is added during the fermentation of acetic acid of potatoes.
도 7은 감자의 알콜발효시 발효시간을 고정하고 반응표면분석을 실시하여 최적의 가수량과 교반속도을 나타낸 등고선도이다.7 is a contour diagram showing the optimum amount of hydrolysis and stirring speed by fixing the fermentation time during alcohol fermentation of potatoes and conducting reaction surface analysis.
도 8은 감자의 알콜발효시 교반속도를 고정하고 반응표면분석을 실시하여 최적의 발효시간과 가수량을 나타낸 등고선도이다.8 is a contour diagram showing the optimum fermentation time and the amount of hydrolysis by fixing the stirring speed during alcohol fermentation of potatoes and performing reaction surface analysis.
도 9는 감자의 알콜발효시 가수량을 고정하고 반응표면분석을 실시하여 최적의 교반속도와 발효시간을 나타낸 등고선도이다.9 is a contour diagram showing the optimum stirring speed and fermentation time by fixing the amount of water during alcohol fermentation of potatoes and performing reaction surface analysis.
도 10은 감자의 알콜발효중 가수량, 발효시간, 교반속도의 변화에 따른 알콜함량의 변화를 4차원 반응표면분석을 실시하여 나타낸 등고선도이다.10 is a contour diagram showing the change of alcohol content according to the change in the hydrophilicity, fermentation time and stirring speed of the alcohol fermentation of potatoes by performing a four-dimensional reaction surface analysis.
도 11은 감자의 초산발효시 총산함량 변화도를 반응표면분석을 실시하여 나타낸 등고선도이다.11 is a contour diagram showing the change in total acid content during acetic acid fermentation of potatoes by performing a response surface analysis.
본 발명은 세척, 파쇄한 감자에 효소제로 누룩, 조효소제, 정제효소, 액체효소 각각 또는 혼합하여 첨가하고 당화력을 측정, 비교하여 당화에 가장 바람직한 발효제를 조사하는 단계; 상기와 동일한 방법으로 감자를 당화시키되 가수량을 80, 110, 140, 170, 200%로 한 후 당화력을 측정, 비교하여 당화에 가장 바람직한 가수량을 조사하는 단계; 파쇄한 감자에 상기 단계에 따라 얻어진 당화에 가장 바람직한 발효제와 바람직한 양의 물을 가수한 후 당화시키고 당화력을 조사하는 단계; 원료 감자를 절간하거나 파쇄한 후 상기와 동일하게 당화시킨 후 알콜발효시켜 당화력과 알콜생성력을 측정하여 당화와 알콜발효에 바람직한 감자의 전처리 조건을 조사하는 단계; 상기 조사한 모든 바람직한 조건에 따라 감자를 당화시킨 다음 1단계로 주모를 접종하여 알콜발효시키고 2단계로 종초를 접종하여 초산발효시켜 감자식초를 제조하고 이때 중심합성계획법에 따라 실험계획을 수립하고 SAS Mathematica program을 활용하여 반응표면분석방법으로 최적의 알콜발효 조건 및 초산발효 조건을 확립하는 단계; 상기 최적의 알콜발효 조건과 초산발효 조건에 따라 파쇄하여 당화시킨 감자를 알콜발효 및 초산발효시키고 이때 초산발효시에 첨가하는 종초의 종류를 달리하여 최종 생산되는 감자식초의 pH, 총산, 환원당, 아미노태질소, 유기산, 유리당, 유리아미노산 함량을 각각 측정하고 색상, 갈색도, 탁도를 각각 조사하여 비교하는 단계; 실험실 규모의 감자식초 제조를 공장규모로 확대하여 원료선별, 세척, 파쇄, 증자, 당화, 담금, 착즙·여과, 발효, 침전 및 숙성, 여과, 살균·냉각, 숙성·여과의 공정을 거쳐 제조하고 제조한 감자식초중 총산 4.0 이상의 액을 선별하여 PET 또는 병용기에 주입하여 포장하는 단계 및; 상기 공장규모로 제조한 감자식초의 고유의 맛, 산도 및 pH 변화, 고유의 색상 변화, 침전상태, 대장균수, 총세균수를 시간경과에 따라 측정하여 보존성을 조사하는 단계로 구성된다.The present invention comprises the steps of adding the yeast, coenzyme, purified enzyme, liquid enzyme to the washed and shredded potato, respectively, or mixed with the enzyme, and measuring the saccharification power to investigate the most preferable fermenting agent for saccharification; The method of glycosylating the same method as described above, but the amount of hydrolysis to 80, 110, 140, 170, 200% after measuring the glycosylation power to compare the most preferred amount of hydrolyzation; A step of saccharifying and saccharifying the crushed potatoes after the most preferred fermentation agent and the desired amount of water for saccharification obtained according to the above steps; Intercalating or crushing the raw potatoes, and then saccharifying them in the same manner as described above, and then examining the pretreatment conditions for the saccharification and alcohol fermentation by measuring the saccharification power and the alcohol production capacity. Potato vinegar was inoculated in the first step after saccharifying the potato according to all the desirable conditions investigated above, alcoholic fermentation by inoculation with the first step inoculated with vinegar in the second step to produce potato vinegar, and then the experimental plan was established according to the central synthesis scheme and SAS Mathematica establishing optimal alcohol and acetic acid fermentation conditions using a reaction surface analysis method using the program; According to the optimum alcohol fermentation conditions and acetic acid fermentation conditions, the potato that is crushed and saccharified by alcohol fermentation and acetic acid fermentation, and at this time, the pH, total acid, reducing sugar, amino of the final potato potato vinegar produced by varying the type of vinegar added during the fermentation of acetic acid Measuring nitrogen nitrogen, organic acid, free sugar, and free amino acid content, and comparing and comparing color, brownness, and turbidity, respectively; Expanded laboratory-scale potato vinegar production to plant scale and manufactured through the process of raw material selection, washing, crushing, steaming, saccharification, immersion, juice and filtration, fermentation, precipitation and aging, filtration, sterilization and cooling, and aging and filtration. Selecting a total solution of at least 4.0 of the prepared potato vinegar and injecting the package into a PET or bottle; The inherent taste, acidity and pH change, intrinsic color change, precipitation state, coliform bacteria, total bacteria count of potato vinegar prepared at the plant scale is measured by the preservation of time.
