KR101793266B1 - The natural preservative manufacturing method of using Mandarin and Natural mineral - Google Patents

The natural preservative manufacturing method of using Mandarin and Natural mineral Download PDF

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KR101793266B1
KR101793266B1 KR1020170102639A KR20170102639A KR101793266B1 KR 101793266 B1 KR101793266 B1 KR 101793266B1 KR 1020170102639 A KR1020170102639 A KR 1020170102639A KR 20170102639 A KR20170102639 A KR 20170102639A KR 101793266 B1 KR101793266 B1 KR 101793266B1
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성수현
정재준
이정옥
강대삼
김세엽
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주식회사 아리바이오
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
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    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
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    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
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    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives

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Abstract

The present invention relates to a method for manufacturing a natural preservative using natural bedrock water and a mandarin concentrate. According to the present invention, toxicity, skin allergy and skin stimulation are minimized. Platinum and silver contained in the natural bedrock water are concentrated and coupled with effective components of mandarin so preservation abilities of an existing natural preservative can be greatly improved.

Description

천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법{The natural preservative manufacturing method of using Mandarin and Natural mineral}BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a natural preservative comprising a natural mineral salt and a mandarin concentrate,

본 발명은 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법에 관한 것으로, 더욱 상세하게는 천연 암반수와 만다린을 이용하기 때문에 독성과 피부 알러지 및 피부 자극을 최소화하면서도 천연 암반수에 함유된 백금 및 은을 농축하여 만다린의 유효성분과 결합시킴으로써 기존 천연 방부제의 방부 능력을 크게 향상시킬 수 있는 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법에 관한 것이다.The present invention relates to a method for producing a natural preservative using natural mineral waters and mandarin concentrate, and more particularly, to a method for producing natural preservatives using natural mineral waters and mandarin concentrate, And a method for producing a natural preservative using natural mineral waters and mandarin concentrate which can significantly improve the preservative ability of existing natural preservatives by combining them with the active ingredients of mandarin.

일반적으로, 방부제(Preservative)라 함은 미생물 증식이나 원하지 않는 화학적 변화로 인한 부패를 방지하기 위해, 음식, 의약품 등에 첨가되는 물질로서, 자연적으로 존재하는 천연 방부재는 소금, 꿀, 목재를 태울 때의 연기 등이 있으나, 식품이나 화장품 등에 제한적으로 이용되기 때문에 합성 방부제를 주로 사용하고 있다. Generally, Preservative is a substance added to foods, medicines, etc. to prevent microbial growth or corruption caused by undesired chemical changes. Natural preservatives that are naturally present include, for example, salt, honey, Smoke, etc., but synthetic preservatives are mainly used because they are limited to foods and cosmetics.

예를 들어 스킨, 로션, 크림, 에센스, 샴푸, 비누, 치약, 및 세정제 등의 각종 화장료는 직접 접촉하는 제품인데다, 포장을 개봉한 후에 비교적 장기간 사용하게 되며, 제품 특성상 변질되기 쉽기 때문에 방부제를 사용하여 방부 처리를 하는 것이 필수적이다. 특히, 근래에는 건강과 웰빙을 중시하는 경향이 증가되고, 이러한 요구를 충족하기 위하여 주로 천연재료를 사용하여 각종 화장료를 제조하기 때문에, 화장료가 변질, 부패될 가능성이 그만큼 증가되고 있다.For example, cosmetics such as skins, lotions, creams, essences, shampoos, soaps, toothpastes, and cleansers are in direct contact with each other. Since they are used for a relatively long period after opening the package, It is necessary to perform a preservative treatment. Particularly, in recent years, there has been an increasing tendency to place importance on health and wellness, and in order to meet such demands, various cosmetic materials are mainly produced using natural materials, and thus the likelihood of cosmetic materials deteriorating and decaying is increasing.

이에 따라, 종래에는 화학물질을 합성하여 이루어지는 합성 방부제를 일정 함량 화장료에 첨가함으로써, 상기 화장료의 변질, 부패를 방지하였다. 이러한 합성 방부제는 화장료에 대한 방부 효과가 탁월하기는 하지만, 화학물질을 합성하여 이루어지는 화학제품이므로 화장료 사용자의 건강에 영향을 미치며, 당연히 건강과 웰빙을 중시하는 화장료 사용자의 요구나 사회 경향과는 배치된다는 문제점이 있다.Accordingly, conventionally, a synthetic preservative made by synthesizing a chemical substance is added to a cosmetic composition in a certain amount to prevent the deterioration and decay of the cosmetic composition. Although these preservatives are excellent in preservative effect on cosmetics, they are chemical products made by synthesizing chemical substances. Therefore, they affect the health of users of cosmetics and naturally have a tendency to be placed with the demands and social trends of users of cosmetics that emphasize health and well- .

한편, 만다린(mandarin)은 만다린계오렌지라고도 하며, 비타민P와 아스코르빈산, 카로티노이드, 리모노이드 플라보노이드, 구마린, 나린제닌 계통의 성분 등이 들어있다. 그 중에서 나린제닌 계통의 성분은 만다린의 껍질 안에 있는 성분인데 항산화작용이 뛰어난 성분으로 산소와 닿으면서 생기는 미생물의 번식을 막아주는 중요한 역할을 한다.Mandarin, also known as mandarin orange, contains vitamin P and ascorbic acid, carotenoids, limonoid flavonoids, guarine, and naringenin ingredients. Among them, the Naringenin component is a component in the shell of mandarin, which is an excellent antioxidant, and plays an important role in preventing the growth of microorganisms that come into contact with oxygen.

