KR100883711B1 - Tobacco material, flavoring agent, and regenerated tobacco material, reduced in stimulus and pungency in the smoking stage, method of preparing tobacco material and method of preparing flavoring agent - Google Patents

Tobacco material, flavoring agent, and regenerated tobacco material, reduced in stimulus and pungency in the smoking stage, method of preparing tobacco material and method of preparing flavoring agent Download PDF

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KR100883711B1
KR100883711B1 KR1020077010688A KR20077010688A KR100883711B1 KR 100883711 B1 KR100883711 B1 KR 100883711B1 KR 1020077010688 A KR1020077010688 A KR 1020077010688A KR 20077010688 A KR20077010688 A KR 20077010688A KR 100883711 B1 KR100883711 B1 KR 100883711B1
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tobacco
tobacco material
flavoring agent
causative
daltons
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KR20070064367A (en
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마사타카 모리
켄지 이토
요시유키 야마다
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니뽄 다바코 산교 가부시키가이샤
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/12Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/14Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products

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Abstract

담배재료는, 착색 산성 수용성 고분자 물질의 함유율을 감소시키는 것에 의해 흡연시의 자극ㆍ매운 맛을 저감시킨 것이다.

Figure R1020077010688

Tobacco material reduces the irritation and spicy taste at the time of smoking by reducing the content rate of coloring acidic water-soluble high molecular substance.

Figure R1020077010688

Description

흡연시의 자극ㆍ매운 맛을 저감시킨 담배재료, 향끽미제, 재생 담배재료, 담배재료의 제조방법, 및 향끽미제의 제조방법{TOBACCO MATERIAL, FLAVORING AGENT, AND REGENERATED TOBACCO MATERIAL, REDUCED IN STIMULUS AND PUNGENCY IN THE SMOKING STAGE, METHOD OF PREPARING TOBACCO MATERIAL AND METHOD OF PREPARING FLAVORING AGENT}TOBACCO MATERIAL, FLAVORING AGENT, AND REGENERATED TOBACCO MATERIAL, REDUCED IN STIMULUS AND PUNGENCY IN THE SMOKING STAGE, METHOD OF PREPARING TOBACCO MATERIAL AND METHOD OF PREPARING FLAVORING AGENT}

본 발명은, 담배의 향끽미 개선의 분야에 관한 것으로서, 상세하게는, 흡연시의 자극ㆍ매운 맛을 저감시킨 담배재료, 향끽미제, 재생 담배재료, 담배재료의 제조방법, 및 향끽미제의 제조방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the field of improving the taste of tobacco, and in particular, a tobacco material, a flavoring agent, a regenerated tobacco material, a method for producing a tobacco material, and a flavoring agent, which have reduced irritation and spicy taste during smoking. It is about a method.

천연 담배재료는, 자극ㆍ매운 맛 등의 불필요한 끽미를 나타내고, 특히 벌리(Burley)종 담배는, 자극ㆍ매운 맛 등의 불필요한 끽미 특징이 강하기 때문에, 종래 여러가지 향료 첨가나 가열 처리 등에 의해 끽미를 개선하는 것이 행하여져 왔다. 그러나, 이와 같은 불필요 끽미의 원인에 관하여는 아직 그 상세한 것은 해명되어 있지 않고, 종래의 끽미개선을 위한 향료기술이나 처리방법은 경험에 근거하는 것이며, 효율이나 비용의 점에서 문제가 있었다(Tobacco Reporter, July 2003, pp.64-70 참조).Natural tobacco material exhibits unwanted tastes such as irritation and spicy taste, and in particular, Burley cigarettes have strong taste characteristics such as irritation and spicy taste. What has been done has been done. However, the details of the cause of such unwanted tastes have not been elucidated yet. Conventional flavoring techniques and treatment methods for improving tastes are based on experience and have problems in terms of efficiency and cost (Tobacco Reporter , July 2003, pp. 64-70).

따라서, 천연 담배재료, 특히 벌리종 담배중의 자극ㆍ매운 맛의 원인성분을 화학적으로 해명할 수 있으면, 그 적확한 저감 처리에 의해, 천연 담배재료의 향끽미를 효율적으로 개선하는 것이 가능하게 된다고 생각된다.Therefore, if the causative ingredient of the irritating and spicy taste in natural tobacco material, especially Burley tobacco, can be chemically clarified, it is possible to efficiently improve the flavor of natural tobacco material by the precise reduction treatment. I think.

발명의 개시Disclosure of the Invention

그래서, 본 발명에서는, 천연 담배재료, 특히 벌리종 담배 중의 자극ㆍ매운 맛의 원인성분을 화학적으로 해명하는 것에 의해, 그 물리적ㆍ화학적 성질에 의거한 형으로 자극ㆍ매운 맛의 원인성분을 저감하고, 또한 천연 담배재료의 향끽미를 개선하는 수단을 제공하는 것을 목적으로 한다.Therefore, in the present invention, by chemically clarifying the causative ingredient of irritation and spicy taste in natural tobacco material, especially Burley tobacco, the causative ingredient of irritation and spicy taste is reduced in a form based on its physical and chemical properties. It is also an object of the present invention to provide a means for improving the flavor of natural tobacco ingredients.

본 발명자들은, 벌리종 담배의 물 추출액을 각종 크로마토그래피 수법에 의해 분획하고, 각 분획을 이용하여 궐련을 제작하고, 관능평가에 의해 자극ㆍ매운 맛이 발현되는 것을 지표로 하여 자극ㆍ매운 맛의 원인성분의 정제를 행하였다. 그 결과, 자극ㆍ매운 맛의 원인성분(이하, 「본 원인성분」이라 한다)이 물 추출액 중에 포함되는 착색 산성 수용성 고분자 물질인 것을 분명하게 하였다. 이 분획정제의 과정에서, 본 원인성분의 저감법의 개발에 관한 물리적ㆍ화학적 성질이 분명하게 되었다. 또, 본 원인성분은, 불휘발성이기 때문에, 직접의 자극ㆍ매운 맛 성분이 아니라, 흡연시에 자극ㆍ매운 맛 성분을 발생하는 전구체 성분이라 생각된다. 본 발명은 이들의 지견에 근거한다.The inventors of the present invention fractionated Burley's tobacco water extract by various chromatographic techniques, produced cigarettes using each fraction, and expressed the stimulus and the pungent taste as an indicator that the irritation and spicy taste were expressed by sensory evaluation. The causative component was purified. As a result, it became clear that the causative component of the irritation and pungent taste (hereinafter, referred to as "the present causal component") is a colored acidic water-soluble high molecular substance contained in the water extract. In the course of fractional purification, the physical and chemical properties of the development of the method for reducing the causative agent became clear. In addition, since the causative component is nonvolatile, it is considered that it is not a direct irritation / taste component, but a precursor component which generates a irritation / taste component when smoking. The present invention is based on these findings.

즉, 본 발명의 제 1의 측면에 의하면, 착색 산성 수용성 고분자 물질의 함유율을 감소시키는 것에 의해 흡연시의 자극ㆍ매운 맛을 저감시킨 것을 특징으로 하는 담배재료가 제공된다.That is, according to the 1st aspect of this invention, the tobacco material characterized by reducing the irritation and spicy taste at the time of smoking by reducing the content rate of a coloring acidic water-soluble high molecular substance is provided.

본 발명의 제 2의 측면에 의하면, 착색 산성 수용성 고분자 물질의 함유율을 감소시키는 것에 의해 자극ㆍ매운 맛 원인성분을 저감시킨 담배 추출액을 포함하는 것을 특징으로 하는 담배 향끽미제가 제공된다.According to the second aspect of the present invention, there is provided a tobacco flavoring agent comprising a tobacco extract having reduced irritation and spicy taste cause components by reducing the content of the colored acidic water-soluble high molecular substance.

