KR20020029444A - Orient tobacco casing and method for preparing the same - Google Patents

Orient tobacco casing and method for preparing the same Download PDF

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KR20020029444A
KR20020029444A KR1020000051094A KR20000051094A KR20020029444A KR 20020029444 A KR20020029444 A KR 20020029444A KR 1020000051094 A KR1020000051094 A KR 1020000051094A KR 20000051094 A KR20000051094 A KR 20000051094A KR 20020029444 A KR20020029444 A KR 20020029444A
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component
extract
orient
layer
flavor
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KR1020000051094A
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KR100369460B1 (en
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강병광
이승훈
이태호
신경은
김대중
박영수
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강병광
주식회사 한불화농
김재홍
한국담배인삼공사
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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18—Treatment of tobacco products or tobacco substitutes
    • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303—Plant extracts other than tobacco
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10—Chemical features of tobacco products or tobacco substitutes

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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Botany (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)
  • Seasonings (AREA)

Abstract

PURPOSE: Provided are an oriental cigarette perfume and a method for preparation of the same to efficiently extract aromatic components and flavoring components from the oriental leaves without loss of them. CONSTITUTION: The oriental perfume is prepared by several steps of firstly extracting the oriental leaves with 70-80% ethanol or isopropyl alcohol; secondly extracting the first extract with 50% ethanol or isopropyl alcohol then filtering the extracts; adding alkali solution to the filtered extract to adjust into pH9.5; fractionally dividing the adjust extract into a perfume fraction and a flavoring fraction with organic solvent; adding glacial acetic acid or lactose in water into the perfume fraction to remove a water phase with nicotine components while adding sugar and amino acid to the flavoring fraction to conduct a browning reaction thereof; admixing the nicotine-free component and the browning reacted flavoring component. The sugar component may be high consistency fructose and the amino acid component is selected from glycine, alanine and valine.

Description

오리엔트 담배 가향료 및 그 제조방법{ORIENT TOBACCO CASING AND METHOD FOR PREPARING THE SAME}ORIENT TOBACCO CASING AND METHOD FOR PREPARING THE SAME}

본 발명은 오리엔트 담배 가향료 및 그 제조방법에 관한 것이다. 좀더 상세하게는 오리엔트엽으로부터 담배추출물을 제조할 때 향기성분 및 풍미성분을 손실함이 없이 효율적으로 추출할 수 있게 하는 담배 가향료의 제조방법에 관한 것이다.The present invention relates to an orient tobacco flavoring agent and a manufacturing method thereof. More particularly, the present invention relates to a method for preparing tobacco flavor, which enables efficient extraction without losing flavor and flavor components when preparing tobacco extract from orient leaves.

최근에 흡연가들은 흡연으로 인한 건강문제가 사회적 이슈로 크게 부각됨에 따라 가능한 한 니코친 함량이 적으면서도 고유의 담배맛은 그대로 간직한 담배를 선호하게 되었다.In recent years, as the health problems caused by smoking have been highlighted as a social issue, smokers have preferred cigarettes that have as little nicotine content as possible but still retain their own taste.

이러한 흡연가들의 기호에 맞추기 위해 특허공고 제91-6520호에서는 엽설, 담배가루 등으로부터 추출한 담배추출물을 담배 가향료로 사용하되 카보닐기를 갖는 당류와 담배추출물을 반응시켜 추출물 중의 자극성 성분을 변화시키고, 이를 담배 제조시에 가향함으로써 자극성이 완화되고 담배향이 향상된 담배를 제조하는 방법을 공개하고 있다. 또, 등록특허 제10-0217828호에서는 원료(황색종) 잎담배추출물을 알카리 수용액으로 처리하여 니코틴을 제거함으로써 저니코틴 담배추출물 제조하는 방법을 공개하고 있다.In order to meet the preferences of smokers, Patent Publication No. 91-6520 uses tobacco extract extracted from leafy tobacco, tobacco powder, and the like as a tobacco flavoring agent, and changes the irritant component in the extract by reacting a saccharide having a carbonyl group with the tobacco extract, It discloses a method for producing tobacco with improved irritation and improved tobacco aroma by flavoring it in the manufacture of tobacco. In addition, Korean Patent No. 10-0217828 discloses a method for preparing low nicotine tobacco extract by treating raw material (yellow species) leaf tobacco extract with an aqueous alkali solution to remove nicotine.

그러나, 이러한 선 기술 방법들은 담배의 향기성분과 담배 맛을 결정하는 일반성분들이 추출용매의 농도에 따라 그 효율 및 성분의 분포가 달라진다는 사실을 간과함으로써 담배의 향과 맛을 결정하는 성분의 손실이 있을 수도 있다는 점을 못보고 넘긴 단점이 있다. 특히, 후술한 등록특허 제10-0217828호 발명은 황색종 잎담배로부터 원하는 바의 저 니코틴 담배추출물은 얻을 수 있을지 모르나 추출 과정에서 담배 향기성분의 손실이 많아서, 순하지만 오리엔트 고유의 향을 느낄 수 없는 무미건조한 담배로 될 수도 있다는 문제점을 안고있다. 더구나, 고유의 담배향을 많이 갖고 있어 고급 담배의 향기성분으로 배합되는 오리엔트엽의 경우는 상기 선 기술방법으로 추출하면 향기성분이 적게 추출되어 오히려 질의 저하를 가져올 수도 있다.However, these prior art methods lose the component that determines the aroma and taste of tobacco by overlooking the fact that the efficiency and distribution of components vary according to the concentration of extractant. There is a drawback to not seeing that there may be. In particular, the invention described below Patent No. 10-0217828 may be obtained low nicotine tobacco extract as desired from the yellow leaf tobacco, but there is a lot of loss of tobacco fragrance component in the extraction process, it is mild but can not feel the inherent aroma The problem is that it can be a dry cigarette. In addition, in the case of the orient leaf, which has a lot of inherent tobacco aroma and is blended as a fragrance component of a high-quality tobacco, the fragrance component may be less extracted when extracted by the above-described prior art method, which may result in deterioration of quality.

오리엔트엽은 특유의 향기와 순한 끽미를 갖고 있는데, 이는 산성분과 수지성분에 기인하는 것으로 알려져 있으며, 또한 순한 맛과 구수한 풍미의 캬라멜취는 오리엔트엽에 함유된 당류가 비효소적 갈변반응에 의해 피라진계 물질로 변환되어 나타나는 것으로 알려져 있다. 주요 향기성분은 3-메틸-부틸산, 솔라논, 3-메틸-발레르산, 네오피타디엔 등이며 오리엔트엽은 타 잎담배에 비하여 이들 성분이 5∼10배나 많이 들어 있다. 그러나 이를 종래 선 기술 방법으로 추출하면 향기성분의 15∼20%만 추출되며, 특히 일부 탄화수소계열의 향기성분인 네오피타디엔 류는 추출이 거의 안된다는 단점이 있다.Orient leaves have a characteristic scent and mild taste, which are known to be due to acid and resin components, and the caramel odor of mild taste and flavor is pyrazine due to the non-enzymatic browning reaction of sugars contained in orient leaves. It is known to be converted to a systemic material. The main fragrance components are 3-methyl-butyl acid, solanone, 3-methyl-valeric acid, neo-pitadiene, etc. Orient leaves contain 5 to 10 times more of these components than other leaf tobacco. However, when extracted by the prior art method, only 15 to 20% of the fragrance components are extracted, and in particular, neo-pitadienes, which are some hydrocarbon-based fragrance components, have a disadvantage in that they are hardly extracted.

이에, 본 발명자는 상기와 같은 문제점을 해결하기 위해 여러 가지로 연구를 거듭한 끝에 오리엔트엽 향미성분을 추출하는 과정 중에 용매의 농도를 달리하여 2단계로 추출하면 오리엔트엽의 고유 향기성분과 풍미성분의 추출효율은 높일 수 있는 방법을 개발하게 되어 본 발명을 완성하기에 이르렀다.Thus, the present inventors have been repeatedly studied in various ways to solve the above problems, the extraction of the orient leaf flavor component in the process of extracting the solvent concentration in two steps by extracting the intrinsic aroma component and flavor component of the orient leaf The extraction efficiency of the method was developed to increase the present invention was completed.