또한, 나린제닌은 암 세포에서 손상된 DNA를 복구하는데 도움을 주며 사람의 전립선암 세포 배양물(LNCaP 세포주)에 DNA 복구 효과가 있다. Base Excision Repair(BER)을 자극함으로써 복제 단계에서 DNA 복구 기능을 발휘하는 것으로 알려져 있다. 특히 나린제닌은 간에서 시토크롬 p450(cytochrome p-450) 효소들을 억제하고 발암물질인 아플라톡신 B1의 활성을 저해하여 항산화 효과가 매우 크며, 항염증, 지방감소, 탄수화물 대사 증진, 면역시스템 조절 등에 효과가 있는 것으로 알려져 있다.In addition, naringenin helps repair damaged DNA in cancer cells and has DNA repair effects on human prostate cancer cell cultures (LNCaP cell lines). It is known to exert DNA repair function during replication by stimulating Base Excision Repair (BER). Naringenin inhibits the cytochrome p-450 enzymes in the liver and inhibits the activity of aflatoxin B1, a carcinogen, and has a very high antioxidative effect. It is effective for anti-inflammation, fat reduction, enhancement of carbohydrate metabolism and control of the immune system. .

이와 같은 나린제닌은 상술한 특성으로 인해, 대한민국 등록특허 제10-1268325호에 개시된 바와 같이 알코올성 간질환 예방용 조성물로 이용되거나, 대한민국 등록특허 제10-0500840호에 개시된 바와 같이 노인성 치매 환자, 고령화로 인한 기억력 감퇴현상의 개선제 등으로 개발되고 있는 실정이다.Due to the above-mentioned characteristics, such naringenin can be used as a composition for preventing alcoholic liver disease as disclosed in Korean Patent Registration No. 10-1268325, or as a composition for preventing or treating senile dementia, And the improvement of the memory decline phenomenon due to the fact that the situation is being developed.

다만, 나린제닌은 미생물 번식을 억제하는 효능이 있음에도 지용성이기 때문에 천연방부제로서 활용이 되지 않고 있다. 구체적으로 지용성 성분은 흡수가 되지 않고 수용성 성분과는 섞이지 않기 때문에 물과 공기 중에 번식하는 미생물의 번식을 억제하는 효과를 제대로 발휘하기 힘들다. 따라서 나린제닌을 천연방부제로서 사용하기 위해서는 지용성 성분을 수용성으로 개질하고 가격 경쟁력을 위해 수율을 향상시키는 노력이 필요한 실정이다.However, Narinenin is not effective as a natural preservative because it is fat-soluble, although it has the effect of inhibiting microbial propagation. Specifically, since the fat-soluble component is not absorbed and does not mix with the water-soluble component, it is difficult to exert the effect of suppressing the propagation of microorganisms propagating in water and air. Therefore, in order to use naringenin as a natural preservative, it is necessary to modify the lipophilic component to be water-soluble and to improve the yield for cost competitiveness.

이러한 문제를 해결하기 위하여 대한민국 등록특허 제10-1612936호에는 만다린을 이용한 천연 방부제가 개시되어 있었다. 다만, 만다린 추출물만으로 방부 능력을 극대화하는 것은 한계가 나타났다.In order to solve such a problem, Korean Patent No. 10-1612936 discloses a natural preservative using mandarin. However, maximizing preservation ability with mandarin extract alone was limited.

1. 대한민국 등록특허 제10-0786564호 (천연 방부제 조성물의 제조 방법)1. Korean Patent No. 10-0786564 (Method for producing natural preservative composition) 2. 대한민국 등록특허 제10-0782599호 (복합천연방부제)2. Korean Patent No. 10-0782599 (Compound Natural Preservative) 3. 대한민국 등록특허 제10-1268325호 (알코올성 간질환 예방용 조성물)3. Korean Patent No. 10-1268325 (composition for the prevention of alcoholic liver disease) 4. 대한민국 등록특허 제10-0500840호 (유자로부터 나린제닌을 정제하는 방법 및 그 용도)4. Korean Patent Registration No. 10-0500840 (Method for Purifying Narinin from Citron and its Use) 5. 대한민국 등록특허 제10-1612936호 (만다린을 이용한 천연 방부제 제조방법)5. Korean Patent No. 10-1612936 (Method for producing natural preservative using mandarin)

상기와 같은 문제점을 감안한 본 발명이 해결하고자 하는 과제는, 천연 암반수와 만다린을 이용하기 때문에 독성과 피부 알러지 및 피부 자극을 최소화하면서도 천연 암반수에 함유된 백금 및 은을 농축하여 만다린의 유효성분과 결합시킴으로써 기존 천연 방부제의 방부 능력을 크게 향상시킬 수 있는 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법을 제공하는 것이다.SUMMARY OF THE INVENTION The present invention has been made in view of the above problems, and it is an object of the present invention to solve the above problems by using natural mineral water and mandarin to minimize the toxicity, skin allergy and skin irritation and to concentrate platinum and silver contained in natural mineral water, It is intended to provide a method for producing natural preservatives using natural mineral waters and mandarin concentrates, which can significantly improve the preservative ability of existing natural preservatives.