본 발명의 제 3의 측면에 의하면, 천연 담배재료로부터의 수계 추출액을 포함하는 향끽미제를 천연 담배재료의 추출 잔사인 섬유를 포함하는 재생 담배 웹(web)에 첨가하여 이루어지는 재생 담배재료가며, 상기 향끽미제가 본 발명의 향끽미제인 것을 특징으로 하는 재생 담배재료가 제공된다.According to a third aspect of the present invention, there is provided a regenerated tobacco material formed by adding a flavoring agent comprising an aqueous extract from a natural tobacco material to a regenerated tobacco web comprising fibers which are the extraction residues of the natural tobacco material. A recycled tobacco material is provided, wherein the flavoring agent is the flavoring agent of the present invention.

본 발명의 제 4의 측면에 의하면, 착색 산성 수용성 고분자 물질을 저감시키는 것을 특징으로 하는 담배재료의 제조방법이 제공된다.According to the 4th aspect of this invention, the manufacturing method of the tobacco material characterized by reducing the coloring acidic water-soluble high molecular substance is provided.

또한, 본 발명의 제 5의 측면에 의하면, 천연 담배재료로부터의 수계 추출액으로 착색 산성 수용성 고분자 물질을 저감시키는 것을 특징으로 하는 향끽미제의 제조방법이 제공된다According to a fifth aspect of the present invention, there is provided a method for producing a flavoring agent, wherein the coloring acidic water-soluble high molecular substance is reduced with an aqueous extract from a natural tobacco material.

발명을 실시하기Implement the invention 위한 최선의 형태 Best form for

이하, 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.

본 발명에서는, 천연 담배재료, 특히 벌리종 담배재료의 자극ㆍ매운 맛의 원인성분을 화학적으로 해명하기 위하여, 벌리종 담배재료를 수계 용매에서 추출하여, 추출액을 획득했다. 추출 잔사는, 실질적으로 섬유로 이루어진다. 이 추출 잔사를 통상의 방법에 의해 슬러리화 하고, 초지(抄紙)하여 재생 웹 시트를 제작하고, 이것을 재각(裁刻)하여 재생 담배살을 얻었다.In the present invention, in order to chemically clarify the causative agent of irritating and spicy taste of natural tobacco material, especially Burley tobacco material, Burley tobacco material was extracted with an aqueous solvent to obtain an extract. The extraction residue consists essentially of fibers. This extraction residue was slurried by a conventional method, papermaking was carried out, a regenerated web sheet was produced, and it was re-cut to obtain regenerated tobacco flesh.

다른 한편, 상기 추출액을 분획 분자량 1만달톤(dalton)의 한외 여과막으로 처리하고, 분자량 1만달톤 미만의 분획과 분자량 1만달톤 이상의 분획을 얻었다. 분자량 1만달톤 미만의 분획을 농축하고, 상기 재생 담배살에 첨가하고, 이것을 이용하여 궐련을 제작했다. 이 궐련을 관능검사에 제공한 바, 추출액을 그대로 첨가한 재생 담배살을 이용하여 제작한 궐련에 대하여 자극ㆍ매운 맛이 거의 없는 점에서 끽미가 대폭 개선되었다는 평가를 얻었다. 이 결과로부터, 분자량 1만달톤 이상의 수용성 고분자 분획에 본 원인성분이 존재한다고 추정했다.On the other hand, the extract was treated with an ultrafiltration membrane having a fractional molecular weight of 10,000 daltons, and a fraction having a molecular weight of 10,000 Daltons and a molecular weight of 10,000 Daltons or more were obtained. Fractions having a molecular weight of less than 10,000 daltons were concentrated, added to the regenerated tobacco flesh, and a cigarette was prepared using this. When this cigarette was used for the sensory test, it was evaluated that the taste was greatly improved in that the cigarette produced using the regenerated tobacco flesh to which the extract was added as it had little irritation and spicy taste. From these results, it was estimated that this causative component exists in the water-soluble polymer fraction of molecular weight 10,000 Daltons or more.

그러나, 분자량 1만달톤 이상의 분획은, 대부분의 향끽미 성분(당, 아미노산, 배당체 등)이 제거되어 있기 때문에, 이것을 상기 재생 담배살에 첨가하여 제작한 궐련에서는 평가할 수 없다. 따라서, 별도 제작한 평가용 궐련에 분자량 1만달톤 이상의 고분자 분획을 첨가하고, 관능시험을 행하였다. 그 결과, 벌리종 같은 자극ㆍ매운 맛이 발현하여, 상기 추정을 뒷받침할 수 있었다.However, since most of the flavor components (sugars, amino acids, glycosides, etc.) have been removed, the fraction having a molecular weight of 10,000 Daltons or more cannot be evaluated in a cigarette produced by adding this to the regenerated tobacco flesh. Therefore, the polymer fraction of 10,000 Daltons or more of molecular weight was added to the evaluation cigarette produced separately, and the sensory test was done. As a result, irritation and spicy tastes, such as Burley species, were expressed, supporting the above estimation.

이상의 검토로부터, 이하의 각 정제 단계에서는, 각 분획에 관하여 분획 분자량 1만달톤의 한외 여과처리를 행하고, 분자량 1만달톤 이상의 성분에 관하여 평가했다.From the above examination, in each of the following purification steps, the ultrafiltration treatment of the fractional molecular weight 10,000 Daltons was performed about each fraction, and the component of molecular weight 10,000 Daltons or more was evaluated.

또한, 각 분획을 사용하여 이하 기술하는 평가용 궐련을 제작하고, 관능검사를 행하고, 자극ㆍ매운 맛의 발현을 지표로 하여 분획을 진행시켰다.In addition, using each fraction, the cigarette for evaluation described below was produced, the sensory test was carried out, and the fraction advanced by making the expression of a stimulus and a spicy taste into an index.

<분획의 관능평가 방법><Sensory Evaluation Method of Fractions>

10명의 전문 패널의 관능평가에 의해, 각 분획을 첨가한 평가용 궐련을, 정제수만을 첨가한 대조 궐련과 비교하여 자극ㆍ매운 맛이 발현될 것인가 여부를 평가했다. 평가용 궐련으로서는, 시판의 초저니코틴ㆍ타르제품(타르 1mg, 니코틴 0.1mg)의 향료 무첨가품을 이용했다. 이 궐련은 가향량에 대하여 끽미효과가 작은 경향이 있지만, 궐련 바로 그것의 끽미에의 영향이 거의 없고, 각 분획의 끽미효과의 판정에는 만족할 수 있는 결과를 얻고 있다. 각 분획의 첨가는, 벌리종 담배 원료 20g 유래의 분획을 1mL의 정제수에 녹이고, 그 10μL(원료 0.2g 유래의 분획에 상당)를 시린지에서 평가용 궐련에 주입하는 것에 의해 행하였다. 궐련 1개피당의 살 양은 약 0.6g이며, 각 분획의 첨가량은, 살의 약 3분의 1 양의 원료에 상당한다.The sensory evaluation of ten expert panelists evaluated whether the evaluation cigarette to which each fraction was added was expressed compared with the control cigarette which added only purified water, and whether the irritation and spicy taste were expressed. As the cigarette for evaluation, a perfume-free additive of a commercially available ultra low nicotine tar product (tar 1 mg, nicotine 0.1 mg) was used. This cigarette tends to have a small taste effect with respect to the amount of flavor. However, the cigarette has little effect on the taste of the cigarette, and a satisfactory result for judging the taste effect of each fraction is obtained. Each fraction was added by dissolving a fraction derived from 20 g of Burley's tobacco raw material into 1 mL of purified water and injecting 10 µL (corresponding to a fraction derived from 0.2 g of raw material) into a cigarette for evaluation in a syringe. The amount of flesh per cigarette is about 0.6 g, and the amount of each fraction added corresponds to about one-third of the amount of meat.