상기 구성에 따라 공장규모로 제조된 본 발명 감자식초는 상온보존의 경우 36개월까지 제품성에는 문제가 없었지만, 37개월 부터는 식초고유의 맛과 침전 및 산도가 조금씩 변하기 시작하였으나, 냉장보관일 때는 37개월까지 제품상의 문제점은 없었고 38개월 부터는 제품이 전체적으로 불안정하기 시작하였다. 따라서 유통방식 및 제품의 특성을 고려한 완전한 제품 보존력을 보증하기 위하여 상온 조건으로 36개월기간을 유통기간으로 설정하였다.The potato vinegar of the present invention manufactured according to the above-described composition has no problem in product quality until 36 months when stored at room temperature, but since 37 months, the taste, sedimentation and acidity of vinegar have started to change little by little. There were no product problems by the month and from 38 months the product started to become unstable overall. Therefore, in order to guarantee complete product retention considering the distribution method and the characteristics of the product, the period of 36 months was set as the normal temperature condition.
본 발명에서 주모는 알콜발효 효모균주는 어느 것이나 사용가능하며 바람직하게Zygosaccharomyces fermentati속 효모균주를 사용하였으며 종초는Acetobacter속 균주는 어느 것이나 사용 가능하였다.In the present invention, any of the alcoholic fermented yeast strains can be used, and preferably, yeast strains of the genus Zygosaccharomyces fermentati were used, and the strains were any strains of the genus Acetobacter .
본 발명에서 초산시 사용하는 초산균 보존용 배지는 표 1에 나타낸 바와 같으며 초산균 분리용 배지는 표 2에 나타낸 바와 같다.Acetic acid preservation medium used for acetic acid in the present invention is as shown in Table 1, and the medium for separating acetic acid bacteria is shown in Table 2.
본 발명에서 사용한 감자는 도 1에 나타낸 바와 같으며 1998년도 강원도에서 생산된 상품성이 떨어지는 불량감자를 사용하였으며, 당화에 사용한 발효제로는 양조용으로 시판되고 있는 누룩(상주곡자 제조), 조효소제(배한산업주식회사 제조) ,정제효소(배한산업주식회사 제조) 및 액체효소(액화효소 KLEISTASE T10S 0.04%와 당화효소 XUE - MEI 0.06%를 혼합한 혼합효소)를 각각 원료 감자량에 대한 백분율 (w/w)로 사용하였다.Potato used in the present invention is as shown in Figure 1 and used inferior potato produced in 1998 in Gangwon-do is poor in commerciality, as a fermentation agent used for saccharification commercially available for brewing Nuruk (resident sangjakja), coenzyme ( Baehan Industrial Co., Ltd.), purified enzyme (Baehan Industrial Co., Ltd.) and liquid enzyme (mixed enzyme mixed with liquefied enzyme KLEISTASE T10S 0.04% and glycosylated enzyme XUE-MEI 0.06%), respectively, as a percentage (w / w) ) Was used.
이하, 본 발명의 구체적인 방법을 실시예와 실험예를 들어 상세히 설명하고자 하지만 본 발명의 권리범위는 이들 실시예에만 한정되는 것은 아니다.Hereinafter, specific examples of the present invention will be described in detail with reference to Examples and Experimental Examples, but the scope of the present invention is not limited to these Examples.
실시예 1: 알콜발효 전처리 조건 확립과 감자식초 제조Example 1 Establishment of Alcohol Fermentation Pretreatment Conditions and Preparation of Potato Vinegar
제 1 공정: 발효제에 따른 당화력 비교Step 1: Comparison of Glycation Ability According to Fermentation Agents
원료 감자 500g을 세척하여 파쇄하고 증자하여 각각 물을 500mL씩 가하여 양조용으로 시판되는 누룩(상주곡자 제조), 조효소제(배한산업주식회사 제조), 정제효소 (배한산업주식회사 제조)또는 액체효소(액화효소 KLEISTASE TIOS 0.04%, 당화효소 XUE-MEI 0.06%의 혼합효소)를 이용하여 60℃, 6시간동안 당화하면서 각각의 발효제에 따른 당화력을 비교하였다. 실험결과, 도 2에 나타낸 바와 같이 각각의 효소제 모두 5, 6시간에서 당의 생성이 가장 높았으며, 6시간째에 누룩, 조효소제, 액체효소, 정제효소 순으로 당의 생성이 높았다. 그러나 누룩과 조효제는 자체에 일부의 전분질을 함유하고 있어 최종 당의 생성량이 많았으며, 정제효소와 액체효소는 당화력은 약하지만 2, 3시간 정도에 당화가 빨리 완료되었다. 따라서 단일 발효제의 사용보다는 발효제를 혼합하여 당화하는 것이 적합하다는 것을 알 수 있었다.500 g of raw potatoes are washed, crushed, steamed, and 500 mL of water is added to each brew for commercial brewing (made by Sangjugoja), coenzyme (manufactured by Baehan Industrial Co., Ltd.), purified enzyme (manufactured by Baehan Industrial Co., Ltd.) or liquid enzyme (liquefied). The saccharification ability of each fermenter was compared while saccharifying at 60 ° C. for 6 hours using enzyme KLEISTASE TIOS 0.04%, glycosylated enzyme XUE-MEI 0.06% mixed enzyme). As a result, as shown in FIG. 2, the sugar production was the highest in each enzyme at 5 and 6 hours, and the sugar production was high in the order of leaven, coenzyme, liquid enzyme, and purified enzyme at 6 hours. However, yeast and adjuvants contained some of the starch in themselves, which produced a large amount of final sugar. The purified enzyme and the liquid enzyme had a weak glycosylation ability, but the saccharification completed quickly in about 2 to 3 hours. Therefore, it was found that saccharification by mixing fermentation agents is more suitable than using a single fermentation agent.
제 2 공정: 가수량에 따른 당화력 비교Second Process: Comparison of Saccharification Capacity According to Hydrolysis Amount
원료 감자 500g을 세척하여 파쇄 후 증자하여 누룩, 조효소제, 정제효소 및 액체효소를 각각 사용하여 원료감자 중량에 대한 백분율로 각각 80, 110, 140, 170 및 200%씩 가수하고 60℃, 6시간동안 당화 후 당화력을 비교하였다. 실험결과, 도 3에 나타낸 바와 같이 발효제 종류에 따른 당화력은 비슷한 경향을 나타내었으며 급수량이 작을수록 당의 생성량은 높았으며, 가수량이 많을수록 당의 생성량은 작았다. 그러나 전체적인 수율과 당의 농도를 고려할 때 급수량은 150% 정도가 적당한 것으로 나타났다.500 g of raw potatoes are washed, crushed, and then steamed to increase 80, 110, 140, 170 and 200%, respectively, as a percentage of the weight of raw potatoes using leaven, coenzyme, purified enzyme and liquid enzyme, respectively. The saccharification power after saccharification was compared. As a result, as shown in FIG. 3, the saccharification ability according to the type of fermentation agent showed a similar tendency. The smaller the water supply, the higher the sugar production, and the higher the hydrolyzate, the smaller the sugar production. However, considering the overall yield and sugar concentration, the water supply was about 150%.