오리엔트엽의 향기성분과 풍미성분은 추출용매의 농도에 따라 그 추출효율이 크게 차이가 남을 발견하게 되었는데, 향기성분은 저농도(50%) 보다 고농도(70∼80%)에서 5∼10배나 추출이 더 잘되며, 주로 캬라멜취와 구수한 토스트 풍미의 피라진계 물질의 전구체가 되는 당류성분은 고농도에서보다 저농도에서 40%나 수율이 더 좋다.It was found that the extraction efficiency of orient leaf and flavor component differed greatly depending on the concentration of the extraction solvent.The fragrance component was extracted 5-10 times at high concentration (70-80%) than low concentration (50%). Better sugars, sugars, which are the precursors of the pyrazine-based materials of mainly caramel and sweet toast flavors, are 40% better at low concentrations than at high concentrations.

본 발명의 목적은 오리엔트엽의 향기성분의 손실 없이 추출할 수 있는 방법을 제공함으로써 오리엔트 향이 풍부하고 또한 구수한 풍미의 담배 가향료를 제공하는데 있다.SUMMARY OF THE INVENTION An object of the present invention is to provide a tobacco flavor with an orient-rich and delicious flavor by providing a method that can be extracted without loss of the aromatic component of the orient leaf.

본 발명의 다른 하나의 목적은 오리엔트엽 추출시에 피라진계 풍미성분과 오리엔트향 추출성분을 2개의 분획으로 별도로 추출하고, 권련의 제조시 흡연자의 기호에 맞게 이들을 조합 가향함으로써 다양한 흡연자의 욕구에 맞는 담배를 제조할 수 있도록 한 담배 가향료를 제공하는데 있다.Another object of the present invention is to extract the pyrazine-based flavor components and orient flavor extract components separately in two fractions during the extraction of the orient lobe, and to combine them according to the taste of smokers in the manufacture of cigarettes to meet the needs of various smokers It is to provide a tobacco flavor for making tobacco.

도 1은 본 발명 실시예 1의 담배추출물 향기성분 분석결과를 보여주는 GC/MS차트 도표.1 is a GC / MS chart chart showing the results of the tobacco extract aroma component analysis of Example 1 of the present invention.

도 2는 본 발명 실시예 2의 담배추출물 향기성분 분석결과를 보여주는 GC/MS차트 도표.Figure 2 is a GC / MS chart chart showing the results of the tobacco extract aroma component analysis of Example 2 of the present invention.

도 3은 종래 담배추출물 향기성분 분석결과를 보여주는 GC/MS차트 도표.Figure 3 is a GC / MS chart chart showing the results of conventional tobacco extract aroma component analysis.

도 4는 또 다른 종래 담배추출물 향기성분 분석결과를 보여주는 GC/MS차트 도표.Figure 4 is a GC / MS chart chart showing the results of another conventional tobacco extract aroma component analysis.

도 5는 본 발명 실시예 1의 갈변반응 후의 피라진계 성분 함량분석 결과를 나타내는 GC/MS차트 도표.5 is a GC / MS chart showing the results of pyrazine-based component content analysis after the browning reaction of Example 1 of the present invention.

도 6은 본 발명 실시예 2의 갈변반응 후의 피라진계 성분 함량분석 결과를 나타내는 GC/MS차트 도표.6 is a GC / MS chart showing the results of pyrazine-based component content analysis after the browning reaction of Example 2 of the present invention.

도 7은 종래 기술의 갈변반응 후의 피라진계 성분 함량분석 결과를 나타내는 GC/MS차트 도표.7 is a GC / MS chart diagram showing the results of pyrazine-based component content analysis after the browning reaction of the prior art.

도 8은 또 다른 종래 기술의 갈변반응 후의 피라진계 성분 함량분석 결과를 나타내는 GC/MS차트 도표.8 is a GC / MS chart diagram showing the results of pyrazine-based component content analysis after another conventional browning reaction.

본 발명은 담배의 오리엔트향 가향료를 제조함에 있어, 오리엔트엽을 1단계로 고농도의 알콜로 추출하고, 2단계로 저농도의 알콜로 추출함으로써 오리엔트엽 향기성분과 당류성분을 최대한으로 추출할 수 있도록 한 오리엔트 담배 가향료 및 그 제조방법에 관한 것이다.In the present invention, in preparing an orient fragrance flavor of tobacco, by extracting the orient leaf with a high concentration of alcohol in one step, and extracting with a low concentration of alcohol in two steps to extract the aromatic components and sugar components of the orient leaf to the maximum An orient tobacco flavoring agent and a method of manufacturing the same.

본 발명의 오리엔트 담배 가향료는 오리엔트엽을 1단계로 70∼80%의 에탄올로 추출하고, 2단계로 50%의 에탄올로 추출하여 여과하고, 그 여액에 알카리를 가하여 pH를 9.5로 맞춘 후에 유기용제를 사용하여 향 추출성분과 풍미성분으로 분획한 후, 상기 풍미성분에는 당과 아미노산을 가하여 비효소적 갈변반응을 시키고, 상기 향 추출성분에는 유기산과 물을 가하여 교반하고 정치하여 물층을 제거함으로써 니코틴을 제거한 다음, 상기 갈변반응을 시킨 풍미성분과 니코틴을 제거한 향 추출성분을 혼합하여서 된 오리엔트 담배 가향료이다.Orient tobacco flavoring agent of the present invention is extracted with 70-80% ethanol in one step, 50% ethanol in two steps and filtered, and added to the filtrate to adjust the pH to 9.5 after organic After fractionation into a flavor extract component and a flavor component using a solvent, a sugar and an amino acid is added to the flavor component to undergo a non-enzymatic browning reaction, and an organic acid and water are added to the flavor extract component by stirring and standing to remove the water layer. After removing nicotine, the flavor component subjected to the browning reaction and the flavor extract component from which nicotine has been removed are orient tobacco flavors.

본 발명의 가향료 제조방법은 아래의 단계로 구성된다.The fragrance preparation method of the present invention comprises the following steps.

(가) 오리엔트엽 스크랩(scrap)에 1단계로 중량기준 (이하 같다) 8∼10배의 70∼80% 에탄올을 가하여 40∼50℃에서 9∼14시간동안 가열 용매순환식으로 추출하고, 이 추출물을 바스켓필터를 사용하여 전처리여과를 한 후, 다시 1㎛ 필터로 여과하여 여액과 잔사를 분리하는 공정;(A) To the orient leaf scrap, add 8 to 10 times 70 to 80% ethanol in one step by weight (same as below), and extract by heating solvent circulation at 40 to 50 ° C for 9 to 14 hours. Pre-filtering the extract using a basket filter, and then filtering the filter with a 1 μm filter to separate the filtrate and the residue;

(나) 2단계로 잔사에 다시 6∼8배의 50% 에탄올을 가하여 40∼50℃에서 4∼7시간동안 가열 용매순환식으로 추출하고, 이 추출물을 바스켓필터를 사용하여 전처리여과를 한 후, 다시 1㎛ 필터로 여과하여 여액과 잔사를 분리하는 공정;(B) Add 6-8 times 50% ethanol to the residue in two steps, extract by heating solvent circulation for 4-7 hours at 40-50 ℃, and extract this filter using pre-filter using basket filter. In addition, the step of separating the filtrate and the residue by filtration with a 1㎛ filter;

(다) 상기 2단계 잔사를 착즙하여 잔사는 폐기한 후, 즙액은 1㎛ 필터로 여과하고 이 여액을 상기 1단계 및 2단계 여액과 혼합하여 45℃에서 브릭스 60∼65°가 되도록 진공 농축하여 농축액을 제조하는 공정;(C) After extracting the second step residue and discarding the residue, the juice solution is filtered with a 1㎛ filter and the filtrate is mixed with the first and second step filtrate and concentrated in vacuo at 45 ℃ to 60 ~ 65 ° brix Preparing a concentrate;