본 발명의 해결하고자 하는 과제는 이상에서 언급된 것들에 한정되지 않으며, 언급되지 아니한 다른 해결과제들은 아래의 기재로부터 당업자에게 명확하게 이해되어 질 수 있을 것이다.The problems to be solved by the present invention are not limited to those mentioned above, and other solutions not mentioned can be clearly understood by those skilled in the art from the following description.

상기와 같은 과제를 해결하기 위한 본 발명에 따른 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법은 적어도 백금과 은 성분이 함유된 천연 암반수를 농축한 천연 암반수 농축액을 마련하는 단계와; 나린제린, 비타민C, 폴리페놀 중 적어도 하나의 성분이 함유된 만다린 농축액을 마련하는 단계와; 용매에 상기 천연 암반수 농축액과, 만다린 농축액와, 수소화붕소나트륨을 투입한 농축액 혼합액을 마련한 다음, 상기 농축액 혼합액에 함유된 수분을 분리하여 제거하는 단계와; 상기 농축액 혼합액에 들어있는 수분이 제거된 농축액 혼합액에서 에틸아세테이트를 제거하여 얻은 추출물에 용매를 혼합하여 희석하는 단계;를 포함하는 것을 특징으로 한다.According to another aspect of the present invention, there is provided a method of preparing a natural preservative using natural mineral waters and a mandarin concentrate according to the present invention comprises the steps of: preparing a natural mineral water concentrate containing at least platinum and silver components; Preparing a mandarin concentrate containing at least one of naringenin, vitamin C, and polyphenol; Separating and removing the water contained in the concentrate mixture liquid after providing the concentrate mixture in which the natural mineral water concentrate, mandarin concentrate and sodium borohydride are added to the solvent; And diluting the extract obtained by removing ethyl acetate from the concentrated liquid mixture removed in the concentrated liquid mixture by mixing the extract with a solvent.

또한, 본 발명에 따른 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법에 있어서, 천연 암반수 농축액은, 천연 암반수를 40~50℃, 0.1~1 Torr의 진공 상태에서 20~30시간 동안 진공 건조하여 얻어지며, 상기 만다린 농축액은, 세척한 만다린 껍질을 1차 분쇄하는 단계와; 상기 1차 분쇄된 만다린 분쇄물을 1차 교반 숙성하는 단계와; 상기 1차 교반 숙성된 분쇄물을 2차 분쇄하는 단계와; 상기 2차 분쇄된 만다린 분쇄물 100중량부를 기준으로 물 20~40중량부와, 에틸아세테이트 80~120중량부를 혼합한 만다린 혼합물을 마련하는 단계와; 상기 만다린 혼합물을 2차 교반 숙성하는 단계와; 상기 2차 교반 숙성된 만다린 혼합물에서 물과 에틸아세테이트를 제거하여 추출물을 얻는 단계와; 상기 추출물에 물 80~120중량부와, 수용성 성분 0.001~0.1중량부를 혼합한 혼합액을 마련하는 단계와; 상기 혼합액을 농축시키는 단계;를 통해 얻어지는 것을 특징으로 한다.In the method for producing a natural preservative using natural mineral waters and mandarin concentrate according to the present invention, the natural mineral waters concentrate can be obtained by vacuum drying natural mineral waters under a vacuum of from 40 to 50 ° C. and from 0.1 to 1 Torr for 20 to 30 hours Wherein the mandarin concentrate comprises: firstly grinding the washed mandarin shell; Aging the primary pulverized mandarin crushed material with primary agitation; Secondly pulverizing the primary aged aged pulverized product; Preparing mandarin mixture in which 20 to 40 parts by weight of water and 80 to 120 parts by weight of ethyl acetate are mixed based on 100 parts by weight of the secondary pulverized mandarin crushed product; Aging the mandarin mixture with secondary agitation; Removing water and ethyl acetate from the secondary agitation-aged mandarin mixture to obtain an extract; Preparing a mixed solution comprising 80 to 120 parts by weight of water and 0.001 to 0.1 part by weight of a water-soluble component; And concentrating the mixed solution.

또한, 본 발명에 따른 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법에 있어서, 농축액 혼합액은 용매로서 에틸아세테이트 100중량부를 기준으로 상기 천연 암반수 농축액 1~50중량부와, 상기 만다린 농축액 1~50중량부와, 상기 수소화붕소나트륨 0.01~1중량부로 이루어지는 것을 특징으로 한다.In the method for preparing a natural preservative using natural mineral waters and a mandarin concentrate according to the present invention, the concentrate mixture is prepared by mixing 1 to 50 parts by weight of the natural mineral water concentrate, 1 to 50 parts by weight of the mandarin concentrate, And 0.01 to 1 part by weight of the sodium borohydride.

또한, 본 발명에 따른 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법에 있어서, 천연 암반수 농축액에 함유된 은 성분은 은 카르보닐([Ag(CO)3]2)에 상기 나린제린, 비타민C, 폴리페놀의 카르보닐기가 결합하여 착화합물을 형성하고, 상기 백금은 상기 착화합물의 배위 결합시 촉매로 작용하고, 상기 수소화붕소나트륨은 환원제로 작용하는 것을 특징으로 한다.Further, the method for producing a natural preservative with natural ambansu and mandarin concentrate according to the invention, the component is a carbonyl ([Ag (CO) 3] 2) Vitamin the Naryn jerin, the C-containing natural ambansu concentrate, The carbonyl group of the polyphenol is combined to form a complex, and the platinum acts as a catalyst in the coordination bond of the complex, and the sodium borohydride acts as a reducing agent.