<분획정제의 예비적 검토><Preliminary Review of Fractional Tablets>

본 원인성분의 분획정제를 목적으로 하여, 여러가지 수용성 고분자의 분획정제 방법을 검토했다. 그러나, 분획조작에 의한 pH나 이온 강도의 변동에 의해 불용화나 수지 등으로의 불가역적인 흡착이 일어나기 때문에, 당초부터의 계통적인 분획는 곤란했다. 따라서, 각종 단위분획조작에서의 지견을 정리한 후, 단위분획법의 조합을 검토했다.For the purpose of fractional purification of the causative component, various purification methods for fractionation of water-soluble polymers were examined. However, since the irreversible adsorption to insolubilization, resin, etc. occurs by the change of pH and ionic strength by a fractionation operation, the systematic fraction from the beginning was difficult. Therefore, after gathering knowledge in various unit fractionation operations, a combination of unit fractionation methods was examined.

<단위분획조작에 있어서의 지견><Knowledge in Unit Fraction Operation>

(1) 본 원인성분은, 정제수보다도 염수 용액에 용해하기 쉽고, 또한 산성 조건하보다도 염기성 조건하 쪽이 용해하기 쉽다. 다만, 수용액의 염기성이 높으면, 반응ㆍ분해의 염려가 있기 때문에, 천연 담배 원료로부터의 추출에는, 약산성의 염(아세트산나트륨)의 수용액을 이용하기로 했다. 추출 온도는, 실온(약 25℃), 60℃, 90℃를 검토했지만, 실온에서의 추출 처리에 의해 얻어진 추출액이 가장 자극ㆍ매운 맛이 강했다.(1) This causative component is easier to dissolve in a brine solution than purified water, and is more easily dissolved under basic conditions than under acidic conditions. However, if the basicity of the aqueous solution is high, there is a risk of reaction and decomposition, so that an aqueous solution of a weakly acidic salt (sodium acetate) is used for extraction from the natural tobacco raw material. Although extraction temperature examined room temperature (about 25 degreeC), 60 degreeC, and 90 degreeC, the extract obtained by the extraction process at room temperature had the strongest and hot taste.

(2) 상기한 바와 같이, 분획 분자량 1만달톤의 한외 여과막에 의한 분획처리에 의해, 분자량 1만달톤 이상의 분획에 자극ㆍ매운 맛을 확인했다.(2) As mentioned above, the fractionation process by the ultrafiltration membrane of the fractional molecular weight 10,000 Daltons confirmed the irritation and spicy taste to the fraction of molecular weight 10,000 Daltons or more.

(3) 본 원인성분은, 다당류 등과 다르고, 역상계 수지에 흡착되어, 물/메탄올 등으로 용출된다.(3) The causative agent differs from polysaccharides and the like, and is adsorbed by a reverse phase resin and eluted with water / methanol or the like.

(4) 본 원인성분은, 디에틸아미노에틸셀룰로오스(DEAE셀룰로오스)와 같은 음이온 교환수지에 흡착되어, 산의 성질을 나타낸다.(4) The causative component is adsorbed by an anion exchange resin such as diethylaminoethyl cellulose (DEAE cellulose) to exhibit the properties of an acid.

(5) 단백질이나 다당류와 다르고, 메탄올/물(부피비 9/1) 혼합 용매에 의해 침전하지 않고, 이 혼합 용매의 가용부에 본 원인성분이 존재했다.(5) Different from proteins and polysaccharides, the causative component was present in the soluble portion of the mixed solvent without being precipitated by the methanol / water (volume ratio 9/1) mixed solvent.

(6) 담배 중의 대표적인 플라보노이드류는, 자극ㆍ매운 맛을 나타내지 않지만, 고분자와 회합하는 성질이 있고, 착색하고 있기 때문에, 방해 성분으로서 제거했다(폴리비닐피롤리돈 수지에의 흡착).(6) Representative flavonoids in tobacco did not exhibit irritation or pungent taste, but had a property of associating with a polymer and were colored, and thus removed as an interference component (adsorption to polyvinylpyrrolidone resin).

상기의 예비적 검토에 근거하여, 최선의 결과가 얻어진 분획정제 스킴을 이하에 상술한다.Based on the above preliminary examination, the fractionation scheme in which the best result is obtained is described in detail below.

<벌리종 담배 원료 중의 자극ㆍ매운 맛 원인성분의 분획정제 스킴><Refining Scheme of Irritating and Spicy Causing Ingredients in Burley Tobacco Ingredients>

벌리종 중골(잎꼭지, 잎의 굵은 지맥부)은 향기가 옅고, 자극ㆍ매운 맛이 현저하기 때문에 검토 대상으로 했다.Burley's middle bone (leaves, thick veins of leaves) had a light fragrance, and the irritation and spicy taste were remarkable.

벌리종 중골원료를 분쇄하고, 10배용의 0.1M 아세트산나트륨 수용액중에서 실온하 30분간 교반하는 것에 의해 추출을 행하였다. 추출액을 여과후, 원심분리하여 세분을 제거했다. 이 추출액을 역상계의 흡착재 컬럼에 제공하고, 컬럼을 물로 세정했다. 물/메탄올 혹은 물/아세토니트릴, 구체적으로는 물/메탄올(6/4)로 용출하는 암갈색의 용액을 감압 농축에 의해 유기용매를 제거하고, 소량의 폴리비닐피롤리돈을 가하여 교반후 여과하여 폴리페놀을 제거했다. 계속하여, 처리액을 DEAE -셀룰로오스에 의한 이온 교환 크로마토그래피에 제공했다. 컬럼을 수세하여 중염기성 성분을 제거한 후, 수산화나트륨 수용액에서 용출했다. 용출액을 한외 여과(분획 분자량 1만달톤)하여 저분자 성분을 제거하고, 수세후, 동결 건조했다. 더욱이, 메탄올/물(9/1)로 분별 침전을 행하여 원심분리하여 침전하는 다당류나 단백질을 제거하고, 상청부를 감압 농축후, 동결 건조하여 최종 정제품을 얻었다. 본 원인성분의 최종 정제품은 원료로부터 수율 약 0.2%에서 획득되어, 향료무첨가 평가용 궐련에 대하여 약 400ppm 농도의 첨가에서, 10명의 전문 패널 전원에 의해 벌리종 특유의 자극ㆍ매운 맛이 발현되는 것이 확인되었다.The Burley seed bone-bone raw material was grind | pulverized, and extraction was performed by stirring for 30 minutes at room temperature in 10-times 0.1 M sodium acetate aqueous solution. The extract was filtered and then centrifuged to remove subdivision. This extract was provided to an adsorber column of a reversed phase, and the column was washed with water. The dark brown solution eluting with water / methanol or water / acetonitrile, specifically water / methanol (6/4), was concentrated under reduced pressure to remove the organic solvent, and a small amount of polyvinylpyrrolidone was added thereto. Polyphenols were removed. Subsequently, the treatment liquid was subjected to ion exchange chromatography with DEAE-cellulose. The column was washed with water to remove the neutral base component, and then eluted with an aqueous sodium hydroxide solution. The eluate was subjected to ultrafiltration (fractional molecular weight 10,000 daltons) to remove the low molecular weight component, and washed with water and lyophilized. Furthermore, fractional precipitation was carried out with methanol / water (9/1) to remove centrifuged polysaccharides and proteins. The supernatant was concentrated under reduced pressure, and freeze-dried to obtain a final product. The final refined product of the causative ingredient was obtained in a yield of about 0.2% from the raw material, and at a concentration of about 400 ppm with respect to the cigarette for flavor-free evaluation, all 10 professional panelists expressed the irritating and pungent taste peculiar to Burley species. Confirmed.