(라) 상기 농축액에 알카리 수용액인 28% NH4OH를 가하여 pH를 9.5로 맞춘 후에 농축액의 2배에 해당하는 유기용제 n-헥산을 가하여 30∼60분간 교반하고 6∼8시간 정치한 후, 헥산층과 물층으로 1차 층 분리를 행하는 공정;(D) 28% NH 4 OH, an aqueous alkaline solution, was added to the concentrated solution to adjust the pH to 9.5, followed by adding an organic solvent n-hexane corresponding to twice the concentration, stirred for 30 to 60 minutes, and allowed to stand for 6 to 8 hours. Performing primary layer separation into a hexane layer and a water layer;

(마) 상기 물층에 다시 1.5배의 n-헥산을 가하고 30∼60분간 교반하여18∼30시간 정치한 후, 2차 층 분리를 행하여 헥산층과 물층으로 분리하는 공정, 이때 향기성분과 니코틴은 헥산층으로 이행되고, 피라진계 풍미성분의 전구물질인 당류는 물층으로 이행된다;(E) 1.5-fold n-hexane was added to the water layer again, stirred for 30 to 60 minutes, allowed to stand for 18 to 30 hours, and the secondary layer was separated to separate the hexane layer and the water layer. Transferred to the hexane layer, and the saccharide, a precursor of the pyrazine flavor component, to the water layer;

(바) 상기 물층에 대해 고과당 15중량%와 푸로필렌글리콜 15중량% 및 글리신, 알라닌, 발린 중에서 선택된 1가지 성분 2중량%를 첨가한 다음 80∼90℃에서 2시간 이상 비효소적 갈변반응을 진행시켜 피라진(Pyrazin)계 풍미성분으로 변환시키는 공정;(F) 15% by weight of high fructose, 15% by weight of furofylene glycol and 2% by weight of one component selected from glycine, alanine, and valine, followed by a non-enzymatic browning reaction at 80-90 ° C. for 2 hours or more. Advancing the pyrazin-based flavor component;

(사) 상기 (라), (마)항에서 1차, 2차 층 분리된 헥산층을 혼합하고 1/2로 농축한 후, 농축액의 15∼20중량%에 해당하는 빙초산 또는 젖산 및 농축액의 70∼80중량%에 해당하는 물을 가하고 10∼15분간 교반한 후, 1∼2시간 정치시켜 니코틴이 함유된 물층은 제거하고, 재차 농축액의 10∼15중량%에 해당하는 빙초산 또는 젖산 및 농축액의 70∼80중량%에 해당하는 물을 가하고 10∼15분간 교반한 후, 1∼2시간 정치시켜 물층은 제거한 다음, 여기에 같은 량의 물만을 가하고 다시 10∼15분간 교반한 후, 2∼3시간 정치시켜 물층은 제거하고 향기성분이 함유된 헥산층을 얻는다. 이 헥산층을 1/3로 농축시켜 동일 량의 95% 에탄올을 가하고 30분간 교반한 후, 에탄올 층을 분리하고 1/4로 농축하여 향 추출성분(앱솔루트)을 만드는 공정;(G) After mixing the hexane layer separated in the primary and secondary layers in (d) and (d) above and concentrating to 1/2, the amount of glacial acetic acid or lactic acid and the concentrated liquid corresponding to 15-20% by weight of the concentrated liquid 70 to 80% by weight of water was added and stirred for 10 to 15 minutes, and then allowed to stand for 1 to 2 hours to remove the water layer containing nicotine, and again to 10 to 15% by weight of glacial acetic acid or lactic acid and concentrate After adding water corresponding to 70 to 80% by weight of the solution and stirring for 10 to 15 minutes, allowing to stand for 1 to 2 hours to remove the water layer, then adding the same amount of water only and stirring for another 10 to 15 minutes, then 2 to After standing for 3 hours, the water layer is removed to obtain a hexane layer containing an aromatic component. Concentrating the hexane layer to 1/3 to add the same amount of 95% ethanol and stirred for 30 minutes, then separating the ethanol layer and concentrated to 1/4 to make a fragrance extract component (absolute);

(아) 상기 피라진(Pyrazin)계 풍미성분을 함유하는 (바)항의 풍미성분과 상기 (사)항의 농축 향 추출성분을 배합하여 오리엔트 담배 가향료를 제조하는 공정으로 구성된다.(H) A process for producing an orient tobacco flavoring agent by blending the flavor component of (bar) containing the pyrazin-based flavor component with the concentrated flavor extract component of the above (g).

상기 추출용매로는 에탄올 외에 이소푸로필알콜이 사용될 수 있고, 유기용제로는 n-헥산 외에 벤젠이 사용될 수 있으며, pH를 맞추기 위한 알카리로는 수산화암모늄 외에 수산화칼륨이 사용될 수 있다. 오리엔트엽의 경우는 고유의 오리엔트향은 풍부하나 순한 맛과 구수한 캬라멜 향취미를 내는 풍미성분은 충분하지 않아 이를 최대한으로 추출할 것이 요구된다. 담배의 풍미성분은 통상 당류와 아미노산류의 함량에 따라 결정이 되는데, 이들 성분은 추출용매의 농도가 50%에서 가장 많이 추출되며, 비효소적 갈변반응에 의해 향취미를 내는 피라진 계통의 풍미성분로 변하게 된다. 오리엔트엽의 경우 본래 내재되어 있는 풍미성분이 충분치 못하므로 본 발명에서는 당류와 아미노산류를 추가로 첨가해 주었다. 본 발명에 사용된 당류로는 고과당이, 아미노산으로는 글리신, 알라닌, 발린 등이 사용되었다. 푸로필렌글리콜은 당과 아미노산을 잘 혼화시켜주기 위한 유화제로서 사용되었다.In addition to ethanol, isoprophyl alcohol may be used as the extraction solvent, benzene may be used in addition to n-hexane, and potassium hydroxide may be used in addition to ammonium hydroxide as an alkali to adjust the pH. In the case of the orient leaf, the inherent orient flavor is abundant, but the mild ingredient and flavor of the caramel flavor are not enough. Flavor component of tobacco is usually determined according to the content of sugars and amino acids, and these components are the most extracted at 50% concentration of the extraction solvent, and the flavor component of the pyrazine system which gives a taste by non-enzymatic browning reaction. Will change to In the case of the orient leaf, since the inherent flavor component is not sufficient, the present invention further added sugars and amino acids. As the sugars used in the present invention, high fructose is used, and amino acids are glycine, alanine, valine and the like. Fulopylene glycol has been used as an emulsifier to mix sugars and amino acids well.

이하 본 발명을 실시예에 의거 상세히 설명한다.Hereinafter, the present invention will be described in detail with reference to Examples.

본 실시예에서 농축액의 오리엔트 향기성분인 3-메틸-부틸산, 솔라논, 3-메틸-발레르산, 네오피타디엔 등은 GC/MS(gas chromatography/mass spectrometry) 분석법으로 분석하였으며, 당류성분이 함유된 농축액의 수율은 총 여액을 동일조건(45℃)에서 브릭스 농도 65°가 될 때까지 감압 농축하여 얻은 농축액을 평량하여 측정하였다.In the present embodiment, the orient aromatic components of the concentrate, 3-methyl-butyl acid, solanone, 3-methyl-valeric acid, neopitadiene and the like were analyzed by gas chromatography / mass spectrometry (GC / MS) analysis. The yield of the contained concentrate was measured by basal weight of the concentrate obtained by concentrating the total filtrate under reduced pressure until the brix concentration was 65 ° under the same conditions (45 ° C).

