KR102620287B1 - The antioxident extracted from pine tree core and method thereof - Google Patents

The antioxident extracted from pine tree core and method thereof Download PDF

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KR102620287B1
KR102620287B1 KR1020200188894A KR20200188894A KR102620287B1 KR 102620287 B1 KR102620287 B1 KR 102620287B1 KR 1020200188894 A KR1020200188894 A KR 1020200188894A KR 20200188894 A KR20200188894 A KR 20200188894A KR 102620287 B1 KR102620287 B1 KR 102620287B1
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pine
core material
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김남희
최훈석
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주식회사 대산
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    • A—HUMAN NECESSITIES
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    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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    • A—HUMAN NECESSITIES
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Abstract

본 발명은 소나무 심재를 포함하는 항산화제에 관한 것으로, 직경 45cm 이상의 소나무를 선별하는 소나무 선별단계; 선별된 소나무의 함수율을 11 내지 19%로 건조시키는 건조단계; 건조된 소나무의 외피와 변재를 제거하여, 섬유질심재 및 친유성심재로 구성된 심재를 분리하는 분리단계; 심재 중 섬유질심재를 제거하여 친유성심재를 추출하는 친유성심재 추출단계; 추출된 친유성심재와 증류수를 혼합하고, 열수추출법으로 1차 증류추출액을 추출하는 1차 증류추출단계; 1차 증류추출액에서 오일성분 및 불순물을 분리하고 35 내지 40℃에서 감압 농축하여 1차시료를 획득하는 1차 여과 및 농축단계; 및 1차시료를 회수하는 1차시료 회수단계를 포함하는 것을 특징으로 한다.The present invention relates to an antioxidant containing pine heartwood, comprising the steps of selecting pine trees with a diameter of 45 cm or more; A drying step of drying the selected pine trees to a moisture content of 11 to 19%; A separation step of removing the outer skin and sapwood of dried pine trees and separating the heartwood consisting of fibrous heartwood and oleophilic heartwood; A lipophilic core material extraction step of extracting the lipophilic core material by removing the fibrous core material from the core material; A first distillation extraction step of mixing the extracted lipophilic core material with distilled water and extracting the first distillation extract by hot water extraction; A primary filtration and concentration step of separating oil components and impurities from the primary distillation extract and concentrating under reduced pressure at 35 to 40°C to obtain a primary sample; and a primary sample recovery step of recovering the primary sample.

Description

소나무 심재로부터 추출된 항산화제 및 이를 추출하는 방법 {THE ANTIOXIDENT EXTRACTED FROM PINE TREE CORE AND METHOD THEREOF}Antioxidants extracted from pine heartwood and method of extracting them {THE ANTIOXIDENT EXTRACTED FROM PINE TREE CORE AND METHOD THEREOF}

본 발명은 항산화 효과가 뛰어날 뿐만 아니라 유해물질의 생성을 저감할 수 있는 소나무 심재가 포함된 항산화제 및 이를 추출하는 방법에 관한 것이다.The present invention relates to an antioxidant containing pine heartwood that not only has excellent antioxidant effects but can also reduce the production of harmful substances, and a method for extracting the same.

현재 시대는 낮은 출산율과 평균 생존나이가 높아지고 있어 고령화 인구가 늘어나고 있다. 이러한 사회 현상에 기인하여 개인의 건강이나 수명과 관련된 각종 기능성 건강식품 시장이 커지고 있다. 한국건강기능식품협회의 통계자료에 따르면 해외 건강 기능성 식품 시장은 1,289억 달러로 최근 7년간 연평균 7.2%로 성장하였고, 국내 건강 기능성 식품 시장규모는 2018년 기준 4조 3000억원으로 2016년보다 약 20% 가량 성장한 것으로 집계되었다. In the current era, the aging population is increasing due to low birth rates and increasing average survival age. Due to this social phenomenon, the market for various functional health foods related to individual health and lifespan is growing. According to statistical data from the Korea Health Functional Foods Association, the overseas health functional food market is worth 128.9 billion dollars, growing at an average annual rate of 7.2% over the past 7 years, and the domestic health functional food market size is 4.3 trillion won as of 2018, about 20 trillion won compared to 2016. It was calculated that there was a growth of about %.

이러한 기능성 건강식품 중 가장 두각을 나타내는 것이 천연 항산화물질이 포함된 항산화제품이다. 항산화제품이란 신체의 활성산소를 제거하여 산화적 스트레스로부터 인체를 방어하도록 돕는 물질로, 주로 비타민 A, 비타민 E. 비타민 C 등과 같은 폴리페놀류 물질과 그 외 다양한 물질이 항산화 작용을 하는 것으로 알려져 있다. 상기한 활성산소가 신체에서 설정값 이상으로 생성되면 염증이 생기거나 변형된 단백질이 생겨 축적될 수 있을 뿐 아니라, 활성산소의 생성속도의 균형이 깨지면 산화적 스트레스가 발생하여 신체 노화가 이르게 오는 등 좋지않은 영향을 끼친다. 이러한 활성산소를 제거하기 위해 신체의 항산화시스템이 작동할 수 있는데 항산화 제품은 이러한 항산화시스템이 효율적으로 일어날 수 있도록 하는 효과가 있다. Among these functional health foods, the most prominent ones are antioxidant products containing natural antioxidants. Antioxidant products are substances that help defend the human body from oxidative stress by removing free radicals from the body. Mainly polyphenols such as vitamin A, vitamin E, and vitamin C, as well as various other substances are known to have antioxidant properties. If the above-mentioned free radicals are generated in the body beyond the set value, inflammation may occur or modified proteins may form and accumulate, and if the balance of the production rate of free radicals is broken, oxidative stress may occur, leading to premature aging of the body. It has a bad effect. The body's antioxidant system can operate to remove these free radicals, and antioxidant products have the effect of allowing this antioxidant system to occur efficiently.

실제로 항산화제 글로벌 시장규모는 2022년 약 41억 4,000만 달러, 우리돈으로 약 4.5조원에 달할 것으로 예측되고 있다. 특히, 항산화제 물질 중 천연재료에서 유래된 항산화제가 시장규모를 크게 늘릴 것으로 예측되고 있으며, 이러한 항산화제는 식품등에 주로 사용될 수 있을 것으로 판단되고 있다. In fact, the global market size for antioxidants is predicted to reach approximately $4.14 billion, or approximately 4.5 trillion won in Korean currency, by 2022. In particular, among antioxidant substances, antioxidants derived from natural ingredients are expected to significantly increase the market size, and these antioxidants are expected to be mainly used in foods.

그러나 대부분의 항산화제 물질은 영양제나 건강식품, 즉 약형태로 제조되기 때문에 기존 식품에 첨가하거나 할 수 없을 뿐 아니라, 천연에서 유래되지 않고 자체가공을 통해 비타민 등을 뽑아내어 제조하기 때문에 섭취 과정에서 부작용이 발생할 수 있는 문제가 있다. However, since most antioxidant substances are manufactured in the form of nutritional supplements or health foods, that is, medicines, they cannot be added to existing foods. Moreover, since they are not derived from nature and are manufactured by extracting vitamins, etc. through self-processing, they cannot be consumed during the intake process. There is a problem that side effects may occur.

