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TW201511695A - A tobacco material and a method of making the same - Google Patents

A tobacco material and a method of making the same Download PDF

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Publication number
TW201511695A
TW201511695A TW103129487A TW103129487A TW201511695A TW 201511695 A TW201511695 A TW 201511695A TW 103129487 A TW103129487 A TW 103129487A TW 103129487 A TW103129487 A TW 103129487A TW 201511695 A TW201511695 A TW 201511695A
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Taiwan
Prior art keywords
extraction
solvent
tobacco
extract
raw material
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TW103129487A
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Chinese (zh)
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Naoyuki Ishida
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Japan Tobacco Inc
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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
    • A24B15/26Use of organic solvents for extraction
    • 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
    • A24B15/241Extraction of specific substances

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

This invention provides a tobacco material with good flavor and taste, and a method of making the same. The tobacco material is that a ration of weight of the extract obtained by extraction using n-hexane as solvent, and weight of the extract obtained by extraction using water as solvent after the extract obtained by extraction using n-hexane as solvent is 0 to 1.5 as ration of weight of the extract by water/weight of the extract by hexane.

Description

菸原料及其製造方法 Tobacco raw material and manufacturing method thereof

本發明係關於菸原料及其製造方法。 The present invention relates to a tobacco material and a method of producing the same.

就調整菸之香吸味的方法而言,從菸葉材料萃取除去特定之成分的技術、或對於菸葉材料一旦進行萃取操作,取得萃取液與萃取殘渣,對於所得到之萃取液進行預定的處理等之後,於萃取殘渣倒回其萃取液之技術已為人所知。 In the method of adjusting the flavor of the smoke, the technique of extracting and removing the specific component from the tobacco leaf material, or extracting the extract and the residue after the extraction of the tobacco leaf material, and performing predetermined treatment on the obtained extract liquid, etc. Thereafter, the technique of reclaiming the residue into the extract is known.

就從菸葉材料萃取除去特定之成分的技術而言,使用脂肪族烴與低級醇之混合溶劑,從菸除去脂質成分之技術已為人所知(日本專利文獻1)。 As a technique for extracting and removing a specific component from a tobacco leaf material, a technique of removing a lipid component from tobacco using a mixed solvent of an aliphatic hydrocarbon and a lower alcohol is known (Japanese Patent Document 1).

對於菸葉材料一旦進行萃取操作,於萃取殘渣倒回其萃取液之技術係以含有界面活性劑之溶液進行菸原料之萃取,除去萃取液中之界面活性劑與多肽之後,將其溶液添加於菸原料之方法已為人所知(日本專利文獻2)。 Once the tobacco leaf material is subjected to an extraction operation, the technique of extracting the residue into the extract is carried out by extracting the tobacco raw material with a solution containing a surfactant, removing the surfactant and the polypeptide in the extract, and then adding the solution to the smoke. A method of raw materials is known (Japanese Patent Document 2).

又,使用超臨界流體而處理菸原料,從藉處理所得到之萃取物除去亞硝胺,藉此從菸材料減少亞硝胺之方法已為人所知(日本專利文獻3)。 Further, a method of treating a tobacco raw material using a supercritical fluid and removing nitrosamine from the extract obtained by the treatment, thereby reducing nitrosamine from the tobacco material is known (Japanese Patent Document 3).

進一步,就另外之技術而言,透過使菸葉材料於加壓下浸漬於作為超臨界流體之二氧化碳中並使其後壓力降至大氣壓之操作,以使菸葉材料所含有之香吸味成分凝縮於菸葉之表面的技術已為人所知(日本專利文獻4)。 Further, in another technique, the tobacco leaf material is immersed in carbon dioxide as a supercritical fluid under pressure and the pressure is reduced to atmospheric pressure, so that the flavor component contained in the tobacco leaf material is condensed on The technique of the surface of the tobacco leaf is known (Japanese Patent Document 4).