[실시예 1]Example 1

오리엔트 농축액의 제조Preparation of Orient Concentrate

용매순환식 추출기에 1단계로 오리엔트엽(바스마종) 스크랩 10㎏과 80% 에탄올 100㎏을 넣고 40℃에서 14시간동안 추출하였다. 추출물을 바스켓필터로 여과한 후, 여액은 다시 1㎛ 필터로 여과하고, 잔사는 2단계로 50% 에탄올 60㎏을 가하여 40℃에서 4시간동안 추출하였다. 2단계 추출물을 바스켓필터로 여과하고 여액은 다시 1㎛ 필터로 여과하여 여액을 1단계 추출여액과 혼합하고, 잔사는 착즙하여 폐기하고, 즙액은 1㎛ 필터로 여과하여 상기 1단계 및 2단계 여액과 혼합 한 후, 45℃에서 브릭스 농도 65°가 될 때까지 감압 농축하였다. 얻어진 오리엔트 농축액은 5.68㎏ 이었다. 농축액의 향기성분은 아래의 조건으로 측정하고 그 결과를 표 1 및 도 1에 나타내었다.10 kg of 80% ethanol scrap and 100 kg of Orient leaf (Basma species) were put into a solvent cyclic extractor and extracted at 40 ° C. for 14 hours. After the extract was filtered through a basket filter, the filtrate was again filtered through a 1 μm filter, and the residue was extracted at 40 ° C. for 4 hours by adding 60 kg of 50% ethanol in two steps. The two-stage extract is filtered with a basket filter, the filtrate is again filtered through a 1 μm filter, the filtrate is mixed with the first-stage extract filtrate, the residue is juiced and discarded, and the juice is filtered with a 1 μm filter to filter the first and second stage filtrates. After mixing with, the mixture was concentrated under reduced pressure at 45 ° C. until the Briggs concentration reached 65 °. The obtained orient concentrate was 5.68 kg. The aroma component of the concentrate was measured under the following conditions, and the results are shown in Table 1 and FIG. 1.

GC/MS 조건GC / MS condition

(1) GC/MS:HP 5890 Series Ⅱ/HP 5970 (Hewlett Packard 사제)(1) GC / MS: HP 5890 Series II / HP 5970 (manufactured by Hewlett Packard)

(2) 컬럼:FFAP (50m x 0.2㎜ x 0.3㎛)(2) column: FFAP (50m x 0.2mm x 0.3㎛)

(3) 오븐 온도:60℃ → 2℃/분 → 210℃(70분)(3) Oven temperature: 60 degrees Celsius → 2 degrees Celsius / minute → 210 degrees Celsius (70 minutes)

(4) 인젝숀 온도:250℃(4) Injection temperature: 250 ℃

(5) 인터페이스 온도: 250℃(5) interface temperature: 250 ℃

(6) 이온화 볼테지:70 eV(6) Ionization Voltage: 70 eV

(7) 캐리어 가스:He(7) carrier gas: He

(8) 흐름 속도:0.8㎖/분(8) flow rate: 0.8ml / min

GC 조건GC condition

(1) GC:시마쯔 16/A (SHIMADZU 사제)(1) GC: Shimatsu 16 / A (product made by SHIMADZU)

(2) 컬럼:FFAP (25m x 0.2㎜ x 0.33㎛)(2) column: FFAP (25m x 0.2mm x 0.33㎛)

(3) 오븐 온도:70℃ → 2.5℃/분 → 135℃ → 3℃/분 → 220℃ (50분)(3) Oven temperature: 70 ° C → 2.5 ° C / min → 135 ° C → 3 ° C / min → 220 ° C (50 minutes)

(4) 인젝숀 온도:260℃(4) Injection temperature: 260 ° C

(5) 검출 온도: 280℃(5) Detecting Temperature: 280 ℃

(6) 분할 방출:50 : 1(6) split release: 50: 1

(7) 흐름 속도:1.7㎖/분(7) flow rate: 1.7ml / min

(8) 시료크기:0.1㎛(8) Sample size: 0.1㎛

시료 주입은 다이렉트 인젝숀(direct injection)으로 하였다.Sample injection was by direct injection.

추출성분의 층 분리Layer Separation of Extracts

상기 오리엔트 농축액 5.68㎏에 28% NH4OH를 가하여 pH를 9.5로 맞춘 후, 11.4㎏의 n-헥산을 가하여 30분간 교반하고 6시간 정치한 후에 헥산층과 물층으로 1차 층 분리를 행한다. 다음 물층에 다시 8.5㎏의 n-헥산을 가하고 30분간 교반하여 18시간 정치한 후, 2차 층 분리를 행하여 헥산층 19.9㎏과 물층 6.1㎏을 분리하였다.After adding 28% NH 4 OH to 5.68 kg of the orient concentrate solution to adjust the pH to 9.5, 11.4 kg of n-hexane was added thereto, stirred for 30 minutes, and allowed to stand for 6 hours, followed by primary layer separation with a hexane layer and a water layer. Next, 8.5 kg of n-hexane was further added to the water layer, stirred for 30 minutes, and allowed to stand for 18 hours. Then, secondary layer separation was performed to separate 19.9 kg of the hexane layer and 6.1 kg of the water layer.

풍미성분의 제조Preparation of Flavor Ingredients

상기 층 분리로 얻어진 물층 6.1㎏에 고과당 15중량%(0.9㎏)과 푸로필렌글리콜 15중량%(0.9㎏), 글리신 2중량%(0.12㎏)을 첨가하고 90℃로 2시간 열처리하여 비효소적 갈변반응을 진행시켜서 풍미성분 7.1㎏을 얻었다. 열처리로 변환된 피라진계 성분의 함량분석은 GC/MS법으로 분석하였다. 분석결과는 표 2 및 도 5에 나타내었다.15 weight% (0.9 kg) of high fructose, 15 weight% (0.9 kg) of furofylene glycol, and 2 weight% (0.12 kg) of glycine were added to 6.1 kg of the water layer obtained by the separation of the layers, and heat-treated at 90 ° C. for 2 hours. Red browning was carried out to obtain 7.1 kg of flavor component. The content analysis of pyrazine-based components converted to heat treatment was analyzed by GC / MS method. The analysis results are shown in Table 2 and FIG.

GC/MS 조건GC / MS condition

(1) GC/MS:HP 6890/HP 5973 (Hewlett Packard 사제)(1) GC / MS: HP 6890 / HP 5973 (manufactured by Hewlett Packard)

(2) 컬럼:HP-Inowax (50m x 0.32㎜ x 0.5㎛)(2) Column: HP-Inowax (50m x 0.32mm x 0.5μm)

(3) 오븐 온도:85℃ → 2℃/분 → 220℃(60분)(3) Oven temperature: 85 degrees Celsius → 2 degrees Celsius / minute → 220 degrees Celsius (60 minutes)

(4) 인젝숀 온도:250℃(4) Injection temperature: 250 ℃

(5) 인터페이스 온도: 240℃(5) interface temperature: 240 ℃

(6) 이온화 볼테지:70 ev(6) Ionization Voltage: 70 ev

(7) 캐리어 가스:He(7) carrier gas: He

(8) 흐름 속도:1.3㎖/분(8) Flow rate: 1.3 ml / min

GC 조건GC condition

(1) GC:HP 5890 series Ⅱ (Hewlrtt Packard 사제)(1) GC: HP 5890 series II (manufactured by Hewlrtt Packard)

(2) 컬럼:HP-Inowax (60m x 0.32㎜ x 0.52㎛)(2) Column: HP-Inowax (60m x 0.32mm x 0.52㎛)

(3) 오븐 온도:85℃ → 2℃/분 → 220℃(60분)(3) Oven temperature: 85 degrees Celsius → 2 degrees Celsius / minute → 220 degrees Celsius (60 minutes)

(4) 인젝숀 온도:260℃(4) Injection temperature: 260 ° C

(5) 검출 온도: 280℃(5) Detecting Temperature: 280 ℃

(6) 분할 방출:65 : 1(6) split release: 65: 1

(7) 흐름 속도:1.7㎖/분(7) flow rate: 1.7ml / min

시료는 전처리(증류시켜 에테르에 용해시킴) 후 인젝숀(injection) 하였다.Samples were pretreated (distilled and dissolved in ether) and then injected.