이와 별개로, 소나무는 우리나라를 대표하는 나무로 전국 산야에서 자라고 있어 쉽게 볼 수 있는 상록 침엽수이다. 일반적으로 이러한 소나무의 목재나 심재는 집을 짓거라 땔감으로 쓰였고, 이외 꽃가루나 솔입, 송기, 솔방울 등은 식용이나 음료제조용으로 많이 사용되었다. 특히 소나무의 껍질이나 소나무잎에는 항산화물질이 고농도로 함유되어 있어, 항산화제 제조를 위해 소나무 껍질이나 소나무잎이 다방면에서 활용되고 있는 실정이다. Separately from this, the pine tree is the representative tree of Korea and is an evergreen coniferous tree that grows in mountains and fields across the country and can be easily seen. In general, the wood and heartwood of these pine trees were used as firewood to build houses, and pollen, pine needles, pine needles, and pine cones were widely used for eating or making beverages. In particular, pine bark and pine leaves contain high concentrations of antioxidants, and pine bark and pine leaves are being used in many ways to manufacture antioxidants.

제10-2010-0082800호 (발명의 명칭 : 소나무로부터 항균활성 및 항산화 활성을 가진 물질을 생산하는 방법)No. 10-2010-0082800 (Title of invention: Method for producing substances with antibacterial and antioxidant activities from pine trees) 그러나 소나무 잎뿐만 아니라 소나무 심재에서 일반적으로 항산화제를 생성하기 힘들 뿐 아니라. 생성된 항산화제 추출효율 역시 낮은 문제가 있어, 이를 해결하기 위한 방안에 대한 필요성이 대두되고 있는 상황이다.However, it is generally difficult to produce antioxidants not only in pine leaves but also in pine heartwood. There is also a problem of low extraction efficiency of the produced antioxidants, and the need for a method to solve this problem is emerging.

본 발명은 상술한 문제점을 해결하기 위하여 안출된 것으로, 본 발명의 목적은 항산화 효능이 높은 소나무 심재가 포함된 항산화 추출물을 제공하는데 있다. 다만, 상기된 바와 같은 기술적 과제로 한정되지 않으며 이하의 설명으로부터 또 다른 기술적 과제가 도출될 수도 있다.The present invention was developed to solve the above-mentioned problems, and the purpose of the present invention is to provide an antioxidant extract containing pine heartwood with high antioxidant efficacy. However, it is not limited to the technical challenges described above, and other technical challenges may be derived from the description below.

본 발명의 일 실시예에 따른 소나무 심재가 포함된 항산화제 추출방법은, 직경 45cm 이상의 소나무를 선별하는 소나무 선별단계; 선별된 소나무의 함수율을 11 내지 19%로 건조시키는 건조단계; 건조된 소나무의 외피와 변재를 제거하여, 섬유질심재 및 친유성심재로 구성된 심재를 분리하는 분리단계; 상기 심재 중 섬유질심재를 제거하여 친유성심재를 추출하는 친유성심재 추출단계; 추출된 상기 친유성심재와 증류수를 혼합하고, 열수추출법으로 1차 증류추출액을 추출하는 1차 증류추출단계; 상기 1차 증류추출액에서 오일성분 및 불순물을 분리하고 35 내지 40℃에서 감압 농축하여 1차시료를 획득하는 1차 여과 및 농축단계; 및 상기 1차시료를 회수하는 1차시료 회수단계를 포함하는 것을 특징으로 한다.An antioxidant extraction method containing pine heartwood according to an embodiment of the present invention includes a pine tree selection step of selecting pine trees with a diameter of 45 cm or more; A drying step of drying the selected pine trees to a moisture content of 11 to 19%; A separation step of removing the outer skin and sapwood of dried pine trees and separating the heartwood consisting of fibrous heartwood and oleophilic heartwood; A lipophilic core material extraction step of extracting the lipophilic core material by removing the fibrous core material among the core materials; A first distillation extraction step of mixing the extracted lipophilic core material with distilled water and extracting the first distillation extract by hot water extraction; A primary filtration and concentration step of separating oil components and impurities from the primary distillation extract and concentrating under reduced pressure at 35 to 40° C. to obtain a primary sample; and a primary sample recovery step of recovering the primary sample.

또한, 상기 열수추출법은 상기 친유성심재 100중량% 대비 상기 증류수 200 내지 5,000 중량%로 혼합하고, 95 내지 100 ℃에서 0.5 내지 8시간동안 증류처리한 것을 특징으로 한다.In addition, the hot water extraction method is characterized in that 200 to 5,000% by weight of the distilled water is mixed with 100% by weight of the lipophilic core material and distilled at 95 to 100 ° C. for 0.5 to 8 hours.

또한, 상기 친유성심재에서 상기 1차 증류추출액이 추출된 잔여심재와 에탄올을 혼합하고, 용매추출법으로 2차 증류추출액을 추출하는 2차 증류추출단계; 상기 2차 증류추출액에서 불순물을 분리하고 35 내지 40℃에서 감압 농축하여 2차시료를 획득하는 2차 여과 및 농축단계; 및 상기 2차시료를 회수하는 2차시료 회수단계를 더 포함하는 것을 특징으로 한다.In addition, a second distillation extraction step of mixing the remaining heartwood from which the first distillation extract was extracted from the lipophilic heartwood with ethanol and extracting the second distillation extract by solvent extraction; A secondary filtration and concentration step of separating impurities from the secondary distillation extract and concentrating under reduced pressure at 35 to 40° C. to obtain a secondary sample; and a secondary sample recovery step of recovering the secondary sample.

또한, 상기 용매추출법은 상기 친유성심재 100중량% 대비 상기 증류수 200 내지 5,000 중량%로 혼합하고, 75 내지 80 ℃에서 0.5 내지 8시간동안 증류처리한 것을 특징으로 한다.In addition, the solvent extraction method is characterized in that 200 to 5,000% by weight of the distilled water is mixed with 100% by weight of the lipophilic core material and distilled at 75 to 80 ° C. for 0.5 to 8 hours.

본 발명의 다른 실시예에 따른 항산화제는, 상기한 항산화제 추출방법 중 하나의 방법으로 추출된 것을 특징으로 한다.The antioxidant according to another embodiment of the present invention is characterized in that it is extracted by one of the antioxidant extraction methods described above.

본 발명에 따른 소나무 심재가 포함된 항산화제 및 이의 추출방법은 아래와 같은 효과가 있다. The antioxidant containing pine heartwood and its extraction method according to the present invention have the following effects.

