KR20090038548A - Preparation mothod of pressed oil reduced benzopyrene using active carbon - Google Patents
Preparation mothod of pressed oil reduced benzopyrene using active carbon Download PDFInfo
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- KR20090038548A KR20090038548A KR1020070103889A KR20070103889A KR20090038548A KR 20090038548 A KR20090038548 A KR 20090038548A KR 1020070103889 A KR1020070103889 A KR 1020070103889A KR 20070103889 A KR20070103889 A KR 20070103889A KR 20090038548 A KR20090038548 A KR 20090038548A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
Abstract
Description
본 발명은 활성탄을 이용하여 벤조피렌이 저감화된 압착유를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing compressed oil with reduced benzopyrene using activated carbon.
벤조피렌(Benzo[a]pyrene)은 다환방향족 탄화수소(PAHs) 그룹에 속하는 황색의 결정성 고체이며, 300~600℃사이 온도에서 불완전연소로 생성되기 때문에 오염원은 매우 다양하다. Benzo [a] pyrene is a yellow crystalline solid belonging to the group of polyaromatic hydrocarbons (PAHs), and since it is produced by incomplete combustion at temperatures between 300 and 600 ° C., there are a variety of pollutants.
주로 콜타르, 자동차배출가스(특히 디젤엔진), 담배연기에 존재하며 환경오염 등으로 인해 농산물, 어패류 등 조리/가공하지 않은 식품에도 존재하고 식품을 고온 가열 조리/가공시 식품의 주성분인 탄수화물, 단백질, 지질 등이 분해되어 생성되기도 한다. Mainly present in coal tar, automobile exhaust gas (especially diesel engine), tobacco smoke, and also in non-cooked / processed foods such as agricultural products and fisheries due to environmental pollution, and carbohydrates and proteins, which are the main components of foods at high temperature heating cooking / processing It is also produced by the decomposition of lipids.
벤조피렌은 잔류기간이 길고 독성도 강하여 더욱 문제화되고 있는데 내분비계장애물질이면서 발암가능물질로 CODEX(국제식품규격위원회) 및 JECFA(FAO·WHO 합동 식품첨가물전문가위원회)의 위해성 평가를 위한 우선순위 목록에 포함되는 등 세계적 관심의 대상 물질이 되고 있다. 국제암연구소(IARC)는 최근 벤조피렌을 그 룹 1의 인체 발암 물질로 등급을 상향조정하였다. 식품에서도 벤조피렌에 대한 문제가 발생하고 있는데 최근 국내에서도 올리브유 등 식용유지에 대한 벤조피렌 검출이 사회적으로 문제가 되어서 저감화에 대한 관심도 높아지고 있다. 식용유지 제조공정 중 생성되는 벤조피렌에 대한 규제는 EU가 2.0ppb, 스페인 5.0ppb, 중국 10ppb로 관리하고 있고 국내에서는 가장 엄격하게 규제하고 있는 EU 기준에 맞춰서 2.0ppb 이하로 권장규격을 설정, 시행하고 있다. Benzopyrene is more problematic due to its long retention period and its high toxicity.It is an endocrine disruptor and a carcinogen, and is listed in the priority list for risk assessment of CODEX (International Food Standards Committee) and JECFA (FAO / WHO Joint Food Additives Expert). It is included and has become a subject of global interest. The International Cancer Institute (IARC) recently upgraded benzopyrene to human carcinogens in group 1. In foods, there is a problem with benzopyrene. Recently, the detection of benzopyrene in edible oils such as olive oil has become a social problem in Korea. Regulations on benzopyrene produced during the edible oil and fat manufacturing process are set at 2.0ppb, Spain 5.0ppb, and China 10ppb. have.
이러한 벤조피렌의 유해성을 저감화하기 위해 생물학적, 물리/화학적인 여러 방법이 제시되고 있고 특히, 식품 중 식용유지에서 생성되는 벤조피렌을 저감화하는 방법으로 정제 배기 시설 설치, 압착유의 볶음 온도 조정 등이 제시되고 있다. In order to reduce the harmfulness of benzopyrene, various biological, physical and chemical methods have been proposed, and in particular, as a method of reducing benzopyrene produced in edible oils in food, installation of refinery exhaust facilities and adjustment of roasting temperature of compressed oil have been proposed. .