오리엔트 향 추출성분의 제조Preparation of Orient Fragrance Extract

상기 층 분리된 헥산층 19.9㎏을 1/2로 농축하고, 여기에 2.0㎏의 빙초산과 8.0㎏의 물을 가하여 15분간 교반한다. 2시간 정치시켜 니코틴이 함유된 물층을 제거하고, 다시 1.5㎏의 빙초산과 8.0㎏의 물을 가하고 위 과정을 반복하여 물층을 제거한 후, 이번에는 같은 량의 물만을 가하여 위 과정을 반복하고 물을 완전히 제거하여 헥산층만을 취하였다. 이렇게 얻어진 헥산층 9.9㎏을 1/3로 농축하고 3.3㎏의 95% 에탄올을 가하여 30분간 교반한 후, 에탄올층을 층 분리하고 1/4로 농축하여 오리엔트 향 추출성분 0.8㎏을 얻었다.19.9 kg of the separated hexane layer was concentrated to 1/2, and 2.0 kg of glacial acetic acid and 8.0 kg of water were added thereto, followed by stirring for 15 minutes. After standing for 2 hours, the nicotine-containing water layer was removed, 1.5 kg of glacial acetic acid and 8.0 kg of water were added again, and the above process was repeated to remove the water layer. This time, only the same amount of water was added and the water was repeated. It was completely removed to take only the hexane layer. The hexane layer thus obtained was concentrated to 1/3 and stirred for 30 minutes by addition of 3.3 kg of 95% ethanol. The ethanol layer was separated and concentrated to 1/4 to obtain 0.8 kg of orient extract component.

오리엔트 담배 가향료의 조합Orient Tobacco Flavor Combination

상기 비효소적 갈변반응으로 얻어진 풍미성분 7.1㎏과 상기 오리엔트 향 추출성분 0.8㎏을 배합하여 오리엔트 담배 가향료 7.9㎏을 제조하였다.7.1 kg of the flavor component obtained by the non-enzymatic browning reaction and 0.8 kg of the orient flavor extract component were combined to prepare 7.9 kg of orient tobacco flavoring agent.

[실시예 2]Example 2

오리엔트 농축액의 제조Preparation of Orient Concentrate

용매순환식 추출기에 1단계로 오리엔트엽(바스마종) 스크랩 10㎏과 70% 이소푸로필알콜 80㎏을 넣고 50℃에서 9시간동안 추출하였다. 추출물을 바스켓필터로 여과한 후, 여액은 다시 1㎛ 필터로 여과하고, 잔사는 2단계로 50% 이소푸로필알콜 80㎏을 가하여 50℃에서 7시간동안 추출하였다. 2단계 추출물을 바스켓필터로 여과하고 여액은 다시 1㎛ 필터로 여과하여 1단계 추출여액과 혼합하고, 잔사는 착즙하여 폐기하고, 즙액은 1㎛ 필터로 여과하여 상기 1단계 및 2단계 여액과 혼합 한 후, 45℃에서 브릭스 농도 65°가 될 때까지 감압 농축하였다. 얻어진 오리엔트 농축액은 5.69㎏ 이었다. 농축액의 향기성분은 실시예 1과 같은 방법으로 성분분석을 행하고 표 1 및 도 2에 나타내었다.10 kg of orient leaf (Basma species) scrap and 80 kg of 70% isofurophyl alcohol were added to the solvent circulation extractor in one step, and extracted at 50 ° C. for 9 hours. After the extract was filtered with a basket filter, the filtrate was again filtered with a 1 μm filter, and the residue was extracted at 50 ° C. for 7 hours by adding 80 kg of 50% isopropyl alcohol in two steps. Filter the two-stage extract with a basket filter, and filter the filtrate again with a 1㎛ filter and mix with the first-stage filtrate, the residue is juiced and discarded, the juice is filtered with a 1㎛ filter and mixed with the first and second filtrates Then, the mixture was concentrated under reduced pressure at 45 ° C. until the brix concentration reached 65 °. The obtained orient concentrate was 5.69 kg. The aroma component of the concentrate was analyzed in the same manner as in Example 1 and shown in Table 1 and FIG.

추출성분의 층 분리Layer Separation of Extracts

상기 오리엔트 농축액 5.69㎏에 28% NH4OH를 가하여 pH를 9.5로 맞춘 후, 11.4㎏의 n-헥산을 가하여 30분간 교반하고 6시간 정치한 후에 헥산층과 물층으로 1차 층 분리를 행한다. 다음 물층에 다시 8.6㎏의 n-헥산을 가하고 30분간 교반하여 18시간 정치한 후, 2차 층 분리를 행하여 헥산층 합계 20㎏과 물층 6.0㎏을 분리하였다.After adding 28% NH 4 OH to 5.69 kg of the orient concentrate solution to adjust the pH to 9.5, 11.4 kg of n-hexane was added thereto, stirred for 30 minutes, and allowed to stand for 6 hours, followed by primary layer separation with a hexane layer and a water layer. Next, 8.6 kg of n-hexane was further added to the water layer, stirred for 30 minutes, and allowed to stand for 18 hours. Secondary layer separation was performed to separate 20 kg of the hexane layer and 6.0 kg of the water layer.

풍미성분의 제조Preparation of Flavor Ingredients

상기 층 분리로 얻어진 물층 6.0㎏에 고과당 0.9㎏과 푸로필렌글리콜 0.9㎏, 알라닌 0.12㎏을 가하고 80℃로 2시간 열처리하여 비효소적 갈변반응을 진행시켜서 풍미성분 6.96㎏을 얻었다. 열처리로 변환된 피라진계 성분의 함량분석은 실시예 1과 동일한 방법으로 분석하고, 그 결과는 표 2 및 도 6에 나타내었다.0.9 kg of high fructose, 0.9 kg of furophilene glycol, and 0.12 kg of alanine were added to 6.0 kg of the water layer obtained by the above-mentioned layer separation, and heat treatment was performed at 80 ° C. for 2 hours to give a non-enzymatic browning reaction to obtain a flavor component of 6.96 kg. Content analysis of pyrazine-based components converted to heat treatment was analyzed in the same manner as in Example 1, and the results are shown in Table 2 and FIG. 6.

오리엔트 향 추출성분의 제조Preparation of Orient Fragrance Extract

상기 층 분리된 헥산층 20㎏을 1/2로 농축하고, 여기에 1.5㎏의 젖산과 7㎏의 물을 가하여 15분간 교반한다. 2시간 정치시켜 니코틴이 함유된 물층을 제거하고, 다시 1㎏의 젖산과 7㎏의 물을 가하고 위 과정을 반복하여 물층을 제거한 후, 이번에는 같은 량의 물만을 가하여 위 과정을 반복하고 물을 완전히 제거하여 헥산층을 취하였다. 이렇게 얻어진 헥산 10㎏을 1/3로 농축하고 3.3㎏의 95% 에탄올을가하여 30분간 교반한 후, 에탄올층을 층 분리하고 1/4로 농축하여 오리엔트 향 추출성분 0.83㎏을 얻었다.20 kg of the separated hexane layer is concentrated to 1/2, and 1.5 kg of lactic acid and 7 kg of water are added thereto, followed by stirring for 15 minutes. After standing for 2 hours, the nicotine-containing water layer was removed, and 1 kg of lactic acid and 7 kg of water were added again, and the above process was repeated to remove the water layer. This time, only the same amount of water was added and the water was repeated. The hexane layer was taken by complete removal. 10 kg of hexane thus obtained was concentrated to 1/3, and 3.3 kg of 95% ethanol was added thereto, followed by stirring for 30 minutes. The ethanol layer was separated and concentrated to 1/4 to obtain 0.83 kg of orient extract component.

오리엔트 담배 가향료의 조합Orient Tobacco Flavor Combination

상기 비효소적 갈변반응으로 얻어진 풍미성분 6.96㎏과 상기 오리엔트 향 추출성분 0.83㎏을 배합하여 오리엔트 담배 가향료 7.79㎏을 제조하였다.6.79 kg of the flavor component obtained by the non-enzymatic browning reaction and 0.83 kg of the orient flavor extract component were combined to prepare 7.79 kg of orient tobacco flavoring agent.