우선, 직경 45cm 미만인 소나무 심재(이하, 비교예)를 활용한 항산화제 추출수율보다 본 발명의 실시예에 따른 소나무 친유성심재를 활용한 항산화제의 추출수율이 월등하게 뛰어난 효과가 있다. 특히, 친유성심재의 1차시료 추출수율은 일반심재의 1차시료 추출수율에 비해 약 4배 이상, 친유성심재의 2차시료 추출수율은 일반심재의 2차시료 추출수율에 비해 약 8배 이상 뛰어난 효과가 있다. First, the extraction yield of antioxidants using lipophilic pine heartwood according to an embodiment of the present invention is significantly superior to the extraction yield of antioxidants using pine heartwood with a diameter of less than 45 cm (hereinafter, comparative example). In particular, the primary sample extraction yield of lipophilic core material is approximately 4 times higher than that of general core material, and the secondary sample extraction yield of lipophilic core material is approximately 8 times higher than that of general core material. It has excellent effects.

이 중에서도, 친유성심재의 2차시료는 친유성심재 40g 중 8.26g이 추출되어 추출수율 21.15%로 매우 높은 추출수율임을 확인할 수 있다. 즉, 친유성심재에서 추출되는 1차시료 및 2차시료의 양이 비교예의 결과에 비해 월등하게 높기 때문에, 항산화제 추출단가가 낮아지고 이에 따라 사업운영 측면에서 사업성 및 경제성이 높아지는 효과가 있다. Among these, the secondary sample of the lipophilic core material was confirmed to have a very high extraction yield of 21.15%, with 8.26 g extracted out of 40 g of the lipophilic core material. In other words, since the amount of primary and secondary samples extracted from the lipophilic core material is much higher than the results of the comparative example, the unit cost of extracting antioxidants is lowered, which has the effect of increasing business feasibility and economic feasibility in terms of business operation.

또한, 친유성심재를 활용한 항산화제의 항산화도는 직경 45cm 미만인 소나무 심재를 활용한 항산화제의 항산화도에 비해 높은 효과가 있다. 특히, 친유성심재의 1차시료는 타 시료에 비해서 월등하게 항산화도가 높을 뿐 아니라, 친유성심재의 2차시료 역시 추출수율이 높음과 동시에 그 항산화도가 비교예에서 추출되는 1차시료와 큰 차이가 없음을 확인할 수 있다. 즉, 높은 추출수율로 항산화제를 추출할 수 있을 뿐 아니라 열수추출과 용매추출을 통해 추출된 모든 항산화제의 항산화도가 높게 나타나는 효과가 있다.In addition, the antioxidant degree of antioxidants using lipophilic heartwood is more effective than that of antioxidants using pine heartwood with a diameter of less than 45 cm. In particular, not only does the primary sample of the lipophilic core material have a significantly higher antioxidant level than other samples, but the secondary sample of the lipophilic core material also has a high extraction yield and its antioxidant degree is comparable to that of the primary sample extracted in the comparative example. You can see that there is no significant difference. In other words, not only can antioxidants be extracted with high extraction yield, but the antioxidant degree of all antioxidants extracted through hot water extraction and solvent extraction is high.

도 1은 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제를 추출하는 단계를 도시한 플로우차트.
도 2는 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제에 사용되는 소나무와 일반적인 비교예의 소나무의 단면을 비교한 사진.
도 3은 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제와 일반적인 비교예의 소나무 심재가 포함된 항산화제의 성분분석 결과를 도시한 그래프
도 4는 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제에서 검출된 성분분석 결과를 도시한 그래프.
도 5는 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제와 일반적인 비교예의 소나무 심재가 포함된 항산화제의 라디칼 소거능 측정결과를 도시한 그래프.Figure 1 is a flow chart showing the steps of extracting antioxidants containing pine heartwood according to an embodiment of the present invention.
Figure 2 is a photograph comparing the cross sections of pine trees used in antioxidants containing pine heartwood according to an embodiment of the present invention and pine trees of a general comparative example.
Figure 3 is a graph showing the results of component analysis of an antioxidant containing pine heartwood according to an embodiment of the present invention and an antioxidant containing pine heartwood of a general comparative example
Figure 4 is a graph showing the results of component analysis detected in antioxidants containing pine heartwood according to an embodiment of the present invention.
Figure 5 is a graph showing the results of measuring the radical scavenging ability of an antioxidant containing pine heartwood according to an embodiment of the present invention and an antioxidant containing pine heartwood of a general comparative example.

이하에서는 첨부된 도면을 참조하여 본 발명의 실시예들을 상세히 설명한다. 이하에서 설명되는 실시예들은 항산화능력이 뛰어날 뿐만 아니라 추출효율 역시 높은 소나무 심재가 포함된 항산화제 및 이의 추출방법에 관한 것이다. Hereinafter, embodiments of the present invention will be described in detail with reference to the attached drawings. The examples described below relate to an antioxidant containing pine heartwood that not only has excellent antioxidant ability but also has a high extraction efficiency, and a method for extracting the same.

다음에 소개되는 실시예 및 도면들은 당업자에게 본 발명의 사상이 충분히 전달될 수 있도록 하기 위해 예로서 제공되는 것이다. 또한, 본 발명의 사용되는 기술 용어 및 과학 용어에 있어서 다른 정의가 없다면, 이 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 통상적으로 이해하고 있는 의미를 가지며, 하기의 설명 및 첨부 도면에서 본 발명의 요지를 불필요하게 흐릴 수 있는 공지 기능 및 구성에 대한 설명은 생략한다.The embodiments and drawings introduced below are provided as examples so that the idea of the present invention can be sufficiently conveyed to those skilled in the art. In addition, if there is no other definition in the technical and scientific terms used in the present invention, they have the meaning commonly understood by those skilled in the art to which this invention pertains, and the present invention is described in the following description and accompanying drawings. Descriptions of known functions and configurations that may unnecessarily obscure the gist of are omitted.

이하, 본 발명의 기술적 사상을 첨부된 도면을 사용하여 더욱 구체적으로 설명한다. 첨부된 도면은 본 발명의 기술적 사상을 더욱 구체적으로 설명하기 위하여 도시한 일예에 불과하므로 본 발명의 기술적 사상이 첨부된 도면의 형태에 한정되는 것은 아니다.Hereinafter, the technical idea of the present invention will be described in more detail using the attached drawings. The attached drawings are merely examples to illustrate the technical idea of the present invention in more detail, so the technical idea of the present invention is not limited to the form of the attached drawings.

도 1은 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제를 추출하는 단계를 도시한 플로우차트이다. Figure 1 is a flow chart showing the steps for extracting antioxidants containing pine heartwood according to an embodiment of the present invention.

도 1을 참조하면, 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제를 추출하는 방법은, 원목선별단계(S110), 건조단계(S120), 심재분리단계(S130), 친유성심재 분리단계(S140), 1차 증류추출단계(S210), 1차 여과 및 농축단계(S220), 1차시료 회수단계(S230), 2차 증류추출단계(S310), 2차 여과 및 농축단계(S320) 및 2차시료 회수단계(S330)를 포함할 수 있다.Referring to Figure 1, the method for extracting antioxidants containing pine heartwood according to an embodiment of the present invention includes a log selection step (S110), a drying step (S120), a heartwood separation step (S130), and a lipophilic heartwood separation step. Step (S140), first distillation and extraction step (S210), first filtration and concentration step (S220), first sample recovery step (S230), second distillation extraction step (S310), second filtration and concentration step (S320) ) and a secondary sample recovery step (S330).