종래의 식용유지에서의 벤조피렌을 저감화하는 방법으로는 식용유지를 점토에 흡수시킨 후 흡수된 식용유지를 탄소화하고 그 탄소를 활성화시켜 산-활성화된 점토를 흡수제로 이용하는 것이 있다(미국특허 5,218,132호). 이 방법에서의 식용유지의 탄소화와 활성화 단계는 활성 작용 인자인 염화아연(zinc chloride)의 존재하에서 열을 가해 이루어지고 활성화 온도는 250℃ 이상이어야 한다. The conventional method for reducing benzopyrene in edible oil and fat is to absorb the edible oil in clay and then carbonize the absorbed edible oil and activate the carbon to use acid-activated clay as an absorbent (US Pat. No. 5,218,132). Carbonization and activation of edible oils and fats in this method is accomplished by applying heat in the presence of the active agonist zinc chloride, and the activation temperature should be at least 250 ° C.
하지만, 이 방법은 일반 식용유지에서는 적용할 수 있지만 압착유 특히 고추씨 기름, 참기름, 들기름의 경우 점토나 온도에 의해 풍미와 색상이 변하는 문제가 발생할 수 있다. However, this method can be applied to general edible oils, but in the case of compressed oil, especially red pepper seed oil, sesame oil, and perilla oil, there may be a problem that the flavor and color change by clay or temperature.
이에 본 발명에서는 압착유에서 발생할 수 있는 상기와 같은 문제점을 제거하기 위해 적당한 온도와 활성탄을 이용하여 벤조피렌을 저감화하는 방법을 개발하였으며, 이로 인해 풍미와 색상이 양호하며 벤조피렌 함량도 감소하는 결과를 얻어 낼 수 있었다.Therefore, the present invention has been developed a method for reducing benzopyrene using a suitable temperature and activated carbon in order to eliminate the above problems that may occur in the pressurized oil, thereby resulting in a good flavor and color and a decrease in the benzopyrene content I could make it.
활성탄(active carbon)은 주로 야자껍질, 목재, 석탄 등을 원료로 사용하여 고온에서 소성 부활시킨 특수 탄소로 활성화 과정에서 분자 크기 정도의 미세 세공이 잘 발달된 무정형탄소의 집합체이다. 활성탄의 제조원료는 식물질, 동물질, 광물질, 산업폐기물 등으로 대별할 수 있으며, 광물질의 경우는 석탄과 석유계열 등으로 구별할 수 있다. 일반적으로 분말활성탄의 제조에는 식물질 원료가 사용되며 입상활성탄의 제조에는 목탄, 야자껍질, 석탄 등이 이용된다.Active carbon is a special carbon that is mainly activated by using coconut shell, wood, and coal as a raw material, and is a collection of amorphous carbon with fine pore size of micropore in the process of activation. Raw materials for activated carbon can be roughly classified into vegetable, animal, mineral and industrial waste, and minerals can be classified into coal and petroleum. Generally, vegetable raw materials are used for the production of powdered activated carbon, and charcoal, coconut shell, coal, and the like are used for producing granular activated carbon.
활성탄의 흡착이론은 고체-액체, 기체-액체, 액체-액체 계면에서 기체 혹은 액체 중의 특정 성분이 농축되는 현상을 말한다. 흡착은 흡착의 형태에 따라 통상 물리적 흡착(physical adsorption)과 화학적 흡착(chemical adsorption)으로 분류한다. 물리적 흡착을 지배하는 힘은 반 데르 발스(van der Waals) 힘이고 화학적 흡착을 지배하는 것은 이온결합 또는 공유결합 등의 화학결합력이다. Adsorption theory of activated carbon refers to a phenomenon in which certain components of gas or liquid are concentrated at the solid-liquid, gas-liquid, and liquid-liquid interface. Adsorption is usually classified into physical adsorption and chemical adsorption according to the type of adsorption. The force that dominates the physical adsorption is the van der Waals force, and the force that dominates the chemical adsorption is the chemical bonding force such as ionic bond or covalent bond.
물리적 흡착의 경우 용질과 흡착제 사이에서 분자의 인력이 용질과 용매 사이의 인력보다 클 때 용질은 흡착제 표면에 달라붙게 된다. In the case of physical adsorption, solutes adhere to the adsorbent surface when the attraction of molecules between the solute and the adsorbent is greater than the attraction between the solute and the solvent.
따라서 본 발명은 상기와 같은 점을 감안한 것으로 압착유의 풍미와 색상을 유지하면서 제조공정 시 생성되는 벤조피렌을 효과적으로 저감화하여 안전성을 확보하기 위한 제조방법이 제공된다.Therefore, in view of the above, the present invention provides a manufacturing method for securing safety by effectively reducing the benzopyrene produced during the manufacturing process while maintaining the flavor and color of the compressed oil.