제 3 공정: 발효제 조건에 따른 당화력 비교Third Step: Comparison of Glycation Ability According to Fermenter Conditions
감자 중량에 150%를 가수하여 각각의 발효제를 사용하여 60℃, 6시간동안 당화하여 당화력을 비교하였다. 이때, 상기 제 1 및 2 공정에 따라 단기간 대량생산을 위하여 당화시간의 단축과 당화력을 높이기 위하여 단일 발효제 보다는 초기 당화력이 높은 정제효소 또는 액체효소를 조효소와 같이 사용하였고 가수량은 150% 정도로 하였다. 실험결과, 도 4에 나타낸 바와 같이 3시간 정도에서 당화가 완료되어 당화시간이 단축되고 전체적으로 당화력도 높았다. 조효소제에 누룩을 혼합한 실험구간이 조효소제에 액체효소를 사용한 실험구간 보다 당화력이 다소 높게 나타났으나, 이는 누룩 자체에 함유된 전분질에 따른 차이로 추정된다. 결론적으로 조효소제와 액체효소의 혼용과 가수량 150%로 3시간의 당화가 당화력이 가장 우수한 것으로 나타났다.150% was added to the potato weight to be glycosylated at 60 ° C. for 6 hours using each fermenter to compare the glycosylation ability. In this case, in order to shorten the saccharification time and increase the saccharification capacity for short-term mass production according to the first and second processes, purified enzyme or liquid enzyme having a higher initial glycosylation power than the single fermentation agent was used together with the coenzyme and the hydrolysis amount was about 150%. As a result, as shown in FIG. 4, the saccharification was completed in about 3 hours, the saccharification time was shortened and the saccharification power was high overall. The experimental section of the co-enzyme mixed with Nuruk was slightly higher than the experimental section using liquid enzyme in the Co-enzyme, but this is presumed to be due to the starch contained in the Nuruk itself. In conclusion, the saccharification ability of the 3 hours of glycosylation with 150% of the mixture of coenzyme and liquid enzyme was the best.
제 4 공정: 감자의 전처리 조건에 따른 당화력 비교Fourth Step: Comparison of Glycation Ability According to Potato Pretreatment Conditions
원료 감자의 증자방법과 절간감자에 따른 당화력을 비교하기 위하여 2㎜ 두께로 슬라이스(slice)하여 121℃, 15분 가압증자 방법, 원료감자를 블렌더 믹서(blander mixer)로 파쇄 방법 및 2㎜ 두께로 슬라이스(slice)하여 45℃에서 열풍건조한 원료 감자에 가수량을 150%로 조절하여 조효소 및 액체효소를 혼합하여 60℃, 3시간동안 당화 및 알콜발효하여 당화력과 알콜생성량을 비교하여 수득율을 검토하였다. 실험결과, 표 3에서 나타낸 바와 같이 당화 후 당의 생성은 가압증자, 파쇄 및 절간감자는 각각 14.2, 11.0 및 9.0。brix로 나타났으며, 당화 후 발효하여 생성된 알콜함량은 각각 6.4, 5.6 및 5.5%로 가압증자 처리된 구간이 가장 높았다. 절간감자의 경우 수율 및 대량생산시 단계별 공정에 따른 생산원가 상승요인과 관능적인 이취(異臭)의 발생으로 감자식초 제조공정에는 적합하지 않는 것으로 추정되었다. 표 4에는 원료 감자 중량에 대한 수득율을 백분율로 나타낸 것으로 가압증자 구간은 알콜분 6.4%에 150%의 수득율을 나타났으며, 파쇄처리 구간은 5.6% 알콜함량에 150%의 수득율, 절간감자는 알콜분 5.5%에 80%의 수득율을 나타내어 식초생산을 위한 1단계 알콜발효의 효율성은 연속적인 공정이 가능한 감자를 파쇄하여 당화 후 알콜발효하는 것이 우수함을 알 수 있었다.In order to compare the method of increasing the raw potato and the saccharification power according to the interpotato potato, slice it to 2mm thickness and pressurize it at 121 ℃ for 15 minutes, crush the raw potato into the blender mixer and 2mm thickness. The raw potato was sliced and hot-dried at 45 ° C. to adjust the amount of hydrolysis to 150%. The crude and liquid enzymes were mixed, and saccharification and alcohol fermentation were performed at 60 ° C. for 3 hours. . As a result, as shown in Table 3, the production of sugar after saccharification was 14.2, 11.0, and 9.0 ° brix for pressurized steam, crushed, and intercalated potatoes, respectively. The alcohol content produced after fermentation was 6.4, 5.6, and 5.5, respectively. The highest percentage of autoclaved sections was%. In the case of interlaced potato, it is estimated that it is not suitable for the potato vinegar manufacturing process due to the increase of production cost and sensual off-flavor due to the yield and mass production process. In Table 4, the yield of the raw potato weight is expressed as a percentage. The autoclave section shows an alcohol yield of 6.4% and 150%. The fracturing section shows a 5.6% alcohol content and a 150% yield. The yield of 80% at 5.5% of the yield showed that the efficiency of alcohol fermentation in the first step for vinegar production was superior to alcohol fermentation after saccharification by crushing potatoes that can be processed continuously.