원목선별단계(S110)는 심재를 추출하기 위한 원목, 즉 소나무를 선별하는 단계이다. 이 단계에서는 흉고직경 45cm 이상의 소나무를 선별할 수 있다. 소나무 흉고직경이 45cm 미만인 경우, 내부의 심재에서 추출되는 폴리페놀 함량이나 항산화력 수준이 낮거나 외부로 추출되는 향이 설정기준 미만인 경우가 많고, 항산화력 수준이 낮아지기 때문에 직경 45cm 이상의 소나무를 선별해서 다음 단계를 진행할 수 있다. The log selection step (S110) is a step of selecting logs, that is, pine trees, to extract heartwood. At this stage, pine trees with a breast height diameter of 45 cm or more can be selected. If the pine tree's breast height diameter is less than 45cm, the polyphenol content or antioxidant power level extracted from the inner heartwood is often low, or the aroma extracted to the outside is often below the set standard, and the level of antioxidant power is lowered. Therefore, pine trees with a diameter of 45cm or more are selected and You can proceed with the steps.

다음 단계인 건조단계(S120)는, 선별된 소나무 원목을 건조하는 단계이다. 상세히, 선별된 소나무 원목을 벌목한 후, 해당 원목의 함수율이 25% 이하, 바람직하게는 11 내지 19% 사이의 값이 될 때까지 원목을 건조시킬 수 있는 단계이다. 이러한 원목의 건조를 위한 건조방법은 주로 자연건조를 활용할 수 있고, 온도는 -10 내지 40℃, 습도 45 내지 85%의 환경에서 17,520시간 이상, 대략적으로 2년 이상의 시간동안 건조를 수행할 수 있다. The next step, the drying step (S120), is the step of drying the selected pine logs. In detail, this is a step in which, after felling the selected pine logs, the logs are dried until the moisture content of the logs reaches a value of 25% or less, preferably between 11 and 19%. The drying method for drying such logs can mainly use natural drying, and drying can be performed for more than 17,520 hours, approximately 2 years or more, in an environment with a temperature of -10 to 40 ℃ and a humidity of 45 to 85%. .

이에 따라, 소나무 원목의 함수율이 11 내지 19% 이하로 건조될 수 있고, 이러한 소나무 원목의 경우, 나무 망치로 원목에 타격을 가하면 내부에 수분이 응축되어 맑은 종소리가 날 수 있고, 이를 기준으로 함수율이 11 내지 19% 이하로 건조되었음을 확인할 수 있다. 다만, 이는 하나의 방법으로 습도측정기를 나무에 삽입시키고 습도측정설정시간만큼 대기함에 따라 나무 내부의 함수율을 측정할 수 있다.Accordingly, the moisture content of pine logs can be dried to 11 to 19% or less, and in the case of such pine logs, when the log is struck with a wooden hammer, moisture is condensed inside and a clear bell sound can be made, and based on this, the moisture content is It can be confirmed that it has dried to less than 11 to 19%. However, this is a method that allows you to measure the moisture content inside the tree by inserting a humidity meter into the tree and waiting for the humidity measurement set time.

도 2는 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제에 사용되는 소나무와 일반 소나무의 단면을 비교한 사진이다. 도 2를 참조하면, 상기 선별단계 및 건조단계를 통해 건조된 소나무 원목의 단면과 선별단계 및 건조단계를 거치지 않은 일반 소나무 원목의 단면을 확인할 수 있다. 육안으로도 선별단계 및 건조단계를 거친 소나무 원목의 심재가 일반 소나무 원목의 심재에 비해 훨씬 두꺼울 뿐만 아니라 색깔이 짙음을 확인할 수 있다. 심재에 함유된 항산화물질이 많을수록 심재의 색깔이 짙어지는 특징이 있기 때문에, 선별단계 및 건조단계를 통해 심재에 함유된 항산화물질 함량이 일반 소나무 심재에 비해 높음을 확인할 수 있다.Figure 2 is a photograph comparing the cross sections of pine trees and regular pine trees used in antioxidants containing pine heartwood according to an embodiment of the present invention. Referring to Figure 2, the cross section of pine logs dried through the selection and drying steps and the cross section of regular pine logs that have not been subjected to the selection and drying steps can be seen. Even with the naked eye, you can see that the heartwood of pine logs that have gone through the selection and drying stages is not only much thicker but also darker in color than the heartwood of regular pine logs. Since the more antioxidants contained in the heartwood, the darker the color of the heartwood, it can be confirmed through the selection and drying steps that the content of antioxidants contained in the heartwood is higher than that of regular pine heartwood.

심재분리단계(S130)는, 건조단계에서 건조된 소나무 원목의 외피와 변재를 제거하여 심재를 분리하는 단계이다. 상세히, 소나무 원목은 내부 중심에 형성된 심재, 심재 주위를 둘러싸는 변재, 그리고 변재를 둘러싸고 외관을 형성하는 외피로 구분될 수 있는데, 이러한 원목에서 외피 및 변재를 제거하는 단계일 수 있다. 이는 원목의 구성 중 심재에 대부분의 항산화 물질 및 폴리페놀이 함유되어 있기 때문에 이러한 부분만 별도로 분리함으로써, 활성산소 제거를 위한 항산화 효과를 극대화시키기 위한 필요부위를 분리해내는 것으로 이해될 수 있다. The heartwood separation step (S130) is a step of separating the heartwood by removing the outer skin and sapwood of the dried pine logs in the drying step. In detail, pine logs can be divided into heartwood formed in the inner center, sapwood surrounding the heartwood, and outer skin surrounding the sapwood and forming the exterior. This may be a step in which the outer skin and sapwood are removed from these logs. This can be understood as separating only these parts to separate the necessary parts to maximize the antioxidant effect for removing free radicals, since the heartwood of the log contains most of the antioxidant substances and polyphenols.

친유성심재 추출단계(S140)는 심재에서 폴리페놀 함량 및 발향성분이 포함된 친유성 심재와, 리그닌 등이 침착된 섬유질 심재를 분리하여 친유성 심재를 획득하는 단계이다. 심재 중에서도 내부에 발향성분과 폴리페놀 함량이 높은 친유성 심재가 본 발명의 효과를 구성하기 위한 특징적인 부분이고, 섬유질 심재의 경우 단순 섬유질인 리그닌 함량이 높아 항산화 능력이 크게 떨어지기 때문이다.The lipophilic heartwood extraction step (S140) is a step of obtaining lipophilic heartwood by separating the lipophilic heartwood containing polyphenol content and aroma components from the heartwood and the fibrous heartwood on which lignin, etc. are deposited. Among the heartwood, lipophilic heartwood with a high content of aromatic components and polyphenols is a characteristic part of the effect of the present invention, and in the case of fibrous heartwood, the antioxidant ability is greatly reduced due to the high content of lignin, a simple fiber.