상기 목적을 달성하기 위한 본 발명에 따르면 참깨, 들깨 또는 고추씨로부터 압착유를 추출하는 단계; 상기 추출한 압착유를 탈산하는 단계; 상기 탈산한 압착유를 활성탄을 이용하여 탈색하는 단계; 및 상기 탈색한 압착유를 탈취하는 단계;를 포함하는 벤조피렌이 저감화된 압착유를 제조하는 방법을 제공한다.According to the present invention for achieving the above object, the step of extracting the compressed oil from sesame, perilla or red pepper seeds; Deoxidizing the extracted compressed oil; Decolorizing the deoxidized pressurized oil using activated carbon; And deodorizing the decolorized pressurized oil. Provides a method of manufacturing a pressurized oil having reduced benzopyrene.
바람직하게는 상기 활성탄은 압착유 대비 0.1~1.0중량%를 사용하는 벤조피렌이 저감화된 압착유를 제조하는 방법을 제공한다.Preferably, the activated carbon provides a method of producing compressed benzopyrene-reduced compressed oil using 0.1 to 1.0% by weight of the compressed oil.
바람직하게는 상기 탈색 단계는 60~110℃에서 10분간 이루어지는 벤조피렌이 저감화된 압착유를 제조하는 방법을 제공한다.Preferably, the decolorizing step provides a method for producing compressed benzopyrene-reduced pressurized oil made at 60 to 110 ° C. for 10 minutes.
더욱 바람직하게는 상기 활성탄의 크기는 12~100메쉬인 벤조피렌이 저감화된 압착유를 제조하는 방법을 제공한다.More preferably, the activated carbon has a size of 12 to 100 mesh, and provides a method of manufacturing compressed oil having reduced benzopyrene.
본 발명을 좀 더 구체적으로 설명하면 다음과 같다. The present invention is described in more detail as follows.
제1 단계(원료 선별)First step (raw material sorting)
원료(참깨, 들깨, 고추씨)에 함유된 이물질을 메쉬(Mesh)를 통해 제거하고, 자석을 통해 금속물을 제거한다.Foreign substances contained in the raw materials (sesame, perilla, red pepper seeds) are removed through the mesh, and metal is removed through the magnet.
제2 단계(추출)Second step (extraction)
먼저 원료를 압착하여 1차 추출이 이루어진다. 더욱 상세하게는 60~70℃에서 원료를 볶고 볶은 원료를 압착기(expeller)로 압착한 후 여과하여 1차 추출을 한다.First, the raw material is compressed to obtain primary extraction. In more detail, the raw material is roasted at 60-70 ° C., and the roasted raw material is compressed with a presser and then filtered to perform primary extraction.
1차 추출 후에 n-헥산(n-hexane)을 사용하여 용매 추출인 2차 추출을 행한다.After the first extraction, second extraction, which is solvent extraction, is performed using n-hexane.
제3 단계(탈산)Third Step (Deoxidation)
추출한 압착유를 50~60℃에서 가성소다 용액으로 유리 지방산을 제거하는 탈산 단계를 거친다.The extracted compressed oil is subjected to a deoxidation step of removing free fatty acids with caustic soda solution at 50-60 ° C.
제4 단계(탈색)Fourth step (bleaching)
탈산 단계를 거친 압착유를 활성탄을 사용하여 탈색하여 벤조피렌을 저감화한다. 더욱 상세하게는 압착유 대비 0.1~1.0중량%의 활성탄을 60~110℃에서 10분간 처리하여 벤조피렌을 저감화한다.The compressed oil which has undergone the deoxidation step is decolorized using activated carbon to reduce benzopyrene. More specifically, 0.1 to 1.0% by weight of activated carbon compared to the pressurized oil is treated at 60 to 110 ° C for 10 minutes to reduce benzopyrene.
제5 단계(탈취)5th Step (Deodorization)
탈색 단계를 거친 압착유를 탈취하여 정제 압착유를 제조한다.The compressed oil which has undergone the decolorizing step is deodorized to produce purified compressed oil.
본 발명에 따르면 압착유(참기름, 들기름, 고추씨기름 등)의 색가와 맛을 유지시키면서 생성되는 벤조피렌을 저감화하는 방법으로 제조 공정에 적용할 경우 벤조피렌을 효과적으로 저감화함으로써 식용유지에 대한 안전성을 확보할 수 있다According to the present invention, when applied to the manufacturing process by reducing the benzopyrene generated while maintaining the color value and taste of the compressed oil (seed oil, perilla oil, red pepper seed oil, etc.), it is possible to secure safety for edible oil and fat by effectively reducing the benzopyrene. have
이하 본 발명을 실시 예에 의하여 보다 구체적으로 설명하기로 한다. 실시 예는 본 발명을 보다 쉽게 이해하기 위하여 제공되는 것일 뿐, 본 발명이 하기 실시 예에 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples. The examples are provided only to more easily understand the present invention, and the present invention is not limited to the following examples.