실시예 2: 발효조건 확립Example 2: Establishment of Fermentation Conditions
본 실시예에서는 상기 실시예 1에서 확립한 알콜발효 전처리 조건에 따라 파쇄한 감자를 당화시킨 후 알콜발효 및 초산발효시켜 감자식초를 제조하면서 중심합성계획에 따라 실험계획을 수립하고 반응표면분석으로 최적 발효조건을 확립하였다. 즉, 원료 감자 500g을 파쇄, 증자하고, 물 750mL을 가한 후 각각의 혼합효소를 사용하여 60℃, 5시간동안 당화시킨 다음 30℃ 진탕배양기에서Zygosaccharomyces fermentati속 효모균주를 첨가하고 3일간 1단계 알콜발효를 하였으며, 착즙 여과하여 고형분을 제거한 후 여액으로 30℃, 250rpm으로 8일간 2단계Acetobacter속초산발효균주를 사용하여 초산발효한 후 초산발효력을 비교하였다. 이때 성분분석 시료는 원심분리하여 상등액으로 각각의 성분을 분석하였다. 실험결과, 1단계 알콜발효 과정에서는 도 5와 같이 당화시 사용한 발효제에 따라 3구간(Ⅰ:조효소 + 누룩, Ⅱ:조효소 + 정제효소, Ⅲ:조효소 + 액체효소)으로 나누어 각 구간마다 발효 3일째에 알콜함량이 각각 3.6, 6.2, 6.6%로 나타났으며, 2단계 초산발효에서는 도 6에서 발효 3일째부터 산의 생성이 시작되어 발효 8일째에 산의 생성은 각각 3.5, 5.8, 6.7%로 나타났으며, 조효소과 액체효소를 처리한 Ⅲ구간에서 가장 높게 나타나서 감자식초의 생산이 가능하였다. 따라서 혼합 발효제로 조효소와 액체효소를 사용하여 파쇄한 감자를 당화시킨 후 발효시켜 감자식초를 제조하여 분석에 이용하였다. 이때, 분석은 감자식초 발효조건을 알콜발효 및 초산발효 2단계로 구분하여 실시하였으며 중심합성계획법에 따라 실험계획을 수립하고 SAS(statistical analysis system), Mathematica program을 활용하여 반응표면분석방법으로 최적 발효조건을 확립하였다.In this embodiment, the potato vinegar is prepared by saccharifying the potato crushed according to the alcohol fermentation pretreatment conditions established in Example 1, and then the experimental plan is established according to the central synthesis plan and optimized by reaction surface analysis. Fermentation conditions were established. In other words, 500 g of raw potatoes were crushed and increased, 750 mL of water was added, and each mixed enzyme was used for saccharification at 60 ° C. for 5 hours. Then, the yeast strain of Zygosaccharomyces fermentati was added in a 30 ° C. shaker incubator, followed by 1 step alcohol After fermentation, the solids were removed by filtration, and the acetate fermentation was compared after the fermentation of acetic acid using two-stage Acetobacter acetic acid fermentation strains for 8 days at 30 ° C and 250 rpm as a filtrate. At this time, the component analysis sample was centrifuged to analyze each component with a supernatant. As a result, the alcohol fermentation process in the first step is divided into three sections (I: coenzyme + yeast, II: coenzyme + purified enzyme, III: coenzyme + liquid enzyme) according to the fermentation agent used for saccharification as shown in FIG. The alcohol content was 3.6, 6.2, and 6.6%, respectively. In the two-stage acetic acid fermentation, acid production was started on the third day of fermentation, and the acid production was 3.5, 5.8, and 6.7% on the eighth day of fermentation, respectively. Potato vinegar was the highest in the Ⅲ section treated with coenzyme and liquid enzyme. Therefore, the crushed potato using coenzyme and liquid enzyme as a mixed fermentation agent and then fermented to prepare potato vinegar was used for analysis. At this time, the analysis was carried out by dividing potato vinegar fermentation conditions into two stages: alcohol fermentation and acetic acid fermentation. The experimental plan was established according to the central synthesis planning method, and the optimal fermentation was performed using the response surface analysis method using SAS (statistical analysis system) and Mathematica program. Conditions were established.
반응표면분석법은 2개 이상의 조건변수가 상호의존적으로 반응변수에 영향을 미칠 때 이 반응변수가 이루는 표면에 대한 통계적 분석을 하고 이에 관련된 설계를 하는 방법이다. 반응표면분석에서는 회귀분석에서와 같이 조건변수와 반응변수간의 함수관계로 부터 조건변수의 변화에 따른 반응량을 예측하는 동시에 반응량이 최대, 최소 또는 최적이 되는 조건변수의 값을 추정하며 가장 합리적인 실험의 설계를 다루게 된다. 반응표면분석에서는 조건변수와 반응변수간 미지의 함수관계를 추정하기 위해 다중회귀모형을 사용하는데 이것은Response surface analysis is a method of statistically analyzing and designing the surface of a response when two or more condition variables influence the response. In the response surface analysis, as in the regression analysis, the most reasonable experiment is performed by estimating the response amount according to the change of the condition variable from the functional relationship between the condition variable and the response variable. The design of Response surface analysis uses multiple regression models to estimate unknown functional relationships between condition and response variables.
Y = βo+ β1X1+ β2X2+ ‥‥ + βkXk+ ε ‥‥‥ (1)Y = β o + β 1 X 1 + β 2 X 2 + ‥‥ + β k X k + ε ‥‥‥‥ (1)
로 표현되는 1차모형과The first model is represented by
‥‥‥(2) ‥‥‥(2)
로 표현되는 2차 모형이 있고, 이 함수의 모수를 추정하기 위해서는 회귀분석에서와 같이 최소 제곱법을 사용하였다. 모수의 추정을 위한 자료는 반응표면분석을 위한 계획된 실험에서 수집하는 것이 효과적이며 이때에 사용되는 반응표면 실험계획법으로 알콜발효 및 초산발효의 최적조건을 수립하고자 하였다.There is a quadratic model that is expressed as, and the least square method is used to estimate the parameters of this function as in the regression analysis. It is effective to collect data for parameter estimation in the planned experiments for response surface analysis, and to establish the optimal conditions for alcohol and acetic acid fermentation using the response surface design.