1차 증류추출단계(S210)는 추출된 친유성심재를 증류수를 활용하여 1차 증류추출액을 추출하는 단계이다. 상세히, 1차 증류추출단계에서는 열수추출법이 사용될 수 있고, 추출된 친유성심재에 증류수를 혼합하여 설정시간동안 설정온도에서 1차 증류추출액의 추출을 수행할 수 있다. 이 경우, 추출된 친유성심재 100 중량% 대비 증류수는 200 내지 5,000 중량%로 혼합될 수 있고, 증류처리는 95 내지 100℃의 온도조건에서 0.5 내지 8시간동안 증류처리될 수 있다. 후술할 실시예에서는 친유성심재 40g을 기준으로 1.5L의 증류수를 혼합하였으며, 온도조건 100℃에서 4.5시간동안 열수추출법을 수행하였다. The first distillation extraction step (S210) is a step of extracting the first distillation extract from the extracted lipophilic heartwood using distilled water. In detail, in the first distillation extraction step, a hot water extraction method can be used, and the extracted lipophilic core material can be mixed with distilled water to perform extraction of the first distillation extract at a set temperature for a set time. In this case, distilled water may be mixed at 200 to 5,000% by weight based on 100% by weight of the extracted lipophilic core material, and distillation treatment may be performed for 0.5 to 8 hours at a temperature of 95 to 100°C. In an example to be described later, 1.5 L of distilled water was mixed with 40 g of lipophilic core material, and hot water extraction was performed at a temperature of 100°C for 4.5 hours.

1차 여과 및 농축단계(S220)에서는 1차 증류추출단계에서 추출된 1차 증류추출액의 오일성분인 화수와 에센셜 오일을 분리하고 불순물을 여과하며, 여과된 1차 증류추출액을 농축하는 단계이다. 여기서 농축단계는 35 내지 40℃에서 감압을 활용하여 설정시간동안 압력을 설정범위만큼 낮추면서 농축을 수행하였으며 이를 통해 1차 증류추출액이 농축되어 1차시료가 획득될 수 있다.In the first filtration and concentration step (S220), the oil components of the first distillation extract extracted in the first distillation extraction step are separated from the essential oil and the impurities are filtered, and the filtered first distillation extract is concentrated. Here, the concentration step was performed by lowering the pressure to a set range for a set time using reduced pressure at 35 to 40°C. Through this, the primary distilled extract was concentrated and a primary sample could be obtained.

1차시료 회수단계(S230)는 획득된 1차시료를 회수하는 단계로 이는 단순 회수단계인 바, 이에 대한 중복설명은 생략한다. The first sample recovery step (S230) is a step of recovering the obtained first sample. Since this is a simple recovery step, redundant description thereof will be omitted.

2차 증류추출단계(S310)는 1차증류추출액이 추출되고 남은 친유성심재, 즉 잔여심재를 에탄올을 활용하여 2차 증류추출액을 추출하는 단계이다. 상세히, 2차 증류추출단계에서는 용매추출법이 사용될 수 있고, 1차증류추출액이 회수되고 남은 친유성심재에 에탄올을 혼합하고 설정시간동안 설정온도에서 2차 증류추출액의 추출을 수행할 수 있다. 이 경우, 추출된 친유성심재 100 중량% 대비 에탄올은 200 내지 5,000 중량%로 혼합될 수 있고, 증류처리는 75 내지 80℃의 온도조건에서 0.5 내지 8시간동안 증류처리될 수 있다. 후술할 실시예에서는 최초 친유성심재 40g에서 1차증류추출액이 제외된 친유섬심재, 즉 잔여친유성심재에 1.5L의 에탄올을 혼합하였으며, 온도조건 78.4℃에서 4.5시간동안 용매추출법을 수행하였다. The second distillation extraction step (S310) is a step in which the second distillation extract is extracted using ethanol from the lipophilic heartwood remaining after the first distillation extract is extracted, that is, the remaining heartwood. In detail, in the second distillation extraction step, a solvent extraction method may be used, and ethanol may be mixed with the lipophilic core material remaining after the first distillation extract is recovered, and extraction of the second distillation extract may be performed at a set temperature for a set time. In this case, ethanol may be mixed in an amount of 200 to 5,000% by weight based on 100% by weight of the extracted lipophilic core material, and distillation treatment may be performed for 0.5 to 8 hours at a temperature of 75 to 80°C. In an example to be described later, 1.5 L of ethanol was mixed with the lipophilic core material from which the primary distillation extract was excluded from 40 g of the initial lipophilic core material, that is, the remaining lipophilic core material, and solvent extraction was performed at a temperature of 78.4°C for 4.5 hours.

2차 여과 및 농축단계(S320)에서는 2차 증류추출단계에서 추출된 2차 증류추출액에서 불순물을 여과하고 여과된 2차 증류추출액을 농축하는 단계이다. 2차 여과 및 농축단계에서는 화수 및 에센셜 오일과 같은 오일성분의 분리는 수행하지 않는다. 또한, 여기서 농축단계는 35 내지 40℃에서 감압을 활용하여 설정시간동안 압력을 설정범위만큼 낮추면서 농축을 수행하였으며, 이를 통해 2차 증류추출액이 농축되어 2차시료가 획득될 수 있다. In the second filtration and concentration step (S320), impurities are filtered from the second distillation extract extracted in the second distillation extraction step and the filtered second distillation extract is concentrated. In the secondary filtration and concentration stage, separation of oil components such as fire water and essential oil is not performed. In addition, here, the concentration step was performed by lowering the pressure to a set range for a set time using reduced pressure at 35 to 40°C, and through this, the secondary distillation extract was concentrated and a secondary sample could be obtained.

2차시료 회수단계(S330)는 획득한 2차시료를 회수하는 단계로 이는 단순 회수단계인 바, 이에 대한 중복설명은 생략한다. The secondary sample recovery step (S330) is a step of recovering the obtained secondary sample. Since this is a simple recovery step, redundant description thereof will be omitted.

아래에서는 상기한 추출단계에 의해 추출된 1차시료 및 2차시료를 포함하는 항산화제에 대한 성분분석과 항산화 능력에 대한 비교실험데이터를 기술한다. 도 3은 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제와 직경 비교예의 소나무 심재가 포함된 항산화제의 성분분석 결과를 도시한 그래프이고, 도 4는 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제에서 검출된 성분분석 결과를 도시한 그래프이며, 도 5는 본 발명의 실시예에 따른 소나무 심재가 포함된 항산화제와 비교예의 소나무 심재가 포함된 항산화제의 라디칼 소거능 측정결과를 도시한 그래프이다.Below, the component analysis of antioxidants including the primary and secondary samples extracted through the above-mentioned extraction step and comparative experimental data on antioxidant ability are described. Figure 3 is a graph showing the results of component analysis of an antioxidant containing pine heartwood according to an embodiment of the present invention and an antioxidant containing pine heartwood of a diameter comparison example, and Figure 4 is a graph showing the results of component analysis of an antioxidant containing pine heartwood according to an embodiment of the present invention. It is a graph showing the results of component analysis detected in the antioxidant containing, and Figure 5 shows the radical scavenging activity measurement results of the antioxidant containing pine heartwood according to an example of the present invention and the antioxidant containing pine heartwood of the comparative example. This is the graph shown.