본 원인성분의 겔 여과 고속액체크로마토그램은, 도 1에 나타나 있다(하기 실시예 1 참조). 도 1에 분명한 바와 같이, 본 원인성분은, 1만∼6만달톤의 분자량을 갖고, 피크 분자량은, 1만 6천달톤이다. 본 원인성분은, 상술한 바와 같이 산성물질이며, 그 수용액은 농도에 따라 다갈색∼흑갈색을 나타낸다(도 2에 나타내는 자외가시흡수스펙트럼 참조). 또한, 담배 중에 포함되는 것 이외의 수용성 고분자인 펙틴이나 단백질 등과는 달리, 함수 알코올에 가용이다.The gel filtration high performance liquid chromatogram of the causative agent is shown in Fig. 1 (see Example 1 below). As apparent from Fig. 1, the causative agent has a molecular weight of 10,000 to 60,000 Daltons, and a peak molecular weight of 16,000 Daltons. This causative component is an acidic substance as mentioned above, and its aqueous solution shows dark brown to black brown depending on concentration (refer to the ultraviolet visible absorption spectrum shown in FIG. 2). Moreover, unlike pectin, protein, etc. which are water-soluble polymers other than what is contained in tobacco, it is soluble in hydrous alcohol.

도 3에 본 원인성분의 적외흡수스펙트럼을 나타낸다. 본 원인성분은, 도 3에 나타낸 바와 같이, 3423, 2935, 1618, 1411, 1261, 1070 및 534cm-1에 흡수 피크를 나타낸다.3 shows the infrared absorption spectrum of the causative agent. As shown in Fig. 3, the causative component exhibits absorption peaks at 3423, 2935, 1618, 1411, 1261, 1070, and 534 cm −1 .

본 원인성분의 원소분석 결과는, 이하와 같다.The elemental analysis of this causal component is as follows.

C:36.2%; H:4.70%; N:4.09%; 회분:12.6%.C: 36.2%; H: 4.70%; N: 4.09%; Ash: 12.6%.

본 원인성분의 자외가시흡수스펙트럼의 특징은, 일반의 식품 등에 있어서의 메라노이진이라는 갈색 고분자에 유사하다. 식품 중의 메라노이진에 관하여는 많은 연구가 되고 있어, 그 생성에는 당질-아미노산 등의 메일러드(비효소적 갈변)반응, 및 폴리페놀류의 효소에 의한 산화적 중합(효소적 갈변)반응이 관여하고 있다고 하고 있다. 그러나, 식품마다 관여하는 성분이 다르기 때문에 화학조성이나 성질이 다르고, 일반적인 화학구조는 미확정이다(타카미야 카즈히코편 「색으로부터 본 식품의 사이언스」, p.183-191(2004); 「전분과학」제38권 제1호 p.73∼79(1991) 참조).The characteristics of the ultraviolet visible absorption spectrum of the causative ingredient are similar to those of brown polymer called meranozin in general foods. There have been many studies on melanoids in foods, and their production involves Maillard (non-enzymatic browning) reactions such as saccharide-amino acids and oxidative polymerization (enzymatic browning) reactions by enzymes of polyphenols. I am doing it. However, because the ingredients involved in each food are different, the chemical composition and properties are different, and the general chemical structure is undetermined (Kazhiko Takamiya, `` Science of Food from Color, '' p.183-191 (2004); "Starch Science"). Vol. 38, No. 1, p. 73-79 (1991)).

한편, 벌리종 담배 원료중의 착색 성분은 갈색 색소(brown pigment)라 불리고, 화학적 성질은 본 원인성분과 유사하고 있다. 갈색 색소에 관하여는 화학적 검토가 행해지고 있어, Arch. Biochem. Biophys., 86, 94-101(1960)이나 Arch. Biochem. Biophys., 93, 580-590(1961)에서는, 폴리페놀(크롤로겐산 및 루틴)의 산화 중합물(효소적 갈변반응)과 단백질이나 철 이온 등이 복합된 고분자 성분이라 생각되고 있다. 그 후의 연구에 의해, 담배중의 갈색 색소는 화학조성이 다른 몇종류로 나눌 수 있는 것이 분명하게 되어 있다(J. Agric. Food Chem., 26(1978), 380-385) 참조).On the other hand, the coloring component in Burley's tobacco raw material is called a brown pigment, and the chemical property is similar to the present causative ingredient. Chemical examination is performed about the brown pigment | dye, Arch. Biochem. Biophys., 86, 94-101 (1960) or Arch. Biochem. Biophys., 93, 580-590 (1961) is considered to be a polymer component in which an oxidative polymerization product (enzymatic browning reaction) of polyphenols (chromoic acid and rutin) is combined with proteins, iron ions, and the like. Subsequent studies have made it clear that brown pigments in tobacco can be divided into several different chemical compositions (see J. Agric. Food Chem., 26 (1978), 380-385).

또한, 잎담배에 관해서 갈색 색소 분석 방법 및 그것을 이용한 정상잎과 품질 저하잎의 판별 방법이 제안되어 있다(일본국특개평 11-83827호 공보). 이 분석법은 잎담배의 조추출액을 물/아세토니트릴 용매계의 역상액체크로마토그래프에서 순차 아세토니트릴의 비율을 증가시켜, 극성이 다른 갈색 색소 성분을 분리하여, 그 비율로부터 정상잎과 품질 저하잎의 판별을 행하는 것이다. 원료잎 담배의 품질등급에는 색조가 판정의 요소로 되어 있어, 그 의미에서 색조의 주체를 이루는 갈색 색소 성분은 중요하다. 그러나, 이 성분의 직접적인 끽미효과에 관하여는 보고가 없다.In addition, a brown pigment analysis method for leaf tobacco and a method for discriminating between normal leaves and deteriorated leaves using the same have been proposed (Japanese Patent Laid-Open No. 11-83827). In this assay, the crude extract of leaf tobacco was gradually increased in acetonitrile ratio in reversed-phase liquid chromatograph of water / acetonitrile solvent system to separate brown pigment components of different polarity, and to distinguish normal leaves and deteriorated leaves from the ratio. To do. In the quality grade of raw leaf tobacco, the color tone is an element of determination, and in that sense, the brown pigment component which constitutes the color tone is important. However, there is no report on the direct taste effect of this ingredient.

이상과 같은 경위에서, 천연 담배재료, 특히 벌리종 담배 원료중의 착색 산성 고분자 성분(본 원인성분)이 벌리종의 독특한 자극ㆍ매운 맛을 발현하는 것을 처음으로 찾아냈다. 또한 본 원인성분이 소위 메라노이진이나 담배의 갈색 색소 성분이라 부르고 있는 성분과 화학적 성질이 유사하다는 것을 밝혔다.In view of the above, it has been found for the first time that a natural tobacco material, particularly a coloring acidic polymer component (the main causative ingredient) in a Burley tobacco ingredient, expresses the distinctive irritation and spicy taste of Burley. It was also found that the causative agent is similar in chemical properties to the so-called melanoids or the brown pigment component of tobacco.

따라서, 본 원인성분을 천연 담배재료, 특히 벌리종 담배 원료로부터 삭감하는 것에 의해, 자극ㆍ매운 맛을 저감하여 효율적으로 향끽미를 개선할 수 있다. 즉, 본 발명에 의해, 착색 산성 수용성 고분자 물질의 함유율을 감소시키는 것에 의해 흡연시의 자극ㆍ매운 맛을 저감시킨 것을 특징으로 하는 담배재료를 제공할 수 있다.Therefore, by reducing this causative ingredient from natural tobacco material, especially Burley tobacco raw material, it can reduce the irritation and spicy taste, and can improve a taste efficiently. That is, according to this invention, the tobacco material characterized by reducing the stimulation and spicy taste at the time of smoking by reducing the content rate of a coloring acidic water-soluble high molecular substance can be provided.

또한, 천연 담배재료를 수계 추출 용매에 의해 추출하여 얻은 추출액으로부터 본 원인성분을 저감시켜 얻어진 추출액은, 그대로, 또는 농축하고, 혹은 동결 건조하여, 자극ㆍ매운 맛의 원인성분이 저감한 담배 향끽미제로서 사용할 수 있다. 그리고, 추출 잔사인 섬유재료를 이용하여 통상의 방법에 의해 제작된 재생 웹 시트에 이 담배 향끽미제를 첨가하는 것에 의해, 재생 담배재료를 얻을 수 있다.In addition, the extract obtained by reducing the causative component from the extract obtained by extracting the natural tobacco material with an aqueous extracting solvent is, as it is, or concentrated or freeze-dried to reduce the causative ingredient of irritation and spicy taste. Can be used as The regenerated tobacco material can be obtained by adding the tobacco flavoring agent to the regenerated web sheet produced by the usual method using the fibrous material as the extraction residue.