제 1 공정: 알콜발효 조건First step: alcoholic fermentation conditions
알콜발효 최적화를 위한 실험계획으로써 상기 중심합성 계획(central composite design)에 따라 반응표면분석을 위해서 SAS(statistical analysis system) package를 사용하였다. 알콜발효시 실험변수로는 가수량(X1), 진탕속도 (X2), 발효시간(X3)이었으며, 이들 요인변수들은 표 5과 같이 -2, -1, 0, 1, 2로써 다섯 수준으로 부호화하여 실험하였다. 실험결과, 중심합성계획에 의해 설계된 실험조건에서 알콜발효 효모에 의한 발효과정의 알콜함량 변화는 표 6에 나타낸 바와 같으며 이에 대한 등고선도와 4차원 반응표면은 도 7, 도 8, 도 9, 도 10에 각각 나타내었다.Zygosaccharomyces fermentati속 효모균주에 의한 알콜발효에서 가장 중요한 변수인 가수량(100∼300㎖), 교반속도(0∼120rpm) 및 발효시간(0∼48hr)에따른 알콜함량은 반응표면 회귀분석을 행한 결과 회귀식의 R2는 0.9254로 유의성이 0.0091로 1% 이내의 유의수준에서 인정되었다(표 7). 알콜함량에 대한 발효조건의 영향은 주로 발효시간의 영향을 받고 있었으며, 가수량과 교반속도의 영향은 미약하였다(표8). 알콜발효에 대한 반응표면 회귀분석에서 정상점이 안장점의 형태를 나타내어(표 9), 다시 능선분석을 하여 본 결과 최적 알콜발효조건과 알콜함량은 가수량 241.35㎖, 교반속도 8.05rpm 및 발효시간 34.81hr에서 8.31%였다. 따라서 최적조건으로 한 변수를 고정시키고 등고선도를 그려본 결과, 발효시간을 34.81시간으로 고정한 반응표면(도 7)은 가수량과 교반속도가 낮은 조건에서 발효시 알콜함량이 증가하였으며, 가수량과 교반속도가 높을 경우에는 감소하였다. 그러나 가수량과 교반속도가 너무 낮을 경우에는 알콜발효가 다소 늦어짐을 알 수 있었다. 그리고 교반속도의 최적조건인 8.05rpm으로 교반속도를 고정한 반응표면(도 8)은 발효시간의 영향을 주로 받아 발효시간의 경과에 따라 계속 증가하는 편이었다. 그러나 발효 30시간 이후에는 거의 변화가 없었다. 가수량의 최적조건인 241.35㎖에서 반응표면(도 9)은 또한 발효시간의 영향을 주로 받아 발효시간의 경과에 따라 계속 증가하는 편이었으며, 24시간 이후에는 큰 변화가 없었으나 교반속도가 낮은 경우에는 알콜함량이 증가하는 경향이었다.As an experimental plan for alcohol fermentation optimization, SAS (statistical analysis system) package was used for response surface analysis according to the central composite design. Experimental variables for alcohol fermentation were hydrolysis (X 1 ), shaking speed (X 2 ) and fermentation time (X 3 ). These factors were -2, -1, 0, 1, 2 as shown in Table 5. The experiment was coded by level. As a result, the alcohol content change of fermentation process by alcoholic yeast under experimental conditions designed by the central synthesis plan is shown in Table 6, and the contour diagram and the four-dimensional reaction surface are shown in Figs. 10 is shown respectively. Reaction surface regression analysis was performed for alcohol content according to the amount of hydrolysis (100-300ml), stirring speed (0-120rpm) and fermentation time (0-48hr), which are the most important variables in alcohol fermentation by yeast strain of Zygosaccharomyces fermentati . R 2 of the regression equation was 0.9254 and the significance was 0.0091, which was recognized at the significance level within 1% (Table 7). The effect of fermentation conditions on alcohol content was mainly affected by fermentation time, and the influence of hydrolysis and stirring speed was slight (Table 8). In the reaction surface regression analysis for alcohol fermentation, the normal point showed the form of saddle point (Table 9), and the ridge analysis showed that the optimum alcohol fermentation condition and alcohol content were 241.35mL of hydrolysis, 8.05rpm stirring speed and 34.81 fermentation time. hr was 8.31%. Therefore, as a result of fixing the parameters at the optimum condition and drawing the contour diagram, the reaction surface (Fig. 7) having the fermentation time fixed at 34.81 hours increased the alcohol content during the fermentation under the condition of low water content and low stirring speed. It decreased when the stirring speed was high. However, when the amount of water and the stirring speed were too low, the alcohol fermentation was found to be somewhat late. And the reaction surface (Fig. 8) fixed to the stirring speed at 8.05rpm, which is the optimum condition of the stirring speed, tended to increase with the passage of the fermentation time, mainly affected by the fermentation time. However, little changed after 30 hours of fermentation. At 241.35 ml, which is the optimum condition for the amount of hydrolysis, the reaction surface (Fig. 9) was also mainly increased by the fermentation time, and continued to increase with the passage of the fermentation time. There was no significant change after 24 hours, but the stirring speed was low. The alcohol content tended to increase.
한편, 알콜 발효조건인 가수량, 교반속도 및 발효시간은 상호 의존성을 가지고 있으므로 세가지 조건 모두를 변화시키면서 반응표면분석을 행하여 4차원 반응표면을 그려 본 결과는 도 10에 나타낸 바와 같았다. 4차원 반응표면은 알콜 발효시간이 경과할수록 알콜함량은 증가하는 경향이었으나 30∼40시간의 범위에서 가장 높았으며, 그 이상의 시간에서는 다소 줄어들었다. 그리고 최적 알콜발효조건은 두 개의 패턴으로 나타났는데, 그 중 하나의 조건은 발효시간 35시간에서 교반속도가 낮고 가수량이 많은 조건에서 알콜함량이 8% 이상으로 높게 나타났으며, 다른 하나의 조건은 같은 35시간의 발효에서 교반속도가 높고 가수량이 적은 조건에서 알콜함량이 8% 이상으로 높게 나타나 교반속도와 가수량은 반비례 관계에 있음을 알 수 있었다. 따라서 능선분석에 의해 결정된 최적조건은 이러한 두 개의 최적조건 중 알콜함량이 더 높은 최적 조건임을 알 수 있으며, 가수량이 많고 교반속도가 낮을수록 생산량이 많고 발효공정의 경제성을 감안할 때 교반속도가 낮고 가수량이 많은 조건이 알콜발효 최적 조건임을 알 수 있었다.On the other hand, since the alcoholic fermentation conditions, the amount of hydrolysis, the stirring speed and the fermentation time have a mutual dependency, the result of drawing the four-dimensional reaction surface by performing reaction surface analysis while changing all three conditions was as shown in FIG. The four-dimensional reaction surface tended to increase with increasing alcohol fermentation time, but it was highest in the range of 30-40 hours and decreased slightly over that time. The optimum alcohol fermentation conditions appeared in two patterns, one of which was found to be higher than 8% of alcohol content under low stirring and high hydrolysis conditions at 35 hours of fermentation. In the same fermentation for 35 hours, the alcohol content was higher than 8% at high stirring speed and low water content, indicating that the stirring speed was inversely related. Therefore, the optimal condition determined by the ridge analysis is that the alcohol content among these two optimum conditions is the higher optimal condition.The higher the water content and the lower the stirring speed, the higher the yield and the economical efficiency of the fermentation process. It was found that a large amount of condition is the optimum condition for alcohol fermentation.