본 발명에 따른 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법은 천연 암반수와 만다린을 이용하기 때문에 독성과 피부 알러지 및 피부 자극을 최소화하면서도 천연 암반수에 함유된 백금 및 은을 농축하여 만다린의 유효성분과 결합시킴으로써 기존 천연 방부제의 방부 능력을 크게 향상시킬 수 있는 효과가 있다.Since natural mineral waters and mandarin are used, the method of producing a natural preservative using natural mineral waters and mandarin concentrate according to the present invention minimizes toxicity, skin allergy and skin irritation, while concentrating platinum and silver contained in natural mineral waters, The preservation ability of the existing natural preservative can be greatly improved.

본 발명의 효과는 이상에서 언급된 것들에 한정되지 않으며, 언급되지 아니한 다른 해결과제들은 아래의 기재로부터 당업자에게 명확하게 이해되어 질 수 있을 것이다.The effects of the present invention are not limited to those mentioned above, and other solutions not mentioned may be clearly understood by those skilled in the art from the following description.

도 1은 본 발명의 바람직한 실시예에 따른 만다린을 이용한 천연 방부제 제조방법의 제조공정 순서도이다.
도 2a 및 도 2b는 본 발명의 천연 방부제 원액 및 천연 방부제를 촬영한 사진이다.
도 3a 내지 도 3d는 실시예 1의 천연 방부제에 대하여 항균 시험을 한 결과를 나타낸 시험데이터이다.
FIG. 1 is a flowchart illustrating a manufacturing process of a method for manufacturing a natural preservative using mandarin according to a preferred embodiment of the present invention.
FIGS. 2A and 2B are photographs of a stock solution of a natural preservative of the present invention and a natural preservative. FIG.
Figs. 3A to 3D are test data showing results of antibacterial tests on the natural preservative of Example 1. Fig.

본 발명을 설명함에 있어서, 관련된 공지기능 혹은 구성에 대한 구체적인 설명이 본 발명의 요지를 불필요하게 흐릴 수 있다고 판단되는 경우 그 상세한 설명은 생략한다. 또한, 후술되는 용어들은 본 발명에서의 기능을 고려하여 정의된 용어들로서 이는 사용자의 의도 또는 판례 등에 따라 달라질 수 있다. 그러므로 그 정의는 본 명세서 전반에 걸친 내용을 토대로 내려져야 할 것이다.In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear. In addition, the terms described below are defined in consideration of the functions of the present invention, and these may vary depending on the intention or precedent of the user. Therefore, the definition should be based on the contents throughout this specification.

도 1은 본 발명의 바람직한 실시예에 따른 만다린을 이용한 천연 방부제 제조방법의 제조공정 순서도이다.FIG. 1 is a flowchart illustrating a manufacturing process of a method for manufacturing a natural preservative using mandarin according to a preferred embodiment of the present invention.

먼저, 본 발명은 천연 암반수와, 대한민국 등록특허 제10-1612936호에 개시된 만다린 농축액을 혼합하여 식품 또는 화장품에 첨가하여 인체에 유해한 영향이 미치는 것을 최소화할 수 있으며, 상기 등록특허에 비해 방부 효과를 크게 향상시킬 수 있는 천연 방부제에 관한 것이다.First, the present invention can minimize the harmful effects on the human body by adding natural minerals and a mandarin concentrate disclosed in Korean Patent No. 10-1612936 to foods or cosmetics, And a natural preservative which can be greatly improved.

본 발명에 따른 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법은 적어도 백금과 은 성분이 함유된 천연 암반수를 농축한 천연 암반수 농축액을 마련하는 S1단계와, 나린제린, 비타민C, 폴리페놀 중 적어도 하나의 성분이 함유된 만다린 농축액을 마련하는 S2단계와, 용매에 상기 천연 암반수 농축액과, 만다린 농축액와, 수소화붕소나트륨을 투입한 농축액 혼합액을 마련한 다음, 상기 농축액 혼합액에 함유된 수분을 분리하여 제거하는 S3단계와, 상기 농축액 혼합액에 들어있는 수분이 제거된 농축액 혼합액에서 에틸아세테이트를 제거하여 얻은 추출물에 용매를 혼합하여 희석하는 S4단계를 포함하여 이루어질 수 있다.A method for preparing a natural preservative using natural mineral waters and a mandarin concentrate according to the present invention comprises a step S1 of providing a concentrated natural mineral water concentrate containing at least platinum and silver components and at least one of naringenin, vitamin C and polyphenol A step S2 of preparing a mandarin concentrate containing the components of the concentrate mixture, and a step of preparing a concentrate mixture liquid in which the natural minerals concentrate, the mandarin concentrate and the sodium borohydride are added to the solvent, and then the water contained in the concentrate mixture is separated and removed And a step S4 in which a solvent is mixed and diluted with the extract obtained by removing ethyl acetate from the concentrated liquid mixture removed in the concentrated liquid mixture.