[先前技術文獻] [Previous Technical Literature] [日本專利文獻] [Japanese Patent Literature]

[日本專利文獻1]日本特公昭58-4544号公報 [Japanese Patent Document 1] Japanese Patent Publication No. Sho 58-4544

[日本專利文獻2]日本特表平7-505521号公報 [Japanese Patent Document 2] Japanese Patent Publication No. 7-505521

[日本專利文獻3]日本特許第3931084号公報 [Japanese Patent Document 3] Japanese Patent No. 3913084

[日本專利文獻4]日本特開平8-23952号公報 [Japanese Patent Document 4] Japanese Patent Laid-Open Publication No. Hei 8-23952

菸葉材料係含有極性相異之許多成分,其等之成分係大致區分成低極性、高極性及兩極性之成分。有關此等之成分,以萃取進行除去時,例如若以低極性之溶劑進行萃取,則菸葉中之低極性與兩極性之成分群可被除去。 Tobacco material contains many components with different polarities, and its components are roughly divided into low polarity, high polarity and bipolar components. When such components are removed by extraction, for example, if extraction is carried out with a solvent of low polarity, the group of low polarity and bipolar components in the tobacco leaves can be removed.

相對於此,以高極性之溶劑進行萃取時,係菸葉材料中之高極性與兩極性之成分群可被除去。 On the other hand, when extracting with a solvent having a high polarity, a group of highly polar and bipolar components in the tobacco leaf material can be removed.

因此,以低極性或高極性之溶劑進行一次之萃取,係除了低極性或高極性之成分外,亦除去兩極性之成分群。藉此,有時對菸原料之香吸味的影響變大。 Therefore, one-time extraction with a solvent of low polarity or high polarity removes the component group of the two polarities in addition to the component of low polarity or high polarity. As a result, the influence on the flavor of the tobacco raw material is sometimes increased.

又,進行萃取之後,將其萃取物添加於菸原料之技術 中,係藉一次之萃取所得到之成分群係含有許多之成分,於其萃取物中施予處理(與抗氧化劑之接触等)之時,認為除了欲除去之成分外,影響香吸味之成分亦變化。因此,認為對香吸味之影響有變大的可能。 Moreover, after extracting, the technique of adding the extract to the raw material of the tobacco In the case where the extract obtained by one-time extraction contains a large number of components, when it is administered to the extract (contact with an antioxidant, etc.), it is considered that in addition to the component to be removed, the flavor is affected. The ingredients also change. Therefore, it is considered that the influence on the flavor is increased.

因如此之情事,本發明之課題在於提供香吸味良好之菸原料,以及提供製造其菸原料之方法。 In view of the above, an object of the present invention is to provide a tobacco raw material having a good scent and a method of producing a tobacco raw material.

本發明人經專心研究之結果,發現一種香吸味優異之菸原料,其係藉由使用正己烷作為溶劑的萃取所得到之萃取物之重量、及其萃取後進一步藉由使用水作為溶劑的萃取所得到之萃取物的重量之比,就水萃取物重量/己烷萃取物重量比,為0以上1.5以下。 As a result of intensive research, the present inventors have found a tobacco raw material excellent in flavor and taste, which is obtained by extracting n-hexane as a solvent, and further extracting water by using water as a solvent. The weight ratio of the extract obtained by the extraction is 0 or more and 1.5 or less in terms of the weight ratio of the water extract/hexane extract.

又,知道一種製造方法可解決上述課題,其係包含如下步驟:第一萃取步驟,其係使用介電率1以上、未達25之溶劑而萃取菸葉材料以得到萃取液及萃取殘渣;第二萃取步驟,其係於第一萃取步驟之後,將第一萃取步驟所得到之萃取殘渣使用介電率25以上之溶劑進行萃取而得到萃取殘渣;及,於經過第二萃取步驟所得到之萃取殘渣中,倒回第一萃取步驟所得到之萃取液而作為菸葉原料之步驟。終完成本發明。 Moreover, it is known that a manufacturing method can solve the above problems, and the method includes the following steps: a first extraction step of extracting a tobacco leaf material using a solvent having a dielectric constant of 1 or more and less than 25 to obtain an extract liquid and an extraction residue; An extraction step, after the first extraction step, extracting the extraction residue obtained in the first extraction step using a solvent having a dielectric constant of 25 or more to obtain an extraction residue; and extracting the residue obtained after the second extraction step In the middle, the step of extracting the extract obtained in the first extraction step as a raw material of tobacco leaves is carried out. The invention is finally completed.

亦即,本發明係如以下。 That is, the present invention is as follows.