[실시예 1] 흡착제 종류에 따른 벤조피렌 저감화 비교 실험Example 1 Comparative Experiment of Benzopyrene Reduction According to Adsorbent Type
흡착제 종류별로 고추씨 기름에 존재하는 벤조피렌의 함량과 매운맛, 색가의 변화를 알아보기 위해 대표적인 흡착제인 백토, 마그네졸, 활성탄을 선택하였다. 고추씨 기름에 백토, 마그네졸, 활성탄을 각각 0.5%, 1.0%을 첨가하고 90℃에서 10분간 열처리하면서 균질화하였다. 위와 같은 방법으로 처리한 후 흡착제를 여과하고 고속액체크로마토그래피(HPLC)를 이용하여 벤조피렌의 저감화 정도와 매운맛을 측정하였고 UV 스펙트럼을 이용하여 색가를 측정하였다. 그 결과는 표 1에 나타내었다. By type of adsorbent To examine the changes in the content, spicy taste, and color value of benzopyrene in red pepper seed oil, representative adsorbents such as clay, magnesol, and activated carbon were selected. 0.5%, 1.0% of white clay, magnesol and activated carbon were added to red pepper seed oil and homogenized by heat treatment at 90 ° C. for 10 minutes. After the treatment in the same manner as above, the adsorbent was filtered and the degree of reduction and spicy taste of benzopyrene was measured using high performance liquid chromatography (HPLC), and the color value was measured using UV spectrum. The results are shown in Table 1.
[표 1]TABLE 1
[규격 : 벤조피렌 (2.0ppb이하), 매운맛 (2800±300SHU), 색가 (600±300CU)][Specification: Benzopyrene (2.0ppb or less), Spicy (2800 ± 300SHU), Color Value (600 ± 300CU)]
실험 결과 색가는 세 가지 흡착제에서 규격(600±300)에 적합한 값을 얻을 수 있었으나 매운맛의 경우 마그네졸에서 규격(2800±300)보다 감소되었음을 확인할 수 있었다. 또한 벤조피렌 함량의 경우 백토와 마그네토의 경우 거의 변화가 없었으나 활성탄을 사용했을 때 0.5%와 1.0%농도에서 감소되었음을 확인할 수 있었다. 즉, 표 1의 결과로 알 수 있듯이, 백토를 사용했을 경우에 매운맛과 색가는 변화가 없었으나 벤조피렌을 저감화할 수 없었고 마그네졸을 사용했을 경우는 매운맛에 영향을 끼쳤을 뿐 아니라 벤조피렌의 함량도 큰 변화가 없었다. 그러나 활성탄을 사용했을 경우 고추씨 기름의 매운맛과 색가에 영향을 끼치지 않고 벤조피렌의 함량도 0.5%에서는 0.16ppb, 1.0%에서는 0.098ppb로 감소됨을 확인할 수 있었다. As a result, the color value was found to be suitable for the standard (600 ± 300) in three adsorbents, but it was confirmed that the spicy taste was reduced from the standard (2800 ± 300) in the magnesol. In addition, the content of benzopyrene was almost unchanged in the case of clay and magneto, but it was confirmed that the concentration was decreased at 0.5% and 1.0% when activated carbon was used. That is, as the results of Table 1 show, the use of white soil did not change the spicy taste and color value, but it was not possible to reduce benzopyrene, and the use of magnesol not only affected the spicy taste but also had a large content of benzopyrene. There was no change. However, when activated carbon was used, it was confirmed that the content of benzopyrene was reduced to 0.16 ppb at 0.5% and 0.098 ppb at 1.0% without affecting the spicy taste and color value of red pepper seed oil.
[실시예 2] 활성탄 조건별 벤조피렌 저감화 실험Example 2 Benzopyrene Reduction Experiment by Activated Carbon Condition
고추씨 기름에서의 벤조피렌 저감화는 실시예 1의 실험결과를 토대로 활성탄이 가장 적합하다고 판단하여 반응시간과 온도, 활성탄 농도를 결정하기 위하여 고추씨 기름에 활성탄을 10분 동안, 각 60℃, 90℃, 110℃에서 반응시켰으며 활성탄 의 농도는 0.1%, 0.5%, 1.0%로 각각 처리하여 저감화 정도를 살펴보았다. 활성탄의 크기는 100 mesh를 사용하였다. 그 결과는 표 2에 나타내었다. Benzopyrene reduction in red pepper seed oil was judged to be the most suitable activated carbon based on the experimental results of Example 1, and activated carbon was added to red pepper seed oil for 10 minutes in order to determine the reaction time, temperature and activated carbon concentration. The reaction was carried out at ℃ and the concentration of activated carbon was treated with 0.1%, 0.5% and 1.0%, respectively, and the degree of reduction was examined. The size of activated carbon was 100 mesh. The results are shown in Table 2.