상기 S1단계의 천연 암반수 농축액은 천연 암반수를 건조하여 얻을 수 있는데, 예를 들어 40~50℃, 0.1~1 Torr의 진공 상태에서 20~30시간 동안 진공 건조하여 얻어지는 것을 예시할 수 있다.The natural mineral water concentrate in step S1 can be obtained by drying natural mineral waters. For example, it can be obtained by vacuum drying at 40 to 50 DEG C and 0.1 to 1 Torr in a vacuum state for 20 to 30 hours.

상기 천연 암반수에는 주요 미네랄 성분(ppm 단위)인 마그네슘(Mg), 나트륨(Na), 칼륨(K), 칼슘(Ca), 및 미세 미네랄 성분(ppb 단위)인 백금(Pt), 은(Ag) 등을 함유하고 있다. 상기 S1단계에서는 상기 천연 암반수에 함유된 성분 중에서 초 극미량 함유된 백금(Pt), 은(Ag)을 농축하는 것을 주요 목적으로 한다.The natural minerals include platinum (Pt), silver (Ag), magnesium (Mg), sodium (Na), potassium (K), calcium (Ca) and fine minerals And so on. In the step S1, the main object is to concentrate platinum (Pt) and silver (Ag) contained in the ultramafic content among components contained in the natural mineral water.

여기서, 상기 백금(Pt)은 상기 S3단계에서 일어나는 반응에 대하여 촉매 역할을 하고, 상기 은(Ag) 성분은 나린제린 등과 함께 반응물이 된다.Here, the platinum (Pt) acts as a catalyst for the reaction occurring in the step S3, and the silver (Ag) component becomes a reactant together with the naringin and the like.

상기 S1단계의 만다린 농축액은 세척한 만다린 껍질을 1차 분쇄하는 단계와, 상기 1차 분쇄된 만다린 분쇄물을 1차 교반 숙성하는 단계와, 상기 1차 교반 숙성된 분쇄물을 2차 분쇄하는 단계와, 상기 2차 분쇄된 만다린 분쇄물 100중량부를 기준으로 물 20~40중량부와, 에틸아세테이트 80~120중량부를 혼합한 만다린 혼합물을 마련하는 단계와, 상기 만다린 혼합물을 2차 교반 숙성하는 단계와, 상기 2차 교반 숙성된 만다린 혼합물에서 물과 에틸아세테이트를 제거하여 추출물을 얻는 단계와, 상기 추출물에 물 80~120중량부와, 수용성 성분 0.001~0.1중량부를 혼합한 혼합액을 마련하는 단계와, 상기 혼합액을 농축시키는 단계를 통해 얻어지는 것을 예시할 수 있다. 만다린 농축액에 대해서는 대한민국 등록특허 제10-1612936호에 이미 개시되어 있으므로 보다 구체적인 설명은 생략한다.The mandarin concentrate of step S1 is obtained by firstly pulverizing the washed mandarin shells, aging the primary pulverized mandarin pulverized product with primary stirring, secondary pulverizing the primary pulverized aged pulverized product And 20 to 40 parts by weight of water and 80 to 120 parts by weight of ethyl acetate based on 100 parts by weight of the secondary pulverized mandarin crushed product; and a step of aging the mandarin mixture by the second agitation Preparing a mixed solution of 80 to 120 parts by weight of water and 0.001 to 0.1 part by weight of a water-soluble component in the extract, removing water and ethyl acetate from the secondary aged mandarin mixture to obtain an extract, , And a step of concentrating the mixed solution. The mandarin concentrate is already disclosed in Korean Patent No. 10-1612936, and thus a more detailed description thereof will be omitted.

그리고 만다린 농축액에는 비타민P와 비타민 C(아스코르빈산), 카로티노이드, 리모노이드 플라보노이드, 구마린, 나린제닌 계통의 성분 등이 들어있다. 그 중에서 나린제닌 계통의 성분은 만다린의 껍질 안에 있는 성분인데 항산화작용이 뛰어난 성분으로 산소와 닿으면서 생기는 미생물의 번식을 막아주는 중요한 역할을 한다. 따라서 만다린 껍질에 함유된 나린제닌 성분은 방부제의 역할과 유화제의 역할을 하지만 화학적인 성분은 아니기에 인체에 큰 자극이나 부작용 걱정 없이 사용할 수 있는 장점이 있다.And mandarin concentrate contains vitamin P and vitamin C (ascorbic acid), carotenoids, limonoid flavonoids, guarine and naringenin ingredients. Among them, the Naringenin component is a component in the shell of mandarin, which is an excellent antioxidant, and plays an important role in preventing the growth of microorganisms that come into contact with oxygen. Therefore, the naringenin ingredient contained in the mandarin shell has a role of preservative and emulsifier, but it is not a chemical ingredient, so it can be used without worrying about big irritation or side effects to the human body.

상기 만다린 농축액에 함유된 나린제린, 비타민C, 폴리페놀의 구조식은 아래표 1에서 확인할 수 있도록 Carbonyl기를 가지고 있다.The structural formulas of naringenin, vitamin C and polyphenol contained in the mandarin concentrate are shown in Table 1 below.