[1]一種菸原料,其係藉由使用正己烷作為溶劑的萃取所得到之萃取物之重量、及其萃取後進一步藉由使用水作為溶劑的萃取所得到之萃取物的重量之比,就水萃取物重量/ 己烷萃取物重量比,為0以上1.5以下。 [1] A tobacco raw material which is a weight ratio of an extract obtained by extraction using n-hexane as a solvent, and a weight ratio of an extract obtained by extraction using water as a solvent after extraction, Water extract weight / The weight ratio of the hexane extract is 0 or more and 1.5 or less.

[2]如[1]項所述之菸原料,其中,藉由使用正己烷作為溶劑的萃取所得到之萃取物之重量、及其萃取後進一步藉由使用水作為溶劑的萃取所得到之萃取物的重量之合計量為萃取前之菸原料的重量之5至17重量%。 [2] The tobacco raw material according to [1], wherein the weight of the extract obtained by extraction using n-hexane as a solvent, and the extraction obtained by further extracting by using water as a solvent after extraction The total weight of the substance is 5 to 17% by weight based on the weight of the raw material of the smoke before extraction.

[3]一種菸原料之製造方法,其係包含如下步驟:第一萃取步驟,其係使用介電率1以上、未達25之溶劑而萃取菸葉材料以得到萃取液及萃取殘渣;第二萃取步驟,其係於第一萃取步驟之後,將第一萃取步驟所得到之萃取殘渣使用介電率25以上之溶劑進行萃取而得到萃取殘渣;及,於經過第二萃取步驟所得到之萃取殘渣中,倒回第一萃取步驟所得到之萃取液而作為菸葉原料之步驟。 [3] A method for producing a tobacco raw material, comprising: a first extraction step of extracting a tobacco leaf material using a solvent having a dielectric constant of 1 or more and less than 25 to obtain an extract liquid and an extraction residue; a step of extracting the extraction residue obtained in the first extraction step using a solvent having a dielectric constant of 25 or more to obtain an extraction residue; and, in the extraction residue obtained by the second extraction step, after the first extraction step And returning the extract obtained in the first extraction step as a step of the tobacco leaf raw material.

[4]如[3]項所述之製造方法,其中,於第一萃取步驟使用之溶劑為介電率1至20之溶劑,於第二萃取步驟使用之溶劑為水。 [4] The production method according to [3], wherein the solvent used in the first extraction step is a solvent having a dielectric constant of 1 to 20, and the solvent used in the second extraction step is water.

[5]如[3]或[4]項所述之製造方法,其中,於第一萃取步驟使用之溶劑為選自正己烷、四氫呋喃及乙醇之1種以上。 [5] The production method according to [3] or [4], wherein the solvent used in the first extraction step is one or more selected from the group consisting of n-hexane, tetrahydrofuran, and ethanol.

[6]一種菸原料,其係藉由如[3]至[5]項中任一項所述之製造方法所得到者。 [6] A tobacco raw material obtained by the production method according to any one of [3] to [5].

[7]一種菸製品,其係使用如[1]、[2]或[6]所述之菸原料的菸製品。 [7] A smoking article which is a smoking article using the tobacco raw material according to [1], [2] or [6].

又,本說明書中所謂之「菸葉材料」係用以製造「菸原料」所使用者,經過萃取步驟等之處理之前的菸葉。本說明書中所謂「菸原料」係對上述「菸葉材料」 加入萃取步驟等之處理所得到者。 In addition, the "tobacco material" used in the present specification is a tobacco leaf used to manufacture a user of "smoke raw material" after being subjected to an extraction step or the like. The term "smoke raw material" in this specification refers to the above "smoke material". The person obtained by the treatment of the extraction step or the like is added.

若依本發明,可提供香吸味良好之菸原料與其製造方法。 According to the present invention, it is possible to provide a tobacco material which is good in flavor and taste and a method for producing the same.

第1圖表示實施例3與比較例2之官能評價結果的圖。 Fig. 1 is a view showing the results of the sensory evaluation of Example 3 and Comparative Example 2.

第2圖表示實施例4與比較例3之官能評價結果的圖。 Fig. 2 is a graph showing the results of the sensory evaluation of Example 4 and Comparative Example 3.

第3圖表示實施例5與比較例4之官能評價結果的圖。 Fig. 3 is a graph showing the results of the sensory evaluation of Example 5 and Comparative Example 4.