우선 본 발명의 실시예에 따른 소나무심재를 포함한 항산화제(이하, 실시예)와 비교예의 소나무 심재를 포함한 항산화제(이하, 비교예)를 제조하였다. 실시예와 비교예의 소나무심재는 모두 40g 정량으로 진행하였으며, 제조단계에서 1차 증류추출단계, 1차 여과 및 농축단계, 1차시료 회수단계, 2차 증류추출단계, 2차 여과 및 농축단계 및 2차시료 회수단계는 동일하게 진행하였다. First, an antioxidant containing pine heartwood according to an example of the present invention (hereinafter referred to as an example) and an antioxidant containing pine heartwood as a comparative example (hereinafter referred to as a comparative example) were prepared. The pine heartwood of the examples and comparative examples were all weighed at 40g, and in the manufacturing stage, the first distillation extraction step, the first filtration and concentration step, the first sample recovery step, the second distillation extraction step, the second filtration and concentration step, and The second sample recovery step was performed in the same manner.

1차 증류추출단계에서 열수추출에 사용된 증류수는 1.5L이고, 열수추출을 위한 온도조건과 시간조건은 각각 ℃와 4.5시간으로 설정하였다. 마찬가지로, 2차 증류추출단계에서 용매추출에 사용된 에탄올은 1.5L이고, 용매추출을 위한 온도조건과 시간조건은 각각 ℃와 4.5시간으로 설정하였다.In the first distillation extraction step, the distilled water used for hot water extraction was 1.5 L, and the temperature and time conditions for hot water extraction were set to ℃ and 4.5 hours, respectively. Likewise, the ethanol used for solvent extraction in the second distillation extraction step was 1.5 L, and the temperature and time conditions for solvent extraction were set to ℃ and 4.5 hours, respectively.

전체 시료는 총 4가지로 추출되었으며, 시료는 실시예 1차시료, 실시예 2차시료, 비교예 1차시료, 비교예 2차시료로 명명하여 설명한다. A total of four samples were extracted, and the samples are named and described as Example 1st Sample, Example 2nd Sample, Comparative Example 1st Sample, and Comparative Example 2nd Sample.

본 발명의 실시예에 따른 소나무 심재와 비교예 소나무 심재의 정보는 표 1과 같다. Information on the pine heartwood according to the examples of the present invention and the pine heartwood of the comparative example is shown in Table 1.

분류 classification 실시예 소나무Example pine tree 비교예 소나무Comparative example pine tree 흉고직경Diameter at breast height 75 cm75cm 35 cm35cm 추정수령Estimated receipt 70년 이상over 70 years 70년 이상over 70 years 건조기간drying period 3년 이상more than 3 years 1년 이상Over 1 year 함수율moisture content 15 ± 4 %15±4% 24 ± 3 %24±3%

실시예와 비교예의 비교 실험은 크게 (1) 생성된 항산화제(시료)의 추출수율 비교, (2) 생성된 항산화제의 성분 비교분석, (3) 생성된 항산화제의 래디컬 소거능 비교분석의 3가지로 수행하였으며 각 단계에 대해서 아래에서 자세히 설명한다. The comparative experiments between the Examples and Comparative Examples largely consisted of (1) comparison of the extraction yield of the produced antioxidants (samples), (2) comparative analysis of the components of the produced antioxidants, and (3) comparative analysis of the radical scavenging ability of the produced antioxidants. It was carried out in stages, and each step is explained in detail below.

(1) 추출수율 비교데이터 (1) Extraction yield comparison data

실시예와 비교예의 추출양과 추출수율은 아래 표 2와 같이 확인되었다. 실시예 1차시료의 추출수율은 11.24%로 비교예 1차시료의 추출수율인 2.64%보다 약 4배 이상 추출됨을 확인할 수 있었고, 특히 실시예 2차시료의 추출수율은 21.15%로 2차시료의 추출수율은 2.605%보다 약 8배 이상 추출됨을 확인할 수 있다. 즉, 실시예의 1차시료 및 2차시료 추출수율이 비교예에 비하여 월등하게 높음을 확인할 수 있고, 이는 동일한 무게의 소나무심재로부터 더 많은 양의 항산화제를 추출할 수 있음을 의미한다. The extraction amount and extraction yield of the examples and comparative examples were confirmed as shown in Table 2 below. The extraction yield of the first sample of the example was 11.24%, which was confirmed to be about 4 times more than the extraction yield of 2.64% of the first sample of the comparative example. In particular, the extraction yield of the second sample of the example was 21.15%. It can be seen that the extraction yield is about 8 times more than 2.605%. In other words, it can be confirmed that the extraction yield of the primary and secondary samples of the example is significantly higher than that of the comparative example, which means that a greater amount of antioxidants can be extracted from the same weight of pine heartwood.

종류type 추출 후 무게(g)Weight after extraction (g) 추출수율(%)Extraction yield (%) 실시예 1차시료Example 1st sample 4.49654.4965 11.2411.24 비교예 1차시료Comparative example 1st sample 1.05811.0581 2.642.64 실시예 2차시료Example 2nd sample 8.46108.4610 21.1521.15 비교예 2차시료Comparative example secondary sample 1.04201.0420 2.612.61

(2) 생산된 항산화제의 성분 비교분석 (2) Comparative analysis of ingredients of produced antioxidants

실시예와 비교예의 시료들에 대한 성분분석방법은 크로마토그래피(LC) 방법을 수행하였다. 분석기기는 Agilent Technologies 1200 series (G1322A Degasser, G1312A Bin pump, G1329A Autosampler, G1315B Detector)를 사용하였고, 분석용 컬럼은 Phenomenex Synergi Hydro-RP 로 4. 6㎛ × 150 mm × 4 ㎛을 사용하였고, 주입되는 시료의 양은 10 ㎕, 컬럼의 온도는 30℃로 실험조건을 수행하였으며, 이동 상 유속은 0.7mL/min, 검출기의 성분파장은 205nm, 254nm, 280nm, 330nm 으로 설정하여 실험을 수행하였다. The component analysis method for the samples of Examples and Comparative Examples was chromatography (LC). The analysis equipment used was Agilent Technologies 1200 series (G1322A Degasser, G1312A Bin pump, G1329A Autosampler, G1315B Detector), and the analysis column was Phenomenex Synergi Hydro-RP with a size of 4.6㎛ × 150 mm × 4 ㎛, and injection The experimental conditions were set to 10 ㎕ of sample and 30°C column temperature. The mobile phase flow rate was 0.7 mL/min, and the component wavelengths of the detector were set to 205 nm, 254 nm, 280 nm, and 330 nm.

또한, 기기분석 설정을 위해 컬럼에 2가지 용매로 acetonitrile(이하, ACN)과 trifluoroacetic acid(이하, TFA)를 주입하였고, ACN의 함량을 10% 수준에서 30분에 걸쳐서 100%까지 올려줬다가 35분까지 해당 함량을 유지하였다가 37분까지 10%로 내린 뒤 3분간 유지하여 40분까지 안정화시켰다. 이 단계에서 TFA는 ACN 대비 0.02% 함량으로 추가되었다. In addition, to set up the instrumental analysis, acetonitrile (hereinafter, ACN) and trifluoroacetic acid (hereinafter, TFA) were injected into the column as two solvents, and the content of ACN was increased from 10% to 100% over 30 minutes and then 35%. The content was maintained until the 37th minute, then lowered to 10%, maintained for 3 minutes, and stabilized until the 40th minute. At this stage, TFA was added at an amount of 0.02% compared to ACN.