나린제린Narinjerin 비타민CVitamin C 폴리페놀Polyphenol

Figure 112017077931852-pat00001
Figure 112017077931852-pat00001
Figure 112017077931852-pat00002
Figure 112017077931852-pat00002
Figure 112017077931852-pat00003
Figure 112017077931852-pat00003

상기 S3단계의 상기 농축액 혼합액은 용매로서 에틸아세테이트 100중량부를 기준으로 상기 천연 암반수 농축액 1~50중량부와, 상기 만다린 농축액 1~50중량부와, 상기 수소화붕소나트륨 0.01~1중량부로 이루어지는 것을 예시할 수 있다.The concentration of the concentrate mixture in step S3 is 1 to 50 parts by weight of the natural mineral water concentrate, 1 to 50 parts by weight of the mandarin concentrate, and 0.01 to 1 part by weight of the sodium borohydride, based on 100 parts by weight of ethyl acetate as a solvent. can do.

상기 천연 암반수 농축액에 함유된 성분 중 예를 들어, 은 성분은 은 카르보닐([Ag(CO)3]2)에 상기 나린제린, 비타민C, 폴리페놀의 카르보닐기(Carbonyl group)가 결합하여 착화합물을 형성함으로써, 나린제린 또는 은 단독으로 사용되는 것에 비해 방부 효과가 현저히 상승된다. 나아가 비타민C, 폴리페놀의 카르보닐기(Carbonyl group)도 은 성분과 결합할 것으로 예상된다.Among the components contained in the natural mineral water concentrate, for example, the silver component is a compound in which a carbonyl group of naringenin, vitamin C and polyphenol binds to silver carbonyl ([Ag (CO) 3 ] 2 ) , The preservative effect is remarkably increased as compared with the case where naringenin or silver is used alone. Furthermore, vitamin C and the carbonyl group of polyphenols are expected to bind to the silver component.

그리고 상기 백금은 상기 착화합물의 배위 결합시 촉매로 작용하고, 상기 수소화붕소나트륨(sodium borohydroride)은 환원제로 작용한다.The platinum acts as a catalyst in the coordination bond of the complex, and the sodium borohydride acts as a reducing agent.

그리고 농축액 혼합액에 함유된 수분을 분리하여 제거하는데, 에틸아세테이트층과 물층으로 상분리되면, 두 용매를 증류로 뽑아낸 후, 선별깔대기로 밑의 물층은 버리고 위에 위치하는 에틸아세테이트는 다시 증류장치로 투입하여 물을 선별해내는 작업공정을 거치게 된다. 추출 후에 얻어낸 에틸아세테이트층에 황산 마그네슘 또는 황산 나트륨과 같은 건조제를 첨가하여 조금이라도 유기층에 남아있는 물기를 제거하는 과정을 3회 정도 반복하여 농축액의 순도를 높이는 것이 바람직하다.Then, the water contained in the concentrate mixture is separated and removed. When the ethyl acetate layer and the water layer are phase-separated, the two solvents are distilled off. The bottom water layer is discarded with a screening funnel. So that the water is sorted out. It is preferable to add a desiccant such as magnesium sulfate or sodium sulfate to the ethyl acetate layer obtained after the extraction to remove the water remaining in the organic layer even a little to repeat the process three times to increase the purity of the concentrate.

상기 S4단계는 상기 농축액 혼합액에서 에틸아세테이트를 분별증류(Fractional Distillation)하여 제거한다. 그 다음 필터로 여과한 다음 분별증류로 얻은 추출물은 식음료, 화장품 등의 기준 및 용도에 맞도록 물 또는 에탄올 등의 용매를 혼합하여 희석하여 천연 방부제 제조를 완료한다.In step S4, ethyl acetate is removed by fractional distillation in the concentrated liquid mixture. Then, the extract obtained by fractional distillation is mixed with a solvent such as water or ethanol to meet the standards and uses of food and beverage, cosmetics and the like and diluted to complete the preparation of the natural preservative.

이하에서는 본 발명에 따른 천연 방부제 제조방법의 보다 바람직한 실시예를 통해 보다 상세히 설명한다.Hereinafter, a more preferred embodiment of the method for producing a natural preservative according to the present invention will be described in more detail.

1. 천연 암반수 농축액 제조1. Manufacture of Natural Mineral Water Concentrate

아래 표 2의 조성비에 나타난 바와 같이 백금과 은 성분이 함유된 천연 암반수를 45℃, 0.5 Torr의 진공 상태에서 24시간 동안 진공 건조하여 천연 암반수 농축액을 마련한다.As shown in the composition ratios in Table 2 below, natural mineral waters containing platinum and silver components are vacuum-dried at 45 ° C under a vacuum of 0.5 Torr for 24 hours to provide a natural mineral water concentrate.