第4圖表示實施例6及比較例1之官能評價結果的圖。 Fig. 4 is a view showing the results of the sensory evaluation of Example 6 and Comparative Example 1.

第5圖表示比較例5與比較例6之官能評價結果的圖。 Fig. 5 is a graph showing the results of the sensory evaluation of Comparative Example 5 and Comparative Example 6.

第6圖表示比較例7之官能評價結果的圖。 Fig. 6 is a graph showing the results of the sensory evaluation of Comparative Example 7.

以下,顯示實施形態及例示物等而詳細說明本發明,但本發明並非受以下之實施形態及例示物等所限定,在不超出本發明之要旨的範圍內可任意變更而實施。 In the following, the present invention will be described in detail with reference to the accompanying drawings, and the embodiments of the present invention, and the present invention is not limited by the scope of the invention.

<本發明之製造方法> <Manufacturing Method of the Present Invention>

本發明之菸原料的製造方法係包含如下步驟:第一萃取步驟,其係使用介電率1以上、未達25之溶劑而萃取菸葉材料以得到萃取液及萃取殘渣;第二萃取步驟,其係於第一萃取步驟之後,將第一萃取步驟所得到之萃取殘渣使用介電率25以上之溶劑進行萃取而得到萃取殘渣;及,於經過第二萃取步驟所得到之萃取殘渣,倒回第一萃取步驟所得到之萃取液而作為菸葉原料之步驟。 The method for producing a tobacco raw material of the present invention comprises the following steps: a first extraction step of extracting a tobacco leaf material using a solvent having a dielectric constant of 1 or more and less than 25 to obtain an extract liquid and a extraction residue; and a second extraction step; After the first extraction step, the extraction residue obtained in the first extraction step is extracted with a solvent having a dielectric constant of 25 or more to obtain an extraction residue; and the extraction residue obtained after the second extraction step is returned to the first The step of extracting the extract obtained as the raw material of the tobacco leaf.

本發明之菸原料之製造方法中,第一萃取步驟係包含使用介電率1以上、未達25之溶劑而萃取菸葉材料以得到萃取液與萃取殘渣的步驟。 In the method for producing a tobacco raw material of the present invention, the first extraction step includes a step of extracting the tobacco leaf material using a solvent having a dielectric constant of 1 or more and less than 25 to obtain an extract liquid and an extraction residue.

對於本發明所使用之菸葉材料,其種類係無特別限定,可舉例如菸草(Nicotiana)屬,菸草菸膠之黄色種、Burley種、圓葉菸草(Nicotiana rustica)之巴西利亞種等。 The type of the tobacco leaf material used in the present invention is not particularly limited, and examples thereof include the genus Nicotiana, the yellow species of tobacco smear, the Burley species, and the Brasilia species of Nicotiana rustica.

此等之菸葉材料係使用如粉碎機之適當的手段而裁切成適當大小(粒徑為0.425至1.18mm左右),可使用以公知之方法乾燥者。 These tobacco leaf materials are cut to an appropriate size (having a particle diameter of about 0.425 to 1.18 mm) by a suitable means such as a pulverizer, and can be dried by a known method.

使用介電率為1以上、未達25之溶劑而萃取經過上述處理之菸葉材料,藉此可萃取菸葉材料所含有之所希望的香吸味成分。 The tobacco leaf material subjected to the above treatment is extracted using a solvent having a dielectric constant of 1 or more and less than 25, whereby the desired flavor component contained in the tobacco leaf material can be extracted.

第一萃取步驟使用的溶劑,更佳為介電率為1以上20以下者。 The solvent used in the first extraction step is more preferably one having a dielectric constant of 1 or more and 20 or less.

介電率為1以上、未達25之溶劑係可舉例如乙醇、異丙醇、醋酸乙酯、具有直鏈或支鏈的碳數5至10之烷、正丙醇、丁醇、苯、甲苯、二甲苯、苯甲基醇、丙酮、四氫呋喃、二乙基醚、1,4-二噁烷、氯仿、二氯甲烷。 Examples of the solvent having a dielectric constant of 1 or more and less than 25 include ethanol, isopropanol, ethyl acetate, a linear or branched carbon number of 5 to 10, n-propanol, butanol, and benzene. Toluene, xylene, benzyl alcohol, acetone, tetrahydrofuran, diethyl ether, 1,4-dioxane, chloroform, dichloromethane.