여기에서, 추출 처리에 제공하는 천연 담배재료로서는, 담배의 잎, 살, 중골, 줄기, 뿌리 및 그들의 혼합물을 이용할 수 있다. 추출 용매로서는, 수계 용매를 이용할 수 있다. 물 등의 수계 추출 용매는, 알카리성이어도, 산성이어도 좋다. 수계 추출 용매로서, 물과 물혼화성 유기용매와의 혼합물도 사용할 수 있다. 그와 같은 유기용매의 예를 들면, 에탄올과 같은 알코올류이다. 이들 추출 용매에는, 염화나트륨과 같은 무기염을 용해하여 이용할 수도 있다. 추출 처리는, 통상, 실온 (약 25℃)∼100℃의 온도에서, 5분∼6시간 정도 행할 수 있다.Here, as the natural tobacco material to be used for the extraction treatment, tobacco leaves, flesh, ribs, stems, roots and mixtures thereof can be used. As the extraction solvent, an aqueous solvent can be used. The aqueous extraction solvent such as water may be alkaline or acidic. As the aqueous extraction solvent, a mixture of water and a water miscible organic solvent can also be used. Examples of such organic solvents are alcohols such as ethanol. In these extraction solvents, inorganic salts such as sodium chloride may be dissolved and used. Extraction processing can be normally performed at the temperature of room temperature (about 25 degreeC)-100 degreeC for about 5 minutes-about 6 hours.

추출 처리의 종료후, 얻어진 추출 혼합물을 예컨대 압착 여과 등에 의한 분리 조작에 제공하고, 추출액과 추출 잔사(섬유)로 나눈다. 얻어진 추출액으로 본 원인성분을 저감시키는 것에 의해, 본 발명의 담배 향끽미제가 얻어진다. 이 담배 향끽미제는, 그대로, 또는 농축하여, 혹은 동결 건조하여 이용할 수 있다.After the completion of the extraction process, the obtained extraction mixture is subjected to, for example, a separation operation by compression filtration or the like, and divided into an extraction liquid and an extraction residue (fiber). The tobacco flavor agent of this invention is obtained by reducing this causative component with the obtained extraction liquid. This tobacco flavor agent can be used as it is, or concentrated or freeze-dried.

다른 한편, 추출 잔사를 이용하여 슬러리를 제작하고, 초지하여 재생 담배 웹을 제조한다. 이 재생 담배 웹은, 그 전부가 상기 추출 잔사에 의해 구성되는 것이라도 좋고, 그 일부가 상기 추출 잔사에 의해 구성되는 것이라도 좋다. 더욱이, 추출 잔사는, 본 발명의 향끽미제를 조제하기 위하여 직접 추출 처리한 결과의 추출 잔사이어도 좋고, 다른 목적에서 천연 담배재료를 추출하여 얻은 추출 잔사이어도 좋다.On the other hand, a slurry is prepared using the extraction residue and papermaking to produce a recycled tobacco web. The regenerated tobacco web may be entirely composed of the extraction residue, or a part thereof may be composed of the extraction residue. Moreover, the extraction residue may be an extraction residue obtained by directly extracting the resultant to prepare the flavoring agent of the present invention, or may be an extraction residue obtained by extracting a natural tobacco material for another purpose.

다음에, 추출액으로부터 본 원인성분을 저감시키기 위한 보다 구체적인 방법을 설명한다. 이 저감방법은, 본 원인성분의 물리적ㆍ화학적 성질에 의거한 것이다. 즉, 본 원인성분은, 분자량이 1만∼6만의 고분자 물질인 것, 펙틴 등의 담배 성분과 비교하여 저극성인 것, 산성의 수용성 고분자 물질인 것 등의 물리적ㆍ화학적 성질을 이용하여, 본 원인성분을 효율적으로 저감하여 향끽미를 개선할 수 있다. 이하에, 본 원인성분의 저감방법에 관하여 상술한다. 또, 천연 담배재료로부터의 추출액의 획득 방법은, 상술한 바와 같다.Next, a more specific method for reducing the causative component seen from the extract will be described. This abatement method is based on the physical and chemical properties of the causative agent. That is, the causative agent is obtained by using physical and chemical properties such as those having a molecular weight of 10,000 to 60,000, substance having a low polarity compared with tobacco components such as pectin, and an acidic water-soluble polymeric substance. The taste can be improved by efficiently reducing the components. Below, the method of reducing this causative component is explained in full detail. In addition, the acquisition method of the extraction liquid from a natural tobacco material is as above-mentioned.

<본 원인성분의 한외 여과법 등에 의한 저감방법><Reduction method by ultrafiltration method of this causative ingredient>

천연 담배 원료로부터의 추출액을 반투막 혹은 호로파이버 등을 이용한 한외 여과법에서 분자량 1천달톤 이상, 바람직하게는 1만달톤 이상의 고분자 성분을 제거한다. 이 제거 조작은 투석법이나 겔 여과법에서도 가능하다. 분자량 1천달톤 미만, 바람직하게는 분자량 1만달톤 미만의 분획을 향끽미제로서 이용할 수 있다.The ultra-filtration method using the semi-permeable membrane or a fluorofiber etc. extracts from the natural tobacco raw material removes the polymer component of molecular weight 1,000 Daltons or more, Preferably 10,000 Daltons or more. This removal operation can also be performed by dialysis or gel filtration. Fractions of less than 1,000 Daltons in molecular weight, preferably less than 10,000 Daltons in molecular weight can be used as flavoring agents.

<본 원인성분의 이온 교환에 의한 저감방법><Reduction method by ion exchange of this causative ingredient>

천연 담배 원료로부터의 추출액을 음이온 교환수지(대표예:DEAE셀룰로오스(DEAE셀로파인(상품명) 등)에 의해 흡착 처리에 제공하고, 여과 등에서 수지를 제거한다. 얻어진 여액은, 본 원인성분이 저감한 것으로 된다. 이 여액을 향끽미제로서 이용할 수 있다. 본 조작에는 이온 교환막도 적용가능하다.The extract from the natural tobacco raw material is supplied to an adsorption treatment by an anion exchange resin (representative example: DEAE cellulose (DEAE Cellopine (trade name), etc.), and the resin is removed by filtration, etc. The filtrate obtained is reduced in the causative component This filtrate can be used as a flavoring agent, and an ion exchange membrane can also be applied to this operation.

<본 원인성분의 흡착 수지 등에 의한 저감방법><Reduction method by adsorption resin etc. of this causative ingredient>

천연 담배 원료로부터의 추출액을 활성탄, 흡착성 수지(폴리스티렌/디비닐벤젠 공중합체 등), 혹은 역상계 흡착제(대표예:옥타데실실리카겔(ODS) 등)에 의한 흡착 처리에 제공하고, 흡착제를 분리하고, 처리액을 얻는다. 흡착제는 물 및 물/알코올 등으로 세정하여 세액(洗液)을 처리액에 가한다. 이 처리액을 담배 향끽미제로서 이용할 수 있다.Extracts from natural tobacco raw materials are subjected to adsorption treatment with activated carbon, adsorbent resins (polystyrene / divinylbenzene copolymers, etc.), or reversed phase adsorbents (e.g. octadecyl silica gel (ODS), etc.), and the adsorbents are separated. , Process liquid is obtained. The adsorbent is washed with water, water / alcohol and the like, and the washing solution is added to the treatment liquid. This treatment liquid can be used as a tobacco flavoring agent.