Figure 112017077931852-pat00004
Figure 112017077931852-pat00004

2. 만다린 농축액 제조2. Manufacture of mandarin concentrate

만다린 껍질을 세척한 다음, 분쇄기에 넣고 1차로 분쇄하여 만다린 분쇄물을 마련하고, 1차 분쇄된 만다린 분쇄물을 교반기에 넣고 38℃에서 48시간 동안 교반하면서 숙성시킨다. 그 다음으로, 숙성한 죽 상태의 만다린을 슈퍼레볼루션밀을 이용하여 나노 사이즈로 가공하고, 나노 가공된 만다린 껍질 100kg에 물 30kg과 에틸아세테이트 100kg을 넣고 40℃에서 3시간 동안 교반하면서 숙성시킨 다음, 분리된 껍질과 물은 버린다. 그 다음으로, 진공 건조기를 39℃의 온도, 1torr의 진공도로 설정하여 에틸아세테이트를 증발시킨 다음, 물 100kg과 레시틴과 가티검을 1 : 1의 중량비로 혼합한 수용성 성분 0.1kg을 넣고 교반한다. 그리고, 진공 건조기를 40℃의 온도, 1torr의 진공도로 설정하여 남아있는 에틸아세테이트가 50ppm 미만이 될 때까지 에틸아세테이트를 증발시켜 도 2c와 같이 액상화시킨다. 그 다음으로, 40℃의 온도에서 회전 농축기를 이용하여 농축하고 필터링을 하여 만다린 농축액을 마련한다.The mandarin shell is washed and then ground in a grinder to prepare a mandarin crushed material. The primary crushed mandarin crushed material is agitated in a stirrer while stirring at 38 ° C for 48 hours. Next, aged mandarin was processed into nano-size using Super Revolution Mill, and 30 kg of water and 100 kg of ethyl acetate were added to 100 kg of nano-processed mandarin shell and aged while stirring at 40 ° C for 3 hours, Separated shells and water are discarded. Next, the vacuum dryer was set at 39 DEG C and a degree of vacuum of 1 torr to evaporate ethyl acetate. Then, 0.1 kg of a water-soluble component obtained by mixing 100 kg of water, lecithin and gatifloin at a weight ratio of 1: 1 was added and stirred. Then, the vacuum dryer is set at a temperature of 40 DEG C and a degree of vacuum of 1 torr, and the ethyl acetate is evaporated until the remaining ethyl acetate becomes less than 50 ppm to be liquefied as shown in FIG. 2C. Next, the concentrate is filtered using a rotary condenser at a temperature of 40 ° C to prepare a mandarin concentrate.

3. 농축액 혼합액 제조3. Preparation of concentrated liquid mixture

에틸아세테이트 100중량부를 기준으로 천연 암반수 농축액 60중량부와, 만다린 농축액 40중량부와, 수소화붕소나트륨 0.1중량부를 혼합하여 농축액 혼합액을 마련한 다음, 1시간 동안 교반한 다음 교반을 중지하여 에틸아세테이트층과 물층으로 상분리시킨다. 에틸아세테이트와, 물을 증류로 뽑아낸 후, 선별깔대기로 밑의 물층은 버리고 위에 위치하는 에틸아세테이트는 다시 증류장치로 투입하여 물을 선별해내는 작업공정을 수행한다. 60 parts by weight of a natural mineral water concentrate, 40 parts by weight of a mandarin concentrate and 0.1 part by weight of sodium borohydride were added to 100 parts by weight of ethyl acetate, and the mixture was stirred for 1 hour. After stirring, Phase separation into a water layer. Ethyl acetate and water are removed by distillation. The lower layer of water is discarded with a screening funnel. Ethyl acetate is placed in the distillation unit and the water is screened.

4. 분별증류 및 여과4. Fractionation and Filtration

농축액 혼합액에서 에틸아세테이트를 분별증류(Fractional Distillation)하여 제거한 다음, 400mesh 필터로 여과하여 도 2a에 나타난 천연 방부제 원액을 얻는다.Ethyl acetate was removed by fractional distillation in the concentrated liquid mixture, and then filtered through a 400 mesh filter to obtain a stock solution of the natural preservative shown in FIG.

그리고 천연 방부제 원액을 희석하여 도 2b에 나타난 천연 방부제 제조를 완료한다.And then diluting the stock solution of the natural preservative to complete the production of the natural preservative shown in FIG. 2B.

도 3a 내지 도 3d는 위 실시예 1의 천연 방부제에 대하여 항균 시험을 한 결과를 나타낸 시험데이터로서, 이를 살펴보면 황색포도산구균, 대장균, 살모넬라균, 흑곰팡이균 4가지의 균에 대하여 모두 99.0%의 감소율을 나타냈는데 이러한 결과는 은 또는 만다린 추출 성분 단독으로 사용한 경우 95.0~98.1%의 감소율을 나타낸 것에 비해 현저히 향상된 항균 효과를 가진다는 것을 확인할 수 있었다.FIG. 3A to FIG. 3D are test data showing the results of antibacterial test on the natural preservative of Example 1, wherein all of the bacteria of Staphylococcus aureus, Escherichia coli, Salmonella and Black fungus were 99.0% . These results showed that the antimicrobial effect was remarkably improved as compared with the reduction rate of 95.0 ~ 98.1% when silver or mandarin extract was used alone.

한편, 본 발명의 상세한 설명에서는 구체적인 실시예에 관해 설명하였으나, 본 발명은 개시된 실시예에 한정되지 않고 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 있어 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 여러 가지 치환, 변형 및 변경이 가능하다. 따라서, 본 발명의 범위는 설명된 실시예에 국한되어 정해져서는 안되며 후술하는 특허청구범위뿐만 아니라 이 특허청구범위와 균등한 것들을 포함하는 것으로 해석되어야 할 것이다.While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, Various permutations, modifications and variations are possible. Accordingly, the scope of the present invention should be construed as being limited to the embodiments described, and it is intended that the scope of the present invention encompasses not only the following claims, but also equivalents thereto.