[비교예 1]Comparative Example 1

오리엔트 농축액의 제조Preparation of Orient Concentrate

용매순환식 추출기에 오리엔트엽(바스마종) 스크랩 10㎏과 80% 에탄올 160㎏을 넣고 40℃에서 18시간동안 추출하였다. 추출물을 바스켓필터로 여과한 후, 여액은 다시 1㎛ 필터로 여과하고, 잔사는 착즙하여 폐기하고, 즙액은 1㎛ 필터로 여과하여 상기 여액과 혼합 한 후, 45℃에서 브릭스 농도 65°가 될 때까지 감압 농축하였다. 얻어진 오리엔트 농축액은 4.14㎏ 이었다. 실시예 1과 같은 방법으로 성분분석을 하여 표 1 및 도 3에 나타내었다.10 kg of orient leaf (Basma species) scrap and 80 kg of ethanol 160 kg were put into a solvent cyclic extractor and extracted at 40 ° C. for 18 hours. After the extract was filtered with a basket filter, the filtrate was again filtered through a 1 μm filter, the residue was juiced and discarded, and the juice solution was filtered with a 1 μm filter and mixed with the filtrate, followed by brix concentration at 65 °. Concentrated under reduced pressure until. The obtained orient concentrate was 4.14 kg. Analysis of the components in the same manner as in Example 1 is shown in Table 1 and FIG.

추출성분의 층 분리Layer Separation of Extracts

상기 오리엔트 농축액 4.14㎏에 28% NH4OH를 가하여 pH를 9.5로 맞춘 후, 8.3㎏의 n-헥산을 가하여 30분간 교반하고 6시간 정치한 후에 헥산층과 물층으로 1차 층 분리를 행한다. 다음 물층에 다시 6.2㎏의 n-헥산을 가하고 30분간 교반하여 18시간 정치한 후, 2차 층 분리를 행하여 헥산층 14.5㎏과 물층 4.5㎏을 분리하였다.After adding 28% NH 4 OH to 4.14 kg of the orient concentrate solution to adjust the pH to 9.5, 8.3 kg of n-hexane was added thereto, stirred for 30 minutes, and allowed to stand for 6 hours, followed by primary layer separation with a hexane layer and a water layer. Next, 6.2 kg of n-hexane was further added to the water layer, stirred for 30 minutes, and allowed to stand for 18 hours. Then, secondary layer separation was performed to separate 14.5 kg of hexane layer and 4.5 kg of water layer.

풍미성분의 제조Preparation of Flavor Ingredients

상기 층 분리로 얻어진 물층 4.5㎏에 고과당 0.67㎏과 푸로필렌글리콜 0.67㎏, 알라닌 0.1㎏을 가하고 80℃로 2시간 열처리하여 비효소적 갈변반응을 진행시켜서 풍미성분 5.22㎏을 얻었다. 열처리로 변환된 피라진계 성분의 함량분석은 GC/MS법으로 분석하였다. 분석결과는 표 2 및 도 7에 나타내었다.0.67 kg of high fructose, 0.67 kg of furophilene glycol, and 0.1 kg of alanine were added to 4.5 kg of the water layer obtained by the above-mentioned layer separation, and heat treatment was performed at 80 ° C. for 2 hours to obtain a non-enzymatic browning reaction to obtain a flavor component of 5.22 kg. The content analysis of pyrazine-based components converted to heat treatment was analyzed by GC / MS method. The analysis results are shown in Table 2 and FIG.

오리엔트 향 추출성분의 제조Preparation of Orient Fragrance Extract

상기 1차와 2차 층 분리된 헥산층을 혼합하여 1/2로 농축하고, 여기에 1.45㎏의 젖산과 5.8㎏의 물을 가하여 15분간 교반한다. 2시간 정치시켜 니코틴이 함유된 물층을 제거하고, 다시 1.1㎏의 젖산과 5.8㎏의 물을 가하고 위 과정을 반복하여 물층을 제거한 후, 이번에는 같은 량의 물만을 가하여 위 과정을 반복하고 물을 완전히 제거하여 헥산층을 취하였다. 이렇게 얻어진 헥산 7.25㎏을 1/3로 농축시키고 2.4㎏의 95% 에탄올을 가하여 30분간 교반한 후, 에탄올층을 분리하고 1/4로 농축하여 오리엔트 향 추출성분 0.6㎏을 얻었다.The hexane layer separated from the primary and secondary layers were mixed and concentrated to 1/2, and then 1.45 kg of lactic acid and 5.8 kg of water were added thereto, followed by stirring for 15 minutes. After standing for 2 hours, the nicotine-containing water layer was removed, and 1.1 kg of lactic acid and 5.8 kg of water were added again and the above process was repeated to remove the water layer. This time, only the same amount of water was added and the water was repeated. The hexane layer was taken by complete removal. 7.25 kg of hexane thus obtained was concentrated to 1/3, 2.4 kg of 95% ethanol was added thereto, stirred for 30 minutes, the ethanol layer was separated and concentrated to 1/4 to obtain 0.6 kg of orient extract component.

오리엔트 담배 가향료의 조합Orient Tobacco Flavor Combination

상기 비효소적 갈변반응으로 얻은 풍미성분 5.22㎏과 상기 오리엔트 향 추출성분 0.6㎏을 배합하여 오리엔트 담배 가향료 5.82㎏을 제조하였다.5.22 kg of the flavor component obtained by the non-enzymatic browning reaction and 0.6 kg of the orient flavor extract component were combined to prepare 5.82 kg of orient tobacco flavoring agent.

[비교예 2]Comparative Example 2

오리엔트 농축액의 제조Preparation of Orient Concentrate

용매순환식 추출기에 오리엔트엽(바스마종) 스크랩 10㎏과 50% 에탄올 160㎏을 넣고 40℃에서 18시간동안 추출하였다. 추출물을 바스켓필터로 여과하여 잔사는 착즙한 후 폐기하고, 여액과 즙액은 혼합하여 1㎛ 필터로 여과하고, 45℃에서 브릭스 농도 65°가 될 때까지 감압 농축하여 오리엔트 농축액 5.82㎏을 얻었다. 실시예 1과 같은 방법으로 향기성분을 분석하고 표 1 및 도 4에 나타내었다.10 kg of orient leaf (Basma species) and 160 kg of 50% ethanol were added to a solvent-circulating extractor, and extracted at 40 ° C. for 18 hours. The extract was filtered with a basket filter and the residue was juiced and discarded. The filtrate and juice were mixed, filtered with a 1 μm filter, and concentrated under reduced pressure at 45 ° C. until the brick concentration reached 65 ° to obtain 5.82 kg of orient concentrate. The fragrance components were analyzed in the same manner as in Example 1 and shown in Table 1 and FIG. 4.

추출성분의 층 분리Layer Separation of Extracts

상기 오리엔트 농축액 5.82㎏에 28% NH4OH를 가하여 pH를 9.5로 맞춘 후, 12㎏의 n-헥산을 가하여 30분간 교반하고 6시간 정치한 후에 헥산층과 물층으로 1차 층 분리를 행한다. 다음 물층에 다시 10㎏의 n-헥산을 가하고 30분간 교반하여 18시간 정치한 후, 2차 층 분리를 행하여 헥산층 22㎏과 물층 6.3㎏을 분리하였다.After adding 28% NH 4 OH to 5.82 kg of the orient concentrate, the pH was adjusted to 9.5, 12 kg of n-hexane was added thereto, stirred for 30 minutes, and allowed to stand for 6 hours, followed by primary layer separation with a hexane layer and a water layer. Next, 10 kg of n-hexane was further added to the water layer, stirred for 30 minutes, and allowed to stand for 18 hours. Then, secondary layer separation was performed to separate 22 kg of the hexane layer and 6.3 kg of the water layer.

풍미성분의 제조Preparation of Flavor Ingredients

상기 층 분리로 얻어진 물층 6.3㎏에 고과당 0.95㎏과 푸로필렌글리콜 0.95㎏, 글리신 0.13㎏을 가하고 90℃로 2시간 열처리하여 비효소적 갈변반응을 진행시켜서 풍미성분 7.3㎏을 얻었다. 열처리로 변환된 피라진계 성분의 함량분석은 GC/MS법으로 분석하였다. 분석결과는 표 2 및 도 8에 나타내었다.0.95 kg of high fructose, 0.95 kg of furophilene glycol, and 0.13 kg of glycine were added to 6.3 kg of the water layer obtained by separating the layers, and the resultant was heat-treated at 90 ° C. for 2 hours to give a non-enzymatic browning reaction to obtain 7.3 kg of flavor component. The content analysis of pyrazine-based components converted to heat treatment was analyzed by GC / MS method. The analysis results are shown in Table 2 and FIG. 8.