<본 원인성분의 산 침전에 의한 저감방법><Reduction method by acid precipitation of the causative agent>

본 원인성분은 산성의 성질을 나타내는 고분자 물질이므로, 그 용액의 pH(수소 이온 농도)를 낮추는 것에 의해 불용화시켜, 분리할 수 있다(상기 문헌J. Agric. Food Chem., 26(1978), 380-385의 수법을 참조). 구체적으로는, 천연 담배 원료로부터의 추출액에 무기산(황산, 인산 등) 또는 유기산(옥살산 등)을 가하여 pH를 바람직하게는 2 이하로 저하시킨다. 여과 또는 원심분리 등으로 침전을 제거한 후, 알칼리(수산화칼슘 등)를 가하여 pH를 원래 상태로 되돌린다. 옥살산을 이용한 경우는, 수산화칼슘으로 처리하는 것에 의해, 수불용성의 옥살산칼슘으로 되어 원심분리 등에 의해 제거할 수 있다. 이 처리액을 향끽미제로서 이용할 수 있다.Since the causative component is a high molecular material having an acidic property, it can be insolubilized and separated by lowering the pH (hydrogen ion concentration) of the solution (J. Agric. Food Chem., 26 (1978), See the technique in 380-385). Specifically, the inorganic acid (sulfuric acid, phosphoric acid, etc.) or organic acid (oxalic acid, etc.) is added to the extract from the natural tobacco raw material, and pH is preferably reduced to 2 or less. After removing the precipitate by filtration or centrifugation or the like, alkali (calcium hydroxide or the like) is added to return the pH to its original state. When oxalic acid is used, it becomes water-insoluble calcium oxalate by treating with calcium hydroxide and can be removed by centrifugation or the like. This treatment liquid can be used as a flavoring agent.

<본 원인성분의 용매침전에 의한 저감방법><Reduction method by solvent precipitation of this causative ingredient>

본 원인성분은 다른 다당류나 단백질 등과 다르고, 물/메탄올(부피비 1/9) 혼합 용매에 가용이지만, 보다 극성이 낮은 용매에는 불용이다. 이 성질을 이용하여 본 원인성분을 다른 성분으로부터 분리할 수 있다. 극성이 낮은 용매로서는, 알코올류, 구체적으로는 메탄올(100%), 에탄올, 이소프로판올 등의 지방족 알코올, 벤질알코올 등의 방향족 알코올, 또는 다른 수가용성 용매 아세톤, 메틸에틸케톤, 아세토니트릴 등을 단독 혹은 혼합 용매로서 이용할 수 있다. 이 경우, 예컨대 헥산과 같이 물은 비혼화성의 용매도 알코올 등을 포함하는 용매에는 가용이기 때문 이용할 수 있다. 더욱이, 용매의 종류를 단계적으로 변경하여 분별 침전을 행하고, 본 원인성분의 분석값을 바탕으로 분획의 취사 선택을 행할 수도 있다.This causative ingredient is different from other polysaccharides and proteins and is soluble in water / methanol (volume ratio 1/9) mixed solvents, but insoluble in solvents having lower polarities. This property can be used to isolate the causative agent from other components. Examples of the solvent having low polarity include alcohols, specifically, aliphatic alcohols such as methanol (100%), ethanol and isopropanol, aromatic alcohols such as benzyl alcohol, or other water-soluble solvents such as acetone, methyl ethyl ketone, acetonitrile or the like. It can be used as a mixed solvent. In this case, for example, water, such as hexane, can be used because an immiscible solvent is soluble in a solvent containing alcohol and the like. Moreover, fractional precipitation can be performed by changing the kind of solvent step by step, and the fraction can be selected based on the analysis value of the causative component.

<상기 처리의 조합에 의한 본 원인성분의 저감방법><Method of reducing the present causative component by the combination of the above treatments>

담배 원료로부터의 본 원인성분의 저감에는, 상기 저감방법의 어느 하나를 단독, 또는 조합시켜서 행할 수 있다. 또한 조건의 선택에 의한 성분의 저감량의 조절이나, 분리한 성분을 적당량 재생 담배 웹에 첨가할 수도 있다.Reduction of the causative agent from the tobacco raw material can be carried out either alone or in combination. In addition, it is also possible to adjust the amount of reduction of the component by the selection of conditions or to add an appropriate amount of the separated component to the recycled tobacco web.

또한, 상기의 저감방법에서 얻은 향끽미제를 2종 이상 혼합할 수도 있다.Moreover, 2 or more types of flavoring agents obtained by said reduction method can also be mixed.

이상 상술한 바와 같이, 본 발명에 따라 착색 산성 수용성 고분자 물질을 천연 담배재료(또는 그 추출액)로부터 제거하는 것에 의해, 최종 담배 제품의 흡연시의 자극ㆍ매운 맛을 저감시킬 수 있다. 그 경우, 착색 산성 수용성 고분자 물질은, 자극ㆍ매운 맛 저감의 감정으로부터, 초기량(천연 담배재료에 존재하는 양, 또는 천연 담배재료로부터 수계 추출 용매로 추출한 그대로의 추출액 중의 중량)의 10% 이상(100%까지), 바람직하게는 50% 이상, 더욱 바람직하게는 80% 이상 저감시키는 것이 바람직하다.As described above, according to the present invention, by removing the colored acidic water-soluble high molecular substance from the natural tobacco material (or its extract), the irritation and spicy taste at the time of smoking of the final tobacco product can be reduced. In that case, the coloring acidic water-soluble high molecular substance is 10% or more of the initial amount (amount present in the natural tobacco material, or the weight in the extract as it is extracted from the natural tobacco material with the aqueous extraction solvent) from the feeling of irritation and spicy taste reduction. (Up to 100%), preferably at least 50%, more preferably at least 80%.

도 1은, 착색 산성 수용성 고분자 물질(자극ㆍ매운 맛 원인성분)의 겔 여과 고속액체크로마토그램이다.BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a gel filtration high performance liquid chromatogram of colored acidic water-soluble high molecular substance (irritant and pungent causative ingredient).

도 2는, 착색 산성 수용성 고분자 물질(자극ㆍ매운 맛 원인성분)의 자외가시 흡수스펙트럼이다.Fig. 2 is an ultraviolet visible absorption spectrum of colored acidic water-soluble high molecular substance (irritation and spicy taste cause component).

도 3은, 착색 산성 수용성 고분자 물질(자극ㆍ매운 맛 원인성분)의 적외흡수스펙트럼이다.Fig. 3 is an infrared absorption spectrum of colored acidic water-soluble high molecular substance (irritant and pungent causative ingredient).

이하, 실시예 및 참고예에 의해 본 발명을 더욱 구체적으로 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples and Reference Examples.