[표 2]TABLE 2
[규격 : 벤조피렌 (2.0ppb이하), 매운맛 (2800±300SHU), 색가 (600±300CU)][Specification: Benzopyrene (2.0ppb or less), Spicy (2800 ± 300SHU), Color Value (600 ± 300CU)]
표 2의 결과를 살펴보면 조건별 활성탄 실험을 시행했을 때 매운맛과 색가는 고추씨 기름의 규격에 적합하였다. 벤조피렌의 저감화 정도를 살펴보면, 110℃, 90℃, 60℃에서 10분간 1.0%의 농도로 반응시켰을 때 벤조피렌 함량이 각각 0.11ppb, 0.098ppb와 0.12ppb로 가장 낮음을 알 수 있었다. 또한 본 실시예의 활성탄의 농도, 온도에서 벤조피렌의 저감화 효과가 대조구에 비해 월등함을 알 수 있었다.Looking at the results of Table 2, the spicy taste and color value were suitable for the specifications of red pepper seed oil when the activated carbon tests were carried out according to the conditions. Looking at the degree of reduction of benzopyrene, it was found that the benzopyrene content was the lowest as 0.11 ppb, 0.098 ppb and 0.12 ppb, respectively, when reacted at 110%, 90 ° C, and 60 ° C at a concentration of 1.0% for 10 minutes. In addition, it was found that the effect of reducing benzopyrene at the concentration and temperature of the activated carbon of the present embodiment was superior to that of the control.
[실시예 3] 활성탄 크기별 벤조피렌 저감화 실험 Example 3 Benzopyrene Reduction Experiment by Activated Carbon Size
제 3단계 (활성탄 크기별 비교 실험)Third Step (Comparison Experiment by Activated Carbon Size)
활성탄 조건별 실험 후 활성탄의 크기별로 고추씨 기름에서의 벤조피렌 저감화 정도를 알아보기로 하였다. 활성탄은 12 mesh, 20 mesh, 100 mesh의 크기를 사용하였고 활성탄 농도는 0.5%로 하였으며, 60℃에서 10분간 반응시켜 저감화 정도를 살펴보았다. 그 결과는 표 3에 나타내었다. After the experiment by activated carbon condition, the degree of benzopyrene reduction in red pepper seed oil was determined by the size of activated carbon. Activated carbon was used as the size of 12 mesh, 20 mesh, 100 mesh and the concentration of activated carbon was 0.5%, and the reduction degree was examined by reacting at 60 ° C for 10 minutes. The results are shown in Table 3.
[표 3]TABLE 3
표 3의 결과를 살펴보면 100 mesh의 활성탄을 사용했을 경우 벤조피렌 함량이 0.19ppb이던 것에 비해 12 mesh와 20 mesh 활성탄을 사용한 경우 0.36pp와 0.52ppb로 벤조피렌 저감화 정도가 작음을 알 수 있었다. 따라서 활성탄의 크기가 미세할수록 벤조피렌을 흡착하는 능력도 증가함을 실험 결과를 바탕으로 알 수 있었다. The results of Table 3 show that the benzopyrene reduction was less than 0.36pp and 0.52ppb when 12 mesh and 20 mesh activated carbon were used when the benzopyrene content was 0.19ppb when 100 mesh activated carbon was used. Therefore, the smaller the size of activated carbon, the more the ability to adsorb benzopyrene was found on the basis of the experimental results.
[실험예 1]Experimental Example 1
고추씨 기름에 0.3%의 활성탄을 60℃에서 10분 동안 반응시켜서 제조된 샘플들의 벤조피렌 저감화 정도를 확인하였다.0.3% activated carbon was reacted with red pepper seed oil at 60 ° C. for 10 minutes to confirm the degree of benzopyrene reduction of the prepared samples.
그 결과는 표 4에 나타내었다. The results are shown in Table 4.
[표 4] TABLE 4
표 4의 결과를 보면 현장 적용 시 벤조피렌 함량은 0.10~0.35ppb 수준으로 저감화가 원활하게 이루어졌음을 확인할 수 있었다.Looking at the results of Table 4, it was confirmed that the benzopyrene content was reduced smoothly to 0.10 to 0.35 ppb level in the field application.
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