제 2 공정: 초산발효 조건Second process: acetic acid fermentation conditions
초산발효 최적화를 위하여 알콜발효와 같이 중심합성 계획(central composite design)을 사용하였으며 반응표면 회귀분석을 위해서 SAS(statistical analysis system) package를 사용하였다. 초산발효조건은 독립변수로 진탕속도(X1), 발효시간(X2)을 설정하였으며, 이들 요인변수들은 표 10와 같이 -2, -1, 0, 1, 2의 5수준으로 부호화하여 실험하였다. 실험결과, 총산에 대한 R2는 상기 제 1 공정의 표 7에 나타낸 바와 같이 0.9190로 높게 나타났으며, 유의성은 0.0264로 5% 이내의 유의수준에서 인정되었다. 교반속도에 따른 총산의 변화는 표 11에 나타낸 바와 같이 150rpm과 200rpm에서 가장 높게 나타나 150∼200rpm 사이에서 교반하는 것이 적당하였으며, 시간의 경과에 따라서도 150rpm에서 총산이 가장 빠르게 증가함을 볼 수 있었다. 총산에 대한 초산발효조건의 영향은 표 12에서와 같이 교반속도와 발효시간 모두 초산발효에 크게 영향을 미쳤으며, 교반속도와 발효시간이 증가할수록 증가하였다. 초산발효의 최적조건은 교반속도 190rpm 및 발효시간 270hr 이상에서 발효하였을 때에 총산이 가장 높게 나타났다. 능선분석에 의한 최적조건(상기 제 1 공정의 표 9)은 190.74 rpm, 279.67hr로써 예측된 총산이 5.54%이었다.In order to optimize acetic acid fermentation, we used central composite design like alcoholic fermentation and SAS (statistical analysis system) package for response surface regression analysis. Acetic acid fermentation conditions were set as independent variables shaking speed (X 1 ), fermentation time (X 2 ), these factor variables were coded to 5 levels of -2, -1, 0, 1, 2 as shown in Table 10 It was. As a result, R 2 for total acidity was as high as 0.9190 as shown in Table 7 of the first step, and significance was recognized at a significance level within 5% at 0.0264. The total acid change according to the stirring speed was the highest at 150rpm and 200rpm, as shown in Table 11, and it was appropriate to stir between 150 ~ 200rpm, and the total acid increased at 150rpm as time passed. . The effect of acetic acid fermentation conditions on total acid had a significant effect on acetic acid fermentation with both stirring speed and fermentation time as shown in Table 12, and increased with increasing stirring speed and fermentation time. The optimum condition of acetic acid fermentation was the highest when fermentation was carried out at agitation speed of 190rpm and fermentation time of 270hr or more. The optimal condition by ridge analysis (Table 9 of the first process) was 190.74 rpm, 279.67 hr, with an estimated total acidity of 5.54%.
실시예 3: 감자식초 제조 및 성분 분석Example 3: Potato Vinegar Preparation and Component Analysis
상기 실시예 1에서 확립한 최적의 당화조건과 실시예 2에서 반응표면분석으로 확립한 최적의 발효조건에 따라 감자식초를 제조하였다. 감자를 증자하여 파쇄시킨 다음 발효제를 이용하여 당화 및 액화시켰다. 전처리시킨 감자에 10%의 주모를 접종하여 최적조건으로 알콜발효시킨 후 여과하여 여액을 발효기질로 사용하였다. 초산발효는 working volume 4L의 발효조(Jarfermenter, 한국발효기(주), Korea)에 여과된 알콜발효액으로 종초를 10% 접종한 후 발효시켰다. 이때, 당화시 사용하는 효소제와 초산발효시 사용하는 균주는 누룩과Acetobacter속 균주를 각각 사용한 경우(A), 조효소제, 액체 효소를 혼합한 복합효소제 및Acetobacter속 균주를 각각 사용한 경우(B)로 각각 나누어서 초산발효를 실시하였으며 상기 (A), (B) 각각의 경우로 제조한 감자식초의 성분을 분석하였다.Potato vinegar was prepared according to the optimum saccharification conditions established in Example 1 and the optimum fermentation conditions established by reaction surface analysis in Example 2. Potatoes were cooked to grind and then saccharified and liquefied using fermenting agents. Inoculated with 10% of the seedlings in the pretreated potato, alcohol fermentation to the optimum conditions and filtered to use the filtrate as a fermentation substrate. Acetic acid fermentation was fermented after inoculating 10% of the vinegar with an alcoholic fermentation solution filtered in a fermenter (Jarfermenter, Korea Fermenter, Korea) of working volume 4L. In this case, the enzymes used for saccharification and the strains used for acetic acid fermentation were used when strains of Nuruk and Acetobacter genus were used (A), coenzyme agents, complex enzymes mixed with liquid enzyme, and strains of Acetobacter genus (B), respectively. The fermentation of acetic acid was carried out by dividing each, and the components of potato vinegar prepared in each case (A) and (B) were analyzed.
제 1 공정: 감자식초의 pH, 총산, 알콜함량, 아미노태질소, 총페놀성물질, 환원당 함량First step: potato vinegar pH, total acid, alcohol content, amino nitrogen, total phenolic substance, reducing sugar content
상기 제조한 감자식초의 pH는 pH meter( Model 671, Metrohm Co., Swiss)를 사용하여 측정하였으며, 총산은 0.1N NaOH 용액으로 중화적정하여 초산으로 환산하였다. 환원당은 DNS 법으로 측정하여 글루코스로 작성한 표준곡선과 비교하여 그 함량을 표시하였다. 알콜함량 측정은 배양액을 원심분리한 후 상등액을 증류하여 alcohol hydrometer로 측정한 값을 Gay Lussac table로 환산하여 계산하였다. 아미노태질소 함량은 Formol 적정법으로 측정하였다. 총페놀성 물질 함량은 Folin-Denis법을 이용하여 측정하였다. 실험결과, 표 13에 나타낸 바와 같이 pH는 누룩으로 당화시키고Acetobacter속 균주를 이용하여 초산발효시킨 감자식초(A)는 3.09로 높았고 감자식초(B)는 2.90으로 낮았다. 총산도 감자식초(A)가 6.12이고 감자식초(B)는5.40으로 낮았다. 환원당은 감자식초(A)가 528.40로 높았고 감자식초(B)는 165.58로 낮았다. 아미노태질소 함량은 감자식초(A)가 886.67mg%로, 감자식초(B)는 43.82mg%에 비해서 상당히 높았다. 총페놀성 물질 함량도 감자식초(A) 89.35, 감자식초(B) 30.72mg%를 나타냈다. The pH of the prepared potato vinegar was measured using a pH meter (Model 671, Metrohm Co., Swiss), the total acid was neutralized titration with 0.1N NaOH solution was converted to acetic acid. Reducing sugars were measured by DNS method and compared with the standard curve prepared with glucose. Alcohol content was measured by centrifugation of the culture broth, distillation of the supernatant, and the value measured by alcohol hydrometer. Amino nitrogen content was measured by Formol titrimetric method. Total phenolic substance content was measured using the Folin-Denis method. As shown in Table 13, the pH was glycosylated with yeast andAcetobacterPotato vinegar (A) fermented by acetic acid strains was high as 3.09 and potato vinegar (B) as low as 2.90. Total acidity of potato vinegar (A) was 6.12 and potato vinegar (B) was low as 5.50. Reducing sugar had a high potato vinegar (A) of 528.40 and a low potato vinegar (B) of 165.58. The amino nitrogen content was 886.67 mg% in potato vinegar (A) and significantly higher than 43.82 mg% in potato vinegar (B). The total phenolic substance content also showed 89.35 potato vinegar (A) and 30.72 mg% potato vinegar (B).