실시예 1:본 원인성분의 분석법Example 1 Assay of Present Causative Ingredients

본 원인성분 저감의 지표로서, 고속액체크로마토그래피를 이용한 본 원인성분의 간이분석법을 구축했다. 벌리종 담배 원료(추출액의 경우는 담배 원료 1.Og 상당분을 동결 건조한 것) 1.0g을 분쇄하고, 이것에 0.1M 아세트산나트륨 수용액 10mL를 가하여, 실온에서 30분간 교반하고, 여과, 원심분리하여 상청부를 역상계 고상 추출 캇트리지(오아시스HLB(6cc, 500mg, 오타즈사))에 통과시키고, 수세후, 아세토니트릴/물(6/4) 10mL에서 용출시켰다. 용출액을 감압 농축하여 아세토니트릴을 제거하고, 폴리비닐피롤리돈 수지(폴리쿠라VT(와코준야쿠))의 미니컬럼에 통과시키고, 더욱이 음이온 교환 고상 추출 캇트리지(본도엘트DEA(500mg, 발리앤사))에 제공했다. 수세후, 0.4N 수산화나트륨 수용액 4mL에서 용출시켜, 용출액을 그대로 한외 여과 디바이스(아미콘울트라4(분획 분자량 1만달톤, 미리포어사))에 의해 원심 한외 여과와 완충액(0.1M 식염을 포함하는 0.1M 인산완충액(pH6.8))교환을 행하고, 최종적으로 동완충액에서 5mL에 메스업하여 고속액체크로마토그래피 분석에 제공했다.As an index for reducing the causative component, a simplified analysis method of the causal component using high performance liquid chromatography was established. 1.0 g of Burley's tobacco raw material (in the case of extract, 1.0 g of tobacco raw material is freeze-dried) was pulverized, 10 ml of 0.1 M aqueous sodium acetate solution was added thereto, stirred at room temperature for 30 minutes, filtered and centrifuged. The supernatant was passed through a reversed phase solid phase extraction cartridge (oasis HLB (6 cc, 500 mg, Otazu Co.)), and washed with water and eluted with 10 mL of acetonitrile / water (6/4). The eluate was concentrated under reduced pressure to remove acetonitrile, passed through a minicolumn of polyvinylpyrrolidone resin (PolyCura VT (Wakjunyaku)), and furthermore, anion exchange solid phase extraction cartridge (Vondoelt DEA (500 mg, volley) Ansa provided)). After washing with water, the solution was eluted in 4 mL of 0.4 N aqueous sodium hydroxide solution, and the eluate was centrifuged with ultrafiltration and buffer (0.1 M saline) using an ultrafiltration device (Amicon Ultra 4 (fractional molecular weight 10,000 Daltons, Myrpor)). 0.1 M phosphate buffer (pH 6.8)) was exchanged, and finally, the volume thereof was made up to 5 mL in the same buffer solution and subjected to high performance liquid chromatography analysis.

<분석 조건><Analysis condition>

고속액체크로마토그래프 기종:아지렌트사 1100형High-speed liquid chromatograph model: azirent company 1100 type

컬럼:프로틴 팩 125(오타즈사)Column: Protein Pack 125 (Otazu Corporation)

용매:0.1M 식염을 포함하는 0.1M 인산완충액(pH6.8)Solvent: 0.1 M phosphate buffer containing 0.1 M salt (pH 6.8)

용매유속:1.0mL/분Solvent Flow Rate: 1.0mL / min

검출기:다이오드앨리;측정 파장 410nm.Detector: diode ally; measuring wavelength 410 nm.

대표적인 크로마토그램을 도 1에 나타낸다. 이 크로마토그램에 있어서의 파장 410nm 피크의 적분값을 본 원인성분 저감의 지표로 한다.Representative chromatograms are shown in FIG. 1. The integral value of the wavelength 410 nm peak in this chromatogram is used as an index of the reduction of the causative component.

또한, 여기에서 얻어진 본 원인성분의 자외가시흡수스펙트럼은 도 2에 나타내는 대로이며, 적외흡수스펙트럼은, 도 3에 나타내는 대로였다. 원소 분석 결과는, 위로 나타낸 대로이다.In addition, the ultraviolet visible absorption spectrum of this causal component obtained here was as showing in FIG. 2, and the infrared absorption spectrum was as showing in FIG. The elemental analysis results are as shown above.

참고예:재생 담배 시트의 제조Reference Example: Production of Recycled Cigarette Sheets

벌리종 담배 원료(중골:라미나 중량비=1:1) 75g을 60℃의 온수 0.75L에 교반하면서 30분 침지후, 압착 여과하여, 여액(추출액)과 추출 잔사(섬유)로 분리했다. 통상의 방법에 의해, 섬유를 슬러리화한 후, 초지하여 재생 담배 웹 시트를 얻었다. 조화 처리후의 재생 담배 웹 시트의 중량은, 20.6g이었다. 이 재생 웹 시트를 재각하여 원료 담배살을 얻었다.75 g of Burley's tobacco raw material (heavy bone: lamina weight ratio = 1: 1) was immersed in 0.75 L of hot water at 60 ° C. for 30 minutes, followed by compression filtration to separate the filtrate (extract liquid) and the extraction residue (fiber). After slurrying the fibers by a conventional method, papermaking was carried out to obtain a recycled tobacco web sheet. The weight of the recycled tobacco web sheet after the roughening treatment was 20.6 g. The recycled web sheet was re-cut to obtain raw tobacco flesh.

다른 한편, 여액(약 0.5L)을 50mL 이하로 감압 농축하고, 상기 원료 담배살에 분무하고, 건조후, 조화 처리(온도 습도 일정 조건에서, 수분평형에 달할때 까지 장치)하여 재생 담배살을 얻었다. 이것을 이용하여 손으로 말기 조작에 의해 궐련(1개피당의 살 양 약 0.6g)을 제작했다.On the other hand, the filtrate (about 0.5L) was concentrated under reduced pressure to 50 mL or less, sprayed onto the raw tobacco meat, dried, and then subjected to a roughening treatment (apparatus under a certain condition of temperature and humidity until the equilibrium of moisture) to reproduce the tobacco cigarette. Got it. Using this, a cigarette (about 0.6 g of flesh per one skin) was produced by rolling operation by hand.

실시예 2Example 2

참고예에서 얻은 여액(0.5L, 원료 75g 상당)을 원심분리(3000rpm, 10분)하여 불용부를 제거한 후, 분획 분자량 1만달톤의 재생 셀룰로오스제 반투막을 이용한 한외 여과 디스크(미리포어사 울트라 셀 PLGC 한외 여과 디스크, 공칭 분획 분자량 10,000)를 이용한 한외 여과 처리를 행하였다. 투과액과 농축액의 동결 건조후의 수량은 각각 12.8g과 2.1g이었다. 투과액의 동결 건조물을 50mL의 물에 용해하고, 참고예에서 얻은 원료단위에 전량 분무 첨가하고, 재생 담배살을 얻었다. 이 재생 담배살을 이용하여, 참고예와 같이 하여 궐련을 제조했다.The filtrate (0.5 L, equivalent to 75 g of raw material) obtained in the reference example was centrifuged (3000 rpm, 10 minutes) to remove the insoluble portion, and then an ultrafiltration disc using a semi-permeable membrane made of regenerated cellulose having a fractional molecular weight of 10,000 Daltons (Millipore Ultra Cell PLGC). An ultrafiltration treatment using an ultrafiltration disc and a nominal fraction molecular weight of 10,000) was performed. The yields after freeze drying of the permeate and the concentrate were 12.8 g and 2.1 g, respectively. The freeze-dried product of the permeate was dissolved in 50 mL of water, sprayed in the total amount to the raw material unit obtained in the reference example, and regenerated tobacco meat was obtained. Using this recycled tobacco flesh, a cigarette was produced as in the reference example.

실시예 3Example 3

참고예 여액(0.5L, 원료 75g 상당)을 원심분리(3000rpm, 10분)하여 불용부를 제거하고, 음이온 교환수지(생화학공업제 DEAE 셀로파인) 50mL(습기찬 수지의 부피)를 가하여 교반흡착을 행한 후, 여과 처리를 행하였다. 처리액을 감압 농축하고, 참고예에서 얻은 원료단위에 전량 분무 첨가하고, 재생 담배살을 얻었다. 이 재생 담배살을 이용하여, 참고예와 같이 하여 궐련을 제조했다.Reference Example Centrifugation (3000 rpm, 10 minutes) of the filtrate (0.5 L, equivalent to 75 g of raw material) was used to remove the insoluble portion, and 50 mL (volume of humid resin) was added to the anion exchange resin (DEAE Cellopine, manufactured by Biochemical Industry). After performing, the filtration process was performed. The treatment liquid was concentrated under reduced pressure, sprayed whole quantity to the raw material unit obtained by the reference example, and regenerated tobacco meat was obtained. Using this recycled tobacco flesh, a cigarette was produced as in the reference example.