도 3을 참조하면, 실시예의 1차시료와 2차시료에서 1번과 2번 파장의 픽이 확인되었음을 확인할 수 있고, 반대로 비교예의 1차시료와 2차시료에서는 어떠한 파장의 픽도 확인되지 않았음을 확인할 수 있다. Referring to FIG. 3, it can be seen that picks of wavelengths 1 and 2 were confirmed in the first and second samples of the example, and conversely, no picks of any wavelength were confirmed in the first and second samples of the comparative example. You can check the sound.

이후, 액상크로마토그래피-질량분석법(이하, LC-MS법)을 활용하여 1번과 2번 파장의 피크값에 대한 화학구조를 분석하였다. 도 4를 참조하면, 피크값 별 분석결과 검출된 화학구조를 확인할 수 있다. 1번 피크값의 화학구조는 pinosylvin으로 확인되었고, 2번 피크값의 화학구조는 pinosylvin methyl ether로 확인되어 실시예의 1차시료 및 2차시료, 즉 실시예의 항산화제에서는 pinosylvin 성분이 검출됨을 확인할 수 있다. Afterwards, the chemical structure of the peak values at wavelengths 1 and 2 was analyzed using liquid chromatography-mass spectrometry (hereinafter referred to as LC-MS method). Referring to Figure 4, the chemical structure detected as a result of analysis for each peak value can be confirmed. The chemical structure of peak value No. 1 was confirmed to be pinosylvin, and the chemical structure of peak value No. 2 was confirmed to be pinosylvin methyl ether, confirming that the pinosylvin component was detected in the first and second samples of the example, that is, the antioxidant of the example. there is.

즉, 실시예의 항산화제에서는 pinosylvin 성분이 검출된데 반하여 비교예의 소나무 심재를 활용한 항산화제에서는 pinosylvin 성분이 검출되지 않았음을 확인할 수 있다. That is, it can be confirmed that the pinosylvin component was detected in the antioxidant of the example, whereas the pinosylvin component was not detected in the antioxidant using pine heartwood of the comparative example.

(3) 생성된 항산화제의 래디컬 소거능 비교분석(3) Comparative analysis of the radical scavenging ability of the produced antioxidants

이후 실시예의 1차시료 및 2차시료를 포함하는 항산화제와 비교예의 1차시료 및 2차시료를 포함하는 항산화제에 대하여 DPPH radical 소거능 비교분석법을 수행하여 항산화도를 측정하였다. 항산화제의 농도별 측정된 항산화도는 아래 표 3과 도 5를 참조하면 확인할 수 있다. Thereafter, the DPPH radical scavenging ability comparative analysis method was performed on the antioxidants including the primary and secondary samples of the Example and the antioxidants including the primary and secondary samples of the Comparative Example to measure the antioxidant degree. The antioxidant degree measured by concentration of antioxidant can be confirmed by referring to Table 3 and Figure 5 below.

시료농도
(ppm)Sample concentration
(ppm) 항산화도 (%)Antioxidant degree (%) 실시예
1차시료Example
1st sample 실시예
2차시료Example
Secondary sample 비교예
1차시료Comparative example
1st sample 비교예
2차시료Comparative example
Secondary sample 1,0001,000 94.594.5 90.290.2 91.891.8 43.343.3 500500 91.291.2 70.070.0 84.984.9 30.830.8 250250 73.373.3 50.350.3 69.369.3 16.616.6 125125 53.653.6 37.437.4 50.150.1 14.714.7

표 3 및 도 5를 참조하면, 열수추출에 의해 추출된 실시예 1차시료의 항산화도는 비교예 1차시료의 항산화도에 비해 모든 시료농도에서 높은 것으로 측정되었으며, 마찬가지로 용매추출에 의해 추출된 실시예 2차시료의 항산화도 역시 비교예 2차시료의 항산화도에 비해 모든 구간에서 2배 이상으로 월등하게 높은 것으로 측정되었다. Referring to Table 3 and Figure 5, the antioxidant degree of the primary sample of Example extracted by hot water extraction was measured to be higher at all sample concentrations compared to the antioxidant degree of the primary sample of Comparative Example, and similarly, the antioxidant degree of the primary sample of Example extracted by hot water extraction was measured to be higher at all sample concentrations. The antioxidant level of the secondary sample of Example was also measured to be significantly higher than the antioxidant level of the secondary sample of Comparative Example, at least twice as high in all sections.

특히, 열수추출에 의해 추출된 실시예 1차시료는 모든 시료와 비교하여도 항산화도가 월등하게 높게 나왔을 뿐만 아니라, 용매추출에 의해 추출된 실시예 2차시료는 열수추출에 의해 추출된 비교예 1차시료와 비교하여도 항산화도가 유사한 수준으로 검출되었음을 확인할 수 있다. In particular, the first sample of Example extracted by hot water extraction not only showed a significantly higher antioxidant level compared to all samples, but the second sample of Example extracted by solvent extraction was compared to the comparative example extracted by hot water extraction. Even when compared to the primary sample, it can be confirmed that the antioxidant level was detected at a similar level.

상기의 단계에 따라 추출된 소나무 심재가 포함된 항산화제는 아래와 같은 효과가 있다. Antioxidants containing pine heartwood extracted according to the above steps have the following effects.

우선, 일반적인 소나무 심재를 활용한 항산화제 추출수율보다 본 발명의 실시예에 따른 소나무 친유성심재를 활용한 항산화제의 추출수율이 월등하게 뛰어난 효과가 있다. 특히, 친유성심재의 1차시료 추출수율은 약 4배 이상, 친유성심재의 2차시료 추출수율은 약 8배 이상 뛰어난 효과가 있다. First, the extraction yield of antioxidants using lipophilic pine heartwood according to an embodiment of the present invention is significantly superior to the extraction yield of antioxidants using general pine heartwood. In particular, the primary sample extraction yield of the lipophilic core material is about 4 times more effective, and the secondary sample extraction yield of the lipophilic core material is about 8 times more effective.

특히, 친유성심재의 2차시료는 친유성심재 40g 중 8.26g이 추출되어 추출수율 21.15%로 매우 높은 추출수율임을 확인할 수 있다. 이에 따라, 동일한 소나무심재에서 추출되는 1차시료 및 2차시료의 양이 월등하게 높음에 따라 항산화제 추출단가가 낮아지고 이에 따라 사업운영측면에서 사업성이 높아지는 효과가 있다. In particular, the secondary sample of the lipophilic core material was confirmed to have a very high extraction yield of 21.15%, with 8.26 g out of 40 g of the lipophilic core material being extracted. Accordingly, as the amount of primary and secondary samples extracted from the same pine heartwood is significantly higher, the unit cost of extracting antioxidants is lowered, which has the effect of increasing business feasibility in terms of business operation.