제 2 공정: 감자식초의 색상, 갈색도 및 탁도Second Process: Color, Brown and Turbidity of Potato Vinegar
상기 제조한 감자식초의 색상은 색차계(Chromameter, Model CR-310, Minolta Co., Japan) Hunter's L, a, b 값을 측정하였으며 갈색도는 spectrophotometer(Shimadzu Co.)를 이용해서 420nm에서, 탁도는 일정량 시료를 취하여 660㎚에서의 흡광도로 측정하였다. 실험결과, 표 14에 나타낸 바와 같이 감자식초(A)의 색상은 감자식초(B)에 비해서 L값이 낮고 갈색도가 낮으며 탁도가 높았으며, 감자식초 (B)의 경우 L값이 높고 갈색도는 낮아서 외적으로 우수하였다.The color of the prepared potato vinegar was measured by the color difference meter (Chromameter, Model CR-310, Minolta Co., Japan) Hunter's L, a, b, and the brownness was turbidity at 420 nm using a spectrophotometer (Shimadzu Co.). The sample was taken at a constant amount and measured by absorbance at 660 nm. As a result, as shown in Table 14, the color of potato vinegar (A) was lower in L value, lower in brown color, and higher in turbidity than potato vinegar (B). The degree was low and excellent externally.
제 3 공정: 감자식초의 유기산 및 유리당 분석Process 3: Organic Acid and Free Sugar Analysis of Potato Vinegar
상기 제조한 감자식초의 유리당 및 유기산 분석은 감자식초 원액을 헥산(hexane)으로 유지성분을 제거하고 0.45㎛ 막 여과(membrane filter)의 여과와 Sep-pak C18로 색소 및 단백질성분을 제거하여 표 15의 조건으로 분석하였다. 실험결과, 표 16에 나타낸 바와 같이 감자식초의 유기산으로 옥살산(oxalic acid), 타르타르산(tartaric acid), 말산(malic acid), 초산(acetic acid), 구연산(citric acid), 숙신산(succinic acid), 락트산(lactic acid)이 확인되었으며 감자식초(A)에서 옥살산(oxalic acid) 358.72mg%, 말산(malic acid) 55.07mg%, 초산(acetic acid) 3544.28mg%, 구연산(citric acid) 1258.71mg%, 숙신산(succinic acid) 278.80mg%로 감자식초(B)에 비해서 유기산의 함량이 높았다. 유리당 성분은 표 17에 나타낸 바와 같이 프럭토스(fructose), 글루코스(glucose), 갈락토스(galactose), 슈크로스(sucrose), 말토스(maltose)가 확인되었고, 조효소제 및 액체효소의 복합효소제 및Acetobacter속 균주를 이용한 감자식초(B)의 총유리당 함량이 256.62mg%로 낮았다. 한편 감자식초(B)에서 슈크로스(sucrose)의 함량은 누룩을 이용하여 당화시킨 감자식초(A) 보다 크게 높았다.The analysis of free sugar and organic acid of the prepared potato vinegar was carried out by removing the oil and fat components of the potato vinegar stock solution with hexane, removing the pigment and protein components by filtration of 0.45 μm membrane filter and Sep-pak C 18 . 15 conditions were analyzed. As a result, as shown in Table 16, the organic acids of potato vinegar are oxalic acid, tartaric acid, malic acid, acetic acid, citric acid, succinic acid, Lactic acid was identified, 358.72mg% of oxalic acid, 55.07mg% of malic acid, 3544.28mg% of acetic acid, 1258.71mg% of citric acid in potato vinegar (A) Succinic acid (278.80mg%) was higher in organic acid than potato vinegar (B). Fructose, glucose, galactose, sucrose and maltose were identified as free sugar components, as shown in Table 17. Coenzyme and liquid enzyme complex enzymes and Acetobacter The total free sugar content of potato vinegar (B) using the genus strain was low as 256.62mg%. On the other hand, the content of sucrose (sucrose) in potato vinegar (B) was significantly higher than potato vinegar (A) saccharified using Nuruk.
제 4 공정: 감자식초의 유리아미노산 분석Fourth step: free amino acid analysis of potato vinegar
상기 제조한 감자식초의 유리 아미노산 정량은 시료 10mL에 에탄올 30mL을 가한 다음 하룻밤 실온에 방치시켜 단백질을 침전 제거한 다음 원심분리 후 상징액을 건조시켜 표 18에 나타낸 조건에 따라 아미노산 자동분석기로 분석하였다. 실험결과, 표 19에 나타낸 바와 같이 누룩을 이용한 감자식초(A)에서 글루타민산(glutamic acid) 함량이 각각 17.48로 특이적으로 높았으며 2종의 감자식초 모두 알라닌(alanine)의 함량이 20mg% 이상이었다.The free amino acid quantification of the prepared potato vinegar was added to 30 mL of ethanol to 10 mL of the sample, and then allowed to stand overnight at room temperature to precipitate proteins, and after centrifugation, the supernatant was dried and analyzed by an amino acid autoanalyzer according to the conditions shown in Table 18. As a result, as shown in Table 19, the content of glutamic acid was 17.48 in the potato vinegar (A) using Nuruk, and the content of alanine was more than 20mg% in the two kinds of potato vinegar. .