오리엔트 향 추출성분의 제조Preparation of Orient Fragrance Extract

상기 1차와 2차 층 분리된 헥산층을 혼합하여 1/2로 농축하고, 여기에 2.2㎏의 빙초산과 8.8㎏의 물을 가하여 15분간 교반한다. 2시간 정치시켜 니코틴이 함유된 물층을 제거하고, 다시 1.65㎏의 젖산과 8.8㎏의 물을 가하고 위 과정을 반복하여 물층을 제거한 후, 이번에는 같은 량의 물만을 가하여 위 과정을 반복하고 물을 완전히 제거하여 헥산층을 취하였다. 이렇게 얻어진 헥산 11㎏을 1/3로 농축시키고 3.6㎏의 95% 에탄올을 가하여 30분간 교반한 후, 에탄올층을 분리하고 1/4로 농축하여 오리엔트 향 추출성분 0.9㎏을 얻었다.The hexane layer separated from the primary and secondary layers was mixed and concentrated to 1/2, and then stirred for 15 minutes by adding 2.2 kg of glacial acetic acid and 8.8 kg of water. After standing for 2 hours, the nicotine-containing water layer was removed. Then, 1.65 kg of lactic acid and 8.8 kg of water were added. The above process was repeated to remove the water layer. This time, only the same amount of water was added and the water was repeated. The hexane layer was taken by complete removal. 11 kg of hexane thus obtained was concentrated to 1/3, 3.6 kg of 95% ethanol was added thereto, stirred for 30 minutes, the ethanol layer was separated, and concentrated to 1/4 to obtain 0.9 kg of orient extract component.

오리엔트 담배 가향료의 조합Orient Tobacco Flavor Combination

상기 비효소적 갈변반응으로 얻어진 풍미성분 7.3㎏과 오리엔트 향 추출성분 0.9㎏을 배합하여 오리엔트 담배 가향료 8.2㎏을 제조하였다.Orient tobacco flavoring agent 8.2kg was prepared by combining 7.3kg of the flavor component obtained by the non-enzymatic browning reaction and 0.9kg of the orient flavor extract component.

단위: % (피크 에리어)Unit:% (peak area) 피크번호Peak number 성 분ingredient 실시예 1Example 1 실시예 2Example 2 비교예 1Comparative Example 1 비교예 2Comparative Example 2 1One 아세트산Acetic acid 0.0610.061 0.0450.045 0.0590.059 0.0340.034 22 3-메틸-부틸산3-Methyl-butyl acid 0.0690.069 0.0500.050 0.0610.061 0.0120.012 33 솔라논Solanone 0.0320.032 0.0240.024 0.0300.030 0.0110.011 44 3-메틸-바레르산3-methyl-bareric acid 0.1770.177 0.1560.156 0.1590.159 0.0220.022 55 니코틴nicotine 0.1700.170 0.1450.145 0.1810.181 0.1120.112 66 네오피타디엔Neophytadiene 0.2270.227 0.1800.180 0.2470.247 -- 2+3+4+62 + 3 + 4 + 6 향기성분 합계Fragrance component total 0.5050.505 0.4100.410 0.4970.497 0.0450.045 농축액 수율(%)Concentrate yield (%) 56.856.8 56.956.9 41.341.3 58.258.2

단위: % (함량)Unit:% (Content) 피크번호Peak number 성 분ingredient 실시예 1Example 1 실시예 2Example 2 비교예 1Comparative Example 1 비교예 2Comparative Example 2 1One 에틸아세테이트Ethyl acetate 0.320.32 0.170.17 0.220.22 0.340.34 22 이소프로필알콜Isopropyl Alcohol 0.250.25 0.040.04 0.040.04 0.160.16 33 2-에톡시부탄2-ethoxybutane 0.200.20 0.140.14 0.120.12 -- 44 메틸피라진Methylpyrazine 0.180.18 0.810.81 0.440.44 1.341.34 55 2,5-디메틸피라진2,5-dimethylpyrazine 0.200.20 0.170.17 0.120.12 0.180.18 66 2,6-디메틸피라진2,6-dimethylpyrazine 1.541.54 1.161.16 0.620.62 1.341.34 77 에틸피라진Ethylpyrazine 0.200.20 0.100.10 0.100.10 0.220.22 88 2,3-디메틸피라진2,3-dimethylpyrazine 0.250.25 0.170.17 0.060.06 0.200.20 99 2-에틸-6-메틸피라진2-ethyl-6-methylpyrazine 0.130.13 0.100.10 0.100.10 -- 1010 트리메틸피라진Trimethylpyrazine -- -- 0.160.16 0.280.28 1111 2-메틸-6-비닐피라진2-methyl-6-vinylpyrazine -- -- 0.240.24 -- 피라진 합계Pyrazine sum 3.503.50 2.512.51 1.841.84 3.563.56 1212 카베올Cabero -- -- -- 0.130.13 3131 시스-3-헥세놀Cis-3-hexenol -- -- -- 0.080.08

상기 표 1로 확인할 수 있는 바와 같이 추출용매인 에탄올의 농도가 높을수록 오리엔트 향성분이 많이 추출되고, 농축액의 수율은 적으며 피라진계 물질의 생성량도 적은 것을 알 수 있다.As can be seen in Table 1, the higher the concentration of the ethanol as the extraction solvent, the more orient fragrance components are extracted, the yield of the concentrate is small, and the amount of pyrazine-based material is also produced.

황색엽 1∼3등급 47%, 버어리엽 1∼2등급 15%, 판상엽 8%, 팽화주맥 15%, 팽화각초 15%로 엽조(오리엔트엽은 배합안함)를 배합한 후, 0.9㎜로 절각하고 상기 각 실시예의 오리엔트 담배 가향료를 가향하여 궐련을 제조하였다. 이와 같이 제조한 궐련 담배는 패널테스트로 끽미를 조사하여 그 결과를 표 3에 나타내었다. 패널리스트는 모두 10명으로, 각 실시예 및 비교예 담배를 한 개비씩 피우게 하고 향 및 맛을 종합적으로 비교하여 가장 좋은 것은 1점, 가장 싫은 것은 4점으로 하여 순위를 정하도록 하였다.Yellow leaf 1 ~ 3 grade 47%, Burley leaf 1 ~ 2 grade 15%, lamellar leaf 8%, puffed vein 15%, puffed kelp 15% A cigarette was prepared by cutting and flavoring the orient tobacco flavor of each of the above examples. Cigarette tobacco prepared as described above was examined by taste in a panel test, the results are shown in Table 3. The panelists were all ten, and each example and a comparative example cigarettes were smoked one by one, and the aroma and taste were compared comprehensively, and the best was one point and the most unpleasant four points were ranked.

시료품 패널원Sample Panel 실시예 1Example 1 실시예 2Example 2 비교예 1Comparative Example 1 비교예 2Comparative Example 2 P1P1 1One 22 44 33 P2P2 1One 22 33 44 P3P3 22 1One 44 33 P4P4 1One 22 33 44 P5P5 1One 33 44 22 P6P6 1One 22 44 33 P7P7 22 1One 44 33 P8P8 1One 22 33 44 P9P9 22 1One 33 44 P10P10 22 1One 44 33 합 계Sum 1414 1717 3636 3333

표 3의 관능검사 테스트로 알 수 있는 바와 같이 본 발명의 용매농도를 달리하여 다단계로 추출한 향료는 종래의 단순 추출향료에 비해 오리엔트 향이 풍부하고 순한 담배의 향취미와 맛을 느낄 수 있게 해준다.As can be seen from the sensory test of Table 3, the perfume extracted in multiple stages by varying the solvent concentration of the present invention is richer in the orient than the conventional simple extract, and allows you to feel the taste and taste of mild tobacco.