실시예 4Example 4

참고예 여액(0.5L, 원료 75g 상당)을 원심분리(3000rpm, 10분)하여 불용부를 제거하고, 역상계 흡착 수지(오아시스 HLB; 수지량 6g×2개피, 오타즈사)의 컬럼을 통과시켜 착색 성분을 흡착시켰다. 처리액을 감압 농축하고, 참고예에서 얻은 원료단위에 전량 분무 첨가하고, 재생 담배살을 얻었다. 이 재생 담배살을 이용하여, 참고예와 같이 하여 궐련을 제조했다.Reference Example A filtrate (0.5 L, equivalent to 75 g of raw material) was centrifuged (3000 rpm, 10 minutes) to remove an insoluble portion, followed by coloring through a column of reversed-phase adsorption resin (Oasis HLB; 6 g × 2 pieces of resin, Otazu Co., Ltd.). The component was adsorbed. The treatment liquid was concentrated under reduced pressure, sprayed whole quantity to the raw material unit obtained by the reference example, and regenerated tobacco meat was obtained. Using this recycled tobacco flesh, a cigarette was produced as in the reference example.

<참고예 및 실시예 2∼4의 분석값 및 끽미평가><Analytical Values and Taste Evaluations of Reference Examples and Examples 2 to 4>

원료 1g에 대응하는 추출액 중의 본 원인성분의 분석값(실시예 1에서 언급한 바와 같이 액체크로마토그램에 있어서의 파장 410nm의 피크 면적;상대값)을 구했다. 또한, 자극ㆍ매운 맛의 감소 평가를 10명의 전문 패널 중, 참고예의 궐련에 대하여 자극ㆍ매운 맛이 분명히 감소했다고 평가한 인원수로 나타냈다. 결과를 표 1 에 나타낸다.The analysis value (peak area of a wavelength of 410 nm in a liquid chromatogram; relative value) in the liquid chromatogram as mentioned in Example 1 was calculated | required in the extract liquid corresponding to 1 g of raw materials. In addition, the evaluation of the reduction in irritation and spicy taste was shown by the number of people who evaluated that the irritation and spicy taste clearly decreased with respect to the cigarette of the reference example among 10 specialized panels. The results are shown in Table 1.

추출액 중의 본 원인성분의 분석값Analysis value of present causative component in extract 자극ㆍ매운 맛의 감소평가Reduction evaluation of irritation and spicy taste 끽미평가 코멘트Taste comments 참고예 (무처리:대조)Reference Example (No Processing: Control) 454.8454.8 자극ㆍ매운 맛 강하고, 나중에 입안에 남아 있음. 벌리종과 같은 쓴맛, 불쾌감, 특이함 강함.Irritation and spicy tastes strong and remain in the mouth later. Bitter, bitter, unpleasant and unusual. 실시예 2 (한외여과처리)Example 2 (Ultrafiltration Treatment) 27.527.5 10/1010/10 자극ㆍ매운 맛이 거의 없고, 나중에 입안에 남은 것도 적다. 불쾌감, 특이함이 강하고, 흡입하기 용이하게 된다.Almost no irritation or spicy taste, and little left in the mouth later. The discomfort and unusualness are strong and it is easy to inhale. 실시예 3 (이온교환처리)Example 3 (Ion Exchange Treatment) 81.081.0 6/106/10 자극ㆍ매운 맛이 감소한다. 나중에 입안에 약간 남는다. 쓴맛이 감소하지만, 산악취가 약간 강하다.Irritation and spicy taste are reduced. Later it remains slightly in your mouth. The bitter taste is reduced, but the mountain odor is slightly stronger. 실시예 4 (역상수지처리)Example 4 (Reverse Resin Treatment) 23.023.0 10/1010/10 자극ㆍ매운 맛이 거의 없고, 나중에 입안에 남은 것도 적다. 약간 악취 있음.Almost no irritation or spicy taste, and little left in the mouth later. There is a slight odor.

이상 본 발명을 여러가지 태양, 실시예 등에 따라 설명했지만, 본 발명은, 이들 태양, 실시예에 의해 제한되는 것은 아니다. 본 발명자들이 초기에 찾아낸 자극ㆍ매운 맛 원인성분은, 벌리종에 한하지 않고, 다른 담배종(예컨대, 황색종, 오리엔트종, 재래종)에도 포함될 수 있는 것이며, 본 발명은 그들 담배종 또는 그들 담배종을 포함하는 천연 담배재료에 적용할 수 있는 것은 말할 필요도 없고, 널리 천연 담배재료 일반에 적용되는 것이다.As mentioned above, although this invention was demonstrated according to various aspects, the Example, etc., this invention is not restrict | limited by these aspects and Examples. The stimulus and spicy taste-causing ingredients that the inventors initially found are not limited to Burley, but can also be included in other tobacco species (for example, yellow, orient, and native), and the present invention relates to those tobacco species or those tobacco. Needless to say, the present invention can be applied to natural tobacco materials including species, and is widely applied to natural tobacco materials in general.

이상 서술한 바와 같이, 본 발명에 따라 담배재료 중의 수가용성 성분 중의 착색 산성 수용성 고분자 물질을 저감시키는 것에 의해, 종래 담배 원료의 끽미개선에 이용되어 있었던 각종 향료의 첨가나 처리 공정을 이용하지 않고, 담배재료의 자극ㆍ매운 맛을 저감시킬 수 있다.As described above, by reducing the coloring acidic water-soluble high molecular substance in the water-soluble component in the tobacco material according to the present invention, without the addition of various flavors and treatment process conventionally used for taste improvement of tobacco raw materials, The irritation and spicy taste of tobacco material can be reduced.

Claims (9)

1만∼6만달톤의 분자량을 갖는 착색 산성 수용성 고분자 물질의 함유율을 감소시키는 것에 의해 흡연시의 자극ㆍ매운 맛을 저감시킨 담배재료.A tobacco material which reduces the irritation and spicy taste during smoking by reducing the content of colored acidic water-soluble high molecular materials having a molecular weight of 10,000 to 60,000 Daltons. 삭제delete 제 1항에 있어서, 상기 담배재료가, 벌리종 담배를 포함하는 담배재료.The tobacco material according to claim 1, wherein the tobacco material comprises Burley type tobacco. 1만∼6만달톤의 분자량을 갖는 착색 산성 수용성 고분자 물질의 함유율을 감소시키는 것에 의해 자극ㆍ매운 맛 원인성분을 저감시킨 담배 추출액을 포함하는 담배 향끽미제.A tobacco flavoring agent comprising a tobacco extract wherein the content of the coloring acidic water-soluble high molecular substance having a molecular weight of 10,000 to 60,000 daltons is reduced to reduce irritant and pungent ingredient. 삭제delete 제 4항에 있어서, 상기 담배 추출액이, 벌리종 담배 유래의 것인 담배 향끽미제.The tobacco flavor according to claim 4, wherein the tobacco extract is derived from Burley tobacco. 천연 담배재료로부터의 수계 추출액을 포함하는 향끽미제를 천연 담배재료의 추출 잔사인 섬유를 포함하는 재생 담배 웹에 첨가하여 이루어지는 재생 담배재료로서, 상기 향끽미제가 제 4항에 기재된 담배 추출액인 것을 특징으로 하는 재생 담배재료.A regenerated tobacco material formed by adding a flavoring agent comprising an aqueous extract from a natural tobacco material to a regenerated tobacco web comprising fibers as an extraction residue of a natural tobacco material, wherein said flavoring agent is a tobacco extract according to claim 4 Recycled tobacco material. 1만∼6만달톤의 분자량을 갖는 착색 산성 수용성 고분자 물질을 저감시키는 것을 포함하는 담배재료의 제조방법.A method for producing a tobacco material comprising reducing a coloring acidic water soluble high molecular substance having a molecular weight of 10,000 to 60,000 daltons. 천연 담배재료로부터의 수계 추출액으로부터, 1만∼6만달톤의 분자량을 갖는 착색 산성 수용성 고분자 물질을 저감시키는 것을 포함하는 향끽미제의 제조방법.A method for producing a flavoring agent comprising reducing a coloring acidic water-soluble high molecular substance having a molecular weight of 10,000 to 60,000 Daltons from an aqueous extract from a natural tobacco material.
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