실시예 4: 감자식초 제조의 규모확대Example 4: Scale-up of Potato Vinegar Production
본 실시예에서는 상기 실시예 1, 2, 3에서 얻어진 실험실 규모의 결과에 기초하여 감자식초 제조공정을 공장규모로 확대하였다. 먼저 원료 감자를 검수·검량한 다음 미숙감자 및 병해충감자를 선별하여 제거하는 원료선별 공정; 선별된 원료 감자를 자동세척기로 깨끗하게 세척하는 원료·세척 공정; 자동파쇄기로 6메쉬 크기로 파쇄하는 공정; 파쇄한 원료 감자를 증자솥에 넣고 정제수를 넣어 95℃에서 1시간 증자하는 공정 이때 액화효소를 첨가; 증자된 원료를 60℃로 냉각하여 발효제(누룩, 조효소제, 정제효소 또는 액체효소)를 첨가하여 5∼6시간 60℃를 유지하면서 교반, 당화하는 공정; 당화된 원료를 담금 탱크에 주입한 후 배양한Zygosaccharomyces fermentati속 효모균주를 넣어 1단 담금한 후 48시간 후에 다시 당화 및 액화한 2단 담금 원료를 투입한 다음 60시간 후에 발효를 끝내는 알콜발효공정; 1차발효가 끝난후 착즙기에 착즙과 동시에 여과를 하는 공정; 착즙·여과한 액과Acetobacter속 균주를 종초로 2차발효조에 넣어 6∼7일 동안 초산발효를 완료하는 초산발효공정; 발효가 완료된 액을 48시간 침전탱크에 넣어 침전시킨 후 숙성탱크로 이송하는 침전 및 숙성 공정; 숙성이 끝난 액을 규조토 여과기로 깨끗하게 여과하는 공정; 여과한 액을 살균탱크에 넣어 65℃에서 30분간 살균후 20℃로 냉각하는 살균, 냉각공정; 살균 냉각된 액을 다시 숙성탱크에 넣어 숙성시킨 후 0.5마이크론 휠타로 최종적으로 여과하는 숙성, 여과공정; 깨끗이 여과된 액의 이화학 검사를 실시하여 총산 4.0이상인 액을 선별하여 세척된 PET 또는 병용기에 주입한 후 뚜껑을 닫는 주입공정; 일정수량씩 안상자, 바깥상자에 넣어 포장한 후 제품은 항목별 검사하여 제품규격의 사양과 같이 적합한 제품에 한하여 완제품으로 한 후 출하하는 공정으로 감자식초를 대량 제조하여 상품화하였다.In this example, on the basis of the laboratory scale results obtained in Examples 1, 2, and 3, the potato vinegar manufacturing process was expanded to plant scale. A raw material selection process of first inspecting and inspecting raw potatoes and then selecting and removing immature potatoes and pest insects; Raw material washing process for washing selected raw potatoes cleanly with an automatic washing machine; Shredding into 6 mesh sizes with an automatic shredder; The shredded raw potatoes are placed in a cooker, and purified water is added to increase the temperature at 95 ° C. for 1 hour. Cooling the cooked raw material to 60 ° C., and adding fermentation agent (leaven, coenzyme, purified enzyme or liquid enzyme) to stir and saccharify while maintaining 60 ° C. for 5 to 6 hours; Alcohol fermentation step of injecting the saccharified raw material into the immersion tank and immersing the yeast strain of the cultured Zygosaccharomyces fermentati in one stage and then adding the saccharified and liquefied two-stage immersion raw material again after 48 hours and then finishing the fermentation after 60 hours; Filtration at the same time as the juice after the end of the first fermentation process; Acetic acid fermentation process to complete the fermentation of acetic acid for 6-7 days by putting the juice and the filtered solution and Acetobacter sp. Strain into the secondary fermentation tank as a seed; Precipitation and maturation process to put the fermentation complete solution into the settling tank for 48 hours and then transferred to the aging tank; Filtering the matured liquid cleanly with a diatomaceous earth filter; Sterilizing and cooling the filtered solution into a sterilization tank and sterilizing at 65 ° C. for 30 minutes and then cooling it to 20 ° C .; Aging and filtration of the sterilized cooled liquid in the aging tank again to ripen and finally filtered with a 0.5 micron filter; Performing a physicochemical test of the filtered solution to clean the solution, and then injecting the solution with a total acidity of 4.0 or more and injecting it into the washed PET or bottle, and then closing the lid; After packing a certain quantity into the inner box and outer box, the products were inspected by item and the finished product was made into a finished product and then shipped as a specification of the product standard.
실험예 1: 대량 생산한 감자식초의 보존성Experimental Example 1: Preservation of Mass Produced Potato Vinegar
상기 실시예 4에서 공장규모로 제조한 감자식초를 PET 또는 병용기에 담고 60℃에서 30분간 저온살균한 후 상온은 30℃, 냉장은 10℃ 이하에서 보관하면서 시간경과에 따른 맛, 산도 및 pH변화, 고유의 색상변화, 침전상태, 대장균수, 총세균수를 측정하여 보존력을 테스트하였다. 색상은 색차계(Chromameter, Model CR-310,Minolta Co., Japan) Hunter's L, a, b 값을 측정하였고, pH는 pH meter( Model 671, Metrohm Co., Swiss)를 사용하여 측정하였으며, 총산은 0.1N NaOH 용액으로 중화적정하여 초산으로 환산하였다. 맛은 관능검사로 12명의 관능검사 요원을 선정하여 5점 평점법으로 검사를 실시하였으며, 침전상태는 육안으로 관찰하였고 대장균수는 Deoxycholate배지에 의한법, 총세균수는 plate count agar 평판배지를 이용하였다. 실험결과, 표 20에 나타낸 바와 같이 감자식초 보존 후 식초고유의 맛과 침전 및 산도가 37개월부터 조금씩 변화가 시작하였으며 냉장보관일 때는 37개월까지 제품상의 문제점은 없었고, 38개월부터 제품이 전체적으로 불안정하기 시작하였으며 상온에서는 37개월부터 제품상 문제점을 나타냈다. 따라서 대량 제조한 감자식초는 유통기간을 36개월로 하는 것이 바람직하였다.Potato vinegar prepared in Example 4 in a PET or bottle in a bottle or pasteurized at 60 ℃ for 30 minutes after the pasteurization at room temperature 30 ℃, refrigeration at 10 ℃ or less while keeping the taste, acidity and pH changes over time The preservative ability was tested by measuring the intrinsic color change, sedimentation status, E. coli and total bacterial count. Color was measured by Chromameter (Model CR-310, Minolta Co., Japan) Hunter's L, a, b values, pH was measured using a pH meter (Model 671, Metrohm Co., Swiss), total The acid was neutralized with 0.1N NaOH solution and converted into acetic acid. Twelve sensory agents were selected by sensory evaluation and tested by five-point scoring method. Precipitation was visually observed. Coliform count was determined by Deoxycholate medium and total bacterial count was used by plate count agar plate. It was. As a result, as shown in Table 20, the taste, precipitation and acidity of vinegar after storage of potato vinegar began to change little by little from 37 months, and there were no product problems until 37 months when refrigerated. At room temperature, the product showed problems from 37 months. Therefore, the mass production of potato vinegar was desirable to have a shelf life of 36 months.
이상, 상기 실시예를 통하여 설명한 바와 같이 본 발명은 파쇄한 감자에 가수하고 누룩, 정제효소, 조효소제 또는 액체효소 등의 혼합효소를 첨가하여 당화시킨 후 1단계로 주모를 첨가하여 알콜발효시키고 2단계로 종초를 첨가하여 초산발효시키므로써 실험실 규모에서 감자식초를 제조하는 뛰어난 효과가 있고 상기 실험실 규모의 감자식초 제조방법에 기초하여 공장 규모로 보존성이 우수한 감자식초를 제조하는 뛰어난 효과가 있으므로 식품산업상 매우 유용한 발명인 것이다.As described above, the present invention is hydrolyzed to shredded potatoes and saccharified by the addition of mixed enzymes such as yeast, purified enzyme, coenzyme or liquid enzyme, and then fermented by alcohol in two stages. The fermentation of acetic acid by adding the vinegar to the step has an excellent effect of producing potato vinegar at the laboratory scale, and on the basis of the laboratory-scale potato vinegar production method has an excellent effect of producing potato vinegar with excellent shelf life on the plant scale It is a very useful invention.
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