또한, 친유성심재를 활용한 항산화제의 항산화도는 일반적인 소나무 심재를 활용한 항산화제의 항산화도에 비해 높은 효과가 있다. 특히, 친유성심재의 1차시료는 타 시료에 비해서 월등하게 항산화도가 높을 뿐 아니라, 친유성심재의 2차시료 역시 추출수율이 높음과 동시에 그 항산화도가 비교예의 소나무에서 추출되는 1차시료와 큰 차이가 없음을 확인할 수 있다. 즉, 높은 추출수율로 항산화제를 추출할 수 있을 뿐 아니라 열수추출과 용매추출을 통해 추출된 모든 항산화제의 항산화도가 높게 나타나는 효과가 있다.In addition, the antioxidant level of antioxidants using lipophilic heartwood is more effective than the antioxidant level of antioxidants using general pine heartwood. In particular, not only does the primary sample of the lipophilic heartwood have a significantly higher antioxidant level than other samples, but the secondary sample of the lipophilic heartwood also has a high extraction yield, and at the same time, its antioxidant degree is higher than that of the primary sample extracted from the pine tree in the comparative example. It can be confirmed that there is no significant difference. In other words, not only can antioxidants be extracted with high extraction yield, but all antioxidants extracted through hot water extraction and solvent extraction have a high antioxidant level.

이제까지 본 발명에 대하여 바람직한 실시예들을 중심으로 살펴보았다. 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자는 본 발명이 본 발명의 본질적인 특성에서 벗어나지 않는 범위에서 변형된 형태로 구현될 수 있음을 이해할 수 있을 것이다. 그러므로 개시된 실시예들은 한정적인 관점이 아니라 설명적인 관점에서 고려되어야 한다. 본 발명의 범위는 전술한 설명이 아니라 특허청구범위에 나타나 있으며, 그와 동등한 범위 내에 있는 모든 차이점은 본 발명에 포함된 것으로 해석되어야 할 것이다.So far, the present invention has been looked at with a focus on preferred embodiments. A person skilled in the art to which the present invention pertains will understand that the present invention may be implemented in a modified form without departing from the essential characteristics of the present invention. Therefore, the disclosed embodiments should be considered from an illustrative rather than a restrictive perspective. The scope of the present invention is indicated in the claims rather than the foregoing description, and all differences within the equivalent scope should be construed as being included in the present invention.

Claims (5)

직경 45cm 이상의 소나무를 선별하는 소나무 선별단계;
선별된 소나무의 함수율을 11 내지 19%로 건조시키는 건조단계;
건조된 소나무의 외피와 변재를 제거하여, 섬유질심재 및 친유성심재로 구성된 심재를 분리하는 분리단계;
상기 심재 중 섬유질심재를 제거하여 친유성심재를 추출하는 친유성심재 추출단계;
추출된 상기 친유성심재와 증류수를 혼합하고, 열수추출법으로 1차 증류추출액을 추출하는 1차 증류추출단계;
상기 1차 증류추출액에서 오일성분 및 불순물을 분리하고, 상기 오일성분을 35 내지 40℃에서 감압 농축하여 1차시료를 획득하는 1차 여과 및 농축단계;
상기 1차시료를 회수하는 1차시료 회수단계;
상기 친유성심재에서 상기 1차 증류추출액이 추출된 잔여심재와 에탄올을 혼합하고, 용매추출법으로 2차 증류추출액을 추출하는 2차 증류추출단계;
상기 2차 증류추출액에서 불순물을 분리하고, 35 내지 40℃에서 감압 농축하여 2차시료를 획득하는 2차 여과 및 농축단계; 및
상기 2차시료를 회수하는 2차시료 회수단계를 더 포함하는 것을 특징으로 하는 소나무 심재로부터 항산화 성분을 추출하는 방법.
A pine tree selection step of selecting pine trees with a diameter of 45 cm or more;
A drying step of drying the selected pine trees to a moisture content of 11 to 19%;
A separation step of removing the outer bark and sapwood of dried pine trees and separating the heartwood consisting of fibrous heartwood and oleophilic heartwood;
A lipophilic core material extraction step of extracting the lipophilic core material by removing the fibrous core material among the core materials;
A first distillation extraction step of mixing the extracted lipophilic core material with distilled water and extracting the first distillation extract by hot water extraction;
A primary filtration and concentration step of separating oil components and impurities from the primary distillation extract and concentrating the oil components under reduced pressure at 35 to 40° C. to obtain a primary sample;
A primary sample recovery step of recovering the primary sample;
A second distillation extraction step of mixing the remaining heartwood from which the first distillation extract was extracted from the lipophilic heartwood with ethanol and extracting the second distillation extract by a solvent extraction method;
A secondary filtration and concentration step of separating impurities from the secondary distillation extract and concentrating under reduced pressure at 35 to 40° C. to obtain a secondary sample; and
A method for extracting antioxidant components from pine heartwood, further comprising a secondary sample recovery step of recovering the secondary sample.
 제 1 항에 있어서,
상기 열수추출법은 상기 친유성심재 100중량% 대비 상기 증류수 200 내지 5,000 중량%로 혼합하고, 95 내지 100 ℃에서 0.5 내지 8시간동안 증류처리한 것을 특징으로 하는 소나무 심재로부터 항산화 성분을 추출하는 방법
According to claim 1,
The hot water extraction method is a method of extracting antioxidant components from pine heartwood, characterized in that 200 to 5,000% by weight of the distilled water is mixed with 100% by weight of the lipophilic heartwood and distilled at 95 to 100 ° C. for 0.5 to 8 hours.
 삭제delete 제 1 항에 있어서,
상기 용매추출법은 상기 친유성심재 100중량% 대비 상기 에탄올 200 내지 5,000 중량%로 혼합하고, 75 내지 80 ℃에서 0.5 내지 8시간동안 증류처리한 것을 특징으로 하는 소나무 심재로부터 항산화 성분을 추출하는 방법.
According to claim 1,
The solvent extraction method is a method of extracting antioxidant components from pine heartwood, characterized in that 200 to 5,000% by weight of the ethanol is mixed with 100% by weight of the lipophilic heartwood and distilled at 75 to 80 ° C. for 0.5 to 8 hours.
 제 1 항, 제 2 항 또는 제 4 항 중 어느 하나의 항의 추출방법으로 추출된 것을 특징으로 하는 소나무 심재로부터 추출된 항산화 성분이 포함된 항산화제.


An antioxidant containing antioxidant components extracted from pine heartwood, characterized in that it is extracted by the extraction method according to any one of claims 1, 2, or 4.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100731613B1 (en) 2006-01-12 2007-06-22 코스맥스 주식회사 Whitening and anti-aging cosmetic composition comprising stem heartwood extract of morus bombycis koidz

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
NILSSON et al., Induction of discolored wood in Scots pine (Pinus sylvestris). Tree Physiology. 2002, Vol. 22, pp. 331-338 1부.*
Venugopal et al., Phenolic compounds in Scots pine heartwood: are kelo trees a unique woody substrate? Canadian Journal of Forest Research. 2016, Vol. 46, pp. 225-233*

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