Claims (5)

오리엔트엽을 용매추출로 제조한 담배 가향료에 있어서, 오리엔트엽을 1단계로 70∼80%의 에탄올 또는 이소푸로필알콜로 추출하고, 2단계로 50%의 에탄올 또는 이소푸로필알콜로 추출하여 여과하고, 그 여액에 알카리를 가하여 pH를 9.5로 맞춘 후에 유기용제를 사용하여 향 추출성분과 풍미성분으로 분획한 후, 상기 풍미성분에는 당과 아미노산을 가하여 비효소적 갈변반응을 시키고, 상기 향 추출성분에는 빙초산 또는 젖산과 물을 가하여 교반하고 정치하여 물층을 제거함으로써 니코틴을 제거한 다음, 상기 갈변반응을 시킨 풍미성분과 니코틴을 제거한 향 추출성분을 혼합하여서 된 오리엔트 담배 가향료.Tobacco flavors prepared by solvent extraction of the orient leaf, the orient leaf is extracted with 70-80% of ethanol or isoprophyl alcohol in one step, and extracted with 50% of ethanol or isoprophyl alcohol in two steps Filtration was added to the filtrate, the pH was adjusted to 9.5, and then fractionated into flavor extract and flavor component using an organic solvent. The flavor component was added with sugar and amino acid to undergo a non-enzymatic browning reaction. Orient tobacco flavoring agent by adding the glacial acetic acid or lactic acid and water, stirring and standing to remove the water layer to remove the nicotine, and then mixing the flavor component subjected to the browning reaction and the flavor extraction component to remove nicotine. 제1항에 있어서, 상기 당성분은 고과당이고, 아미노산성분은 글리신, 알라닌, 발린 중에서 선택한 하나임을 특징으로 하는 오리엔트 담배 가향료.The orient tobacco flavoring agent of claim 1, wherein the sugar component is high fructose and the amino acid component is one selected from glycine, alanine, and valine. 오리엔트엽을 알콜로 추출함에 있어서,In extracting the orient leaf with alcohol, (가) 오리엔트엽 스크랩(scrap)에 1단계로 중량기준 8∼10배의 70∼80% 에탄올 또는 이소푸로필알콜을 가하여 40∼50℃에서 9∼14시간동안 가열 용매순환식으로 추출하고, 이 추출물을 바스켓필터를 사용하여 전처리여과를 한 후, 다시 1㎛ 필터로 여과하여 여액과 잔사를 분리하는 공정;(A) To the orient leaf scrap, add 8 to 10 times 70 to 80% ethanol or isoprophyl alcohol on a weight basis in one step and extract by heating solvent circulation at 40 to 50 ℃ for 9 to 14 hours. Pretreatment of the extract with a basket filter, followed by filtration with a 1 μm filter to separate the filtrate and the residue; (나) 2단계로 잔사에 다시 6∼8배의 50% 에탄올 또는 이소푸로필알콜을 가하여 40∼50℃에서 4∼7시간동안 가열 용매순환식으로 추출하고, 이 추출물을 바스켓필터를 사용하여 전처리여과를 한 후, 다시 1㎛ 필터로 여과하여 여액과 잔사를 분리하는 공정;(B) Add 6-8 times 50% ethanol or isoprophyl alcohol to the residue in two steps and extract by heating solvent circulation for 4-7 hours at 40-50 ℃, and extract this extract using a basket filter. After pre-filtering, filtering with a 1 μm filter to separate the filtrate and the residue; (다) 상기 2단계 잔사를 착즙하여 잔사는 폐기한 후, 즙액은 1㎛ 필터로 여과하고 이 여액을 상기 1단계 및 2단계 여액과 혼합하여 45℃에서 브릭스 60∼65°가 되도록 진공 농축하여 농축액을 제조하는 공정;(C) After extracting the second step residue and discarding the residue, the juice solution is filtered with a 1㎛ filter and the filtrate is mixed with the first and second step filtrate and concentrated in vacuo at 45 ℃ to 60 ~ 65 ° brix Preparing a concentrate; (라) 상기 농축액에 알카리를 가하여 pH를 9.5로 맞춘 후에 농축액의 2배에 해당하는 n-헥산을 가하여 30∼60분간 교반하고 6∼8시간 정치한 후, 헥산층과 물층으로 1차 층 분리를 행하는 공정;(D) add alkali to the concentrate to adjust the pH to 9.5, add n-hexane corresponding to twice the concentrate, stir for 30 to 60 minutes, allow to stand for 6 to 8 hours, and separate the primary layer into a hexane layer and a water layer. Performing a step; (마) 상기 물층에 다시 1.5배의 n-헥산을 가하고 30∼60분간 교반하여 18∼30시간 정치한 후, 2차 층 분리를 행하여 헥산층과 물층으로 분리하는 공정;(E) adding 1.5-fold n-hexane to the water layer again, stirring for 30 to 60 minutes, allowing to stand for 18 to 30 hours, and then separating the second layer into a hexane layer and a water layer; (바) 상기 물층에 대해 고과당 15중량%와 푸로필렌글리콜 15중량% 및 글리신, 알라닌, 발린 중에서 선택된 1가지 성분 2중량%를 첨가한 다음, 80∼90℃에서 2시간 이상 비효소적 갈변반응을 진행시켜 피라진(Pyrazin)계 풍미성분으로 변환시키는 공정;(F) 15% by weight of high fructose, 15% by weight of furofylene glycol and 2% by weight of one component selected from glycine, alanine, and valine were added to the water layer, followed by non-enzymatic browning at 80 to 90 ° C for at least 2 hours. Advancing the reaction to convert the pyrazin-based flavor component; (사) 상기 (라), (마)항에서 1차, 2차 층 분리된 헥산층을 혼합하고 1/2로 농축한 후, 농축액의 15∼20중량%에 해당하는 빙초산 또는 젖산 및 농축액의 70∼80중량%에 해당하는 물을 가하고 10∼15분간 교반한 후, 1∼2시간 정치시켜 니코틴이 함유된 물층은 제거하고, 재차 농축액의 10∼15중량%에 해당하는 빙초산 또는 젖산 및 농축액의 70∼80중량%에 해당하는 물을 가하고 10∼15분간 교반한 후,1∼2시간 정치시켜 물층은 제거한 다음, 여기에 같은 량의 물만을 가하고 다시 10∼15분간 교반한 후, 2∼3시간 정치시켜 물층은 제거하고 향기성분이 함유된 헥산층을 얻고, 상기 헥산층을 1/3로 농축시켜 동일 량의 95% 에탄올을 가하고 30분간 교반한 후, 에탄올 층을 분리하고 1/4로 농축하여 향 추출성분을 만드는 공정;(G) After mixing the hexane layer separated in the primary and secondary layers in (d) and (d) above and concentrating to 1/2, the amount of glacial acetic acid or lactic acid and the concentrated liquid corresponding to 15-20% by weight of the concentrated liquid 70 to 80% by weight of water was added and stirred for 10 to 15 minutes, and then allowed to stand for 1 to 2 hours to remove the water layer containing nicotine, and again to 10 to 15% by weight of glacial acetic acid or lactic acid and concentrate After adding water corresponding to 70 to 80% by weight of the solution and stirring for 10 to 15 minutes, allowing to stand for 1 to 2 hours to remove the water layer, and then adding the same amount of water only and stirring for another 10 to 15 minutes, then 2 to After standing for 3 hours, the water layer was removed to obtain a hexane layer containing fragrance components. The hexane layer was concentrated to 1/3, the same amount of 95% ethanol was added and stirred for 30 minutes. Making a fragrance extract component by concentrating with; (아) 상기 피라진계 풍미성분을 함유하는 (바)항의 풍미성분과 상기 (사)항의 농축 향 추출성분을 배합하여 오리엔트 담배 가향료를 제조하는 공정으로 구성됨을 특징으로 하는 오리엔트 담배 가향료의 제조방법.(H) preparation of an orient tobacco flavoring agent, comprising the step of mixing the flavor component of (bar) containing the pyrazine-based flavoring component with the concentrated flavor extract component of the item (g); Way. 제 3항에 있어서, 알카리가 수산화암모늄, 수산화칼륨 중에서 선택한 하나임을 특징으로 하는 오리엔트 담배 가향료의 제조방법.4. The method of claim 3, wherein the alkali is one selected from ammonium hydroxide and potassium hydroxide. 제 3항에 있어서, 상기 알콜이 에탄올임을 특징으로 하는 오리엔트 담배 가향료의 제조방법.4. The method of claim 3, wherein the alcohol is ethanol.
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