Claims (4)

적어도 백금과 은 성분이 함유된 천연 암반수를 농축한 천연 암반수 농축액을 마련하는 단계와;
나린제린, 비타민C, 폴리페놀 중 적어도 하나의 성분이 함유된 만다린 농축액을 마련하는 단계와;
용매에 상기 천연 암반수 농축액과, 만다린 농축액와, 수소화붕소나트륨을 투입한 농축액 혼합액을 마련한 다음, 상기 농축액 혼합액에 함유된 수분을 분리하여 제거하는 단계와;
상기 농축액 혼합액에 들어있는 수분이 제거된 농축액 혼합액에서 에틸아세테이트를 제거하여 얻은 추출물에 용매를 혼합하여 희석하는 단계;를 포함하고,
상기 천연 암반수 농축액은 천연 암반수를 40~50℃, 0.1~1 Torr의 진공 상태에서 20~30시간 동안 진공 건조하여 얻어지며,
상기 만다린 농축액은 세척한 만다린 껍질을 1차 분쇄하는 단계와; 상기 1차 분쇄된 만다린 분쇄물을 1차 교반 숙성하는 단계와; 상기 1차 교반 숙성된 분쇄물을 2차 분쇄하는 단계와; 상기 2차 분쇄된 만다린 분쇄물 100중량부를 기준으로 물 20~40중량부와, 에틸아세테이트 80~120중량부를 혼합한 만다린 혼합물을 마련하는 단계와; 상기 만다린 혼합물을 2차 교반 숙성하는 단계와; 상기 2차 교반 숙성된 만다린 혼합물에서 물과 에틸아세테이트를 제거하여 추출물을 얻는 단계와; 상기 추출물에 물 80~120중량부와, 수용성 성분 0.001~0.1중량부를 혼합한 혼합액을 마련하는 단계와; 상기 혼합액을 농축시키는 단계;를 통해 얻어지며,
상기 천연 암반수 농축액에 함유된 은 성분은 은 카르보닐([Ag(CO)3]2)에 상기 나린제린, 비타민C, 폴리페놀의 카르보닐기가 결합하여 착화합물을 형성하고,
상기 백금은 상기 착화합물의 배위 결합시 촉매로 작용하며, 상기 수소화붕소나트륨은 환원제로 작용하는 것을 특징으로 하는 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법.
Providing a natural mineral water concentrate obtained by concentrating natural minerals containing at least platinum and silver components;
Preparing a mandarin concentrate containing at least one of naringenin, vitamin C, and polyphenol;
Separating and removing water contained in the concentrate mixture solution after preparing a mixture of the natural mineral water concentrate, mandarin concentrate and sodium borohydride in a solvent;
And removing the ethyl acetate from the concentrated liquid mixture removed in the concentrated liquid mixture to dilute the extract obtained by mixing the extract with a solvent,
The natural mineral water concentrate is obtained by vacuum drying natural mineral waters under a vacuum of from 40 to 50 DEG C and from 0.1 to 1 Torr for 20 to 30 hours,
Wherein the mandarin concentrate is obtained by firstly pulverizing the washed mandarin shell; Aging the primary pulverized mandarin crushed material with primary agitation; Secondly pulverizing the primary aged aged pulverized product; Preparing mandarin mixture in which 20 to 40 parts by weight of water and 80 to 120 parts by weight of ethyl acetate are mixed based on 100 parts by weight of the secondary pulverized mandarin crushed product; Aging the mandarin mixture with secondary agitation; Removing water and ethyl acetate from the secondary agitation-aged mandarin mixture to obtain an extract; Preparing a mixed solution comprising 80 to 120 parts by weight of water and 0.001 to 0.1 part by weight of a water-soluble component; And concentrating the mixed solution,
The silver component contained in the natural mineral water concentrate is a compound in which the carbonyl group of naringin, vitamin C and polyphenol binds to silver carbonyl ([Ag (CO) 3 ] 2 ) to form a complex,
Wherein the platinum acts as a catalyst in the coordination bond of the complex and sodium borohydride acts as a reducing agent.
삭제delete 제1항에 있어서,
상기 농축액 혼합액은 용매로서 에틸아세테이트 100중량부를 기준으로 상기 천연 암반수 농축액 1~50중량부와, 상기 만다린 농축액 1~50중량부와, 상기 수소화붕소나트륨 0.01~1중량부로 이루어지는 것을 특징으로 하는 천연 암반수와 만다린 농축액을 이용한 천연 방부제 제조방법.


The method according to claim 1,
Wherein the concentrate mixture is composed of 1 to 50 parts by weight of the natural mineral water concentrate, 1 to 50 parts by weight of the mandarin concentrate, and 0.01 to 1 part by weight of sodium borohydride as a solvent, based on 100 parts by weight of ethyl acetate. And a method for producing a natural preservative using mandarin concentrate.


삭제delete
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005169387A (en) * 2003-11-20 2005-06-30 Nobuaki Ando Apparatus for producing organic mineral water, method therefor, and organic mineral water
JP2008063295A (en) * 2006-09-08 2008-03-21 Dhc Co Skin care preparation containing platinum/silver colloid
KR101612936B1 (en) * 2016-01-21 2016-04-15 주식회사 케이앤피나노 The natural preservative manufacturing method of using Mandarin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005169387A (en) * 2003-11-20 2005-06-30 Nobuaki Ando Apparatus for producing organic mineral water, method therefor, and organic mineral water
JP2008063295A (en) * 2006-09-08 2008-03-21 Dhc Co Skin care preparation containing platinum/silver colloid
KR101612936B1 (en) * 2016-01-21 2016-04-15 주식회사 케이앤피나노 The natural preservative manufacturing method of using Mandarin

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