前述之烷係可舉例如戊烷、正己烷、環己烷、庚烷、辛烷、壬烷、癸烷。 The above-mentioned alkane may, for example, be pentane, n-hexane, cyclohexane, heptane, octane, decane or decane.

上述之中係可舉例如不使用醋酸乙酯之低分子的有機酸酯的態樣。 Among the above, for example, a state in which a low molecular organic acid ester of ethyl acetate is not used can be mentioned.

上述之中較佳可使用的溶劑可舉例如乙醇、正己烷、庚烷、二乙醚、四氫呋喃。 The solvent which can be preferably used among the above may, for example, be ethanol, n-hexane, heptane, diethyl ether or tetrahydrofuran.

上述之介電率為1以上、未達25之溶劑係可使用1種,亦可混合複數種而使用。使用經混合之溶劑時,係調製成經混合之溶劑的介電率為1以上、未達25。 The solvent having a dielectric constant of 1 or more and less than 25 may be used alone or in combination of plural kinds. When the solvent to be mixed is used, the dielectric ratio of the solvent to be mixed is 1 or more and less than 25.

萃取係可在常溫常壓下進行,亦可加溫至例如40至80℃左右而在加壓下之1000至2000psi進行。 又,以SI單位系顯示壓力時,以1psi≒6894.757Pa之換算式進行計算。 The extraction system can be carried out at normal temperature and pressure, or can be heated to, for example, about 40 to 80 ° C and at 1000 to 2000 psi under pressure. Further, when the pressure is displayed in the SI unit system, the calculation is performed in a conversion formula of 1 psi ≒ 689.957.

萃取時間係無特別制限,但可舉例如5分鐘至1小時。 The extraction time is not particularly limited, but may be, for example, 5 minutes to 1 hour.

萃取係可為1次,亦可以複數次進行。又,萃取係使用後述之高速溶劑萃取裝置而進行。 The extraction system can be carried out once or several times. Further, the extraction was carried out using a high-speed solvent extraction apparatus to be described later.

第一萃取步驟中,亦可適宜設置分開萃取液與萃取殘渣之操作。可舉例如將萃取物倒入於至具有適當孔徑之濾紙或篩網,分開成萃取液與萃取殘渣之方法。 In the first extraction step, the operation of separating the extract and extracting the residue may be appropriately set. For example, a method of pouring the extract into a filter paper or a sieve having a suitable pore diameter and separating it into an extract and a residue for extraction may be mentioned.

所得到之萃取殘渣係以適當方法乾燥之。乾燥方法可舉例如凍結乾燥。 The resulting extraction residue is dried by a suitable method. The drying method can be, for example, freeze-drying.

對經過上述之第一萃取步驟所得到之萃取殘渣,使用介電率為25以上之溶劑而進一步進行萃取操作,可萃取未於第一萃取步驟萃取的菸葉材料中之成分。 The extraction residue obtained by the first extraction step described above is further subjected to an extraction operation using a solvent having a dielectric constant of 25 or more, and the components in the tobacco material not extracted in the first extraction step may be extracted.

使用於第二萃取步驟之介電率為25以上之溶劑係無特別制限,但可舉例如水、甲醇、含有其等之混合溶劑等。 The solvent used in the second extraction step having a dielectric constant of 25 or more is not particularly limited, and examples thereof include water, methanol, and a mixed solvent containing the same.

第二萃取步驟之萃取的條件係可與第一萃取步驟同樣地,在常溫常壓下進行,亦可加溫至40至80℃左右,並進一步加壓下以1000至2000psi進行萃取。 The extraction conditions of the second extraction step may be carried out at normal temperature and pressure in the same manner as in the first extraction step, or may be heated to about 40 to 80 ° C, and further extracted at 1000 to 2000 psi under pressure.

萃取時間係無特別制限,但可舉例如5分鐘至1小時。 The extraction time is not particularly limited, but may be, for example, 5 minutes to 1 hour.

萃取係可為1次,亦可進行複數次。萃取係亦可使用後述之高速溶劑萃取裝置而進行。 The extraction system can be one time or multiple times. The extraction system can also be carried out using a high-speed solvent extraction apparatus to be described later.

第一萃取步驟及第二萃取步驟中,相較於第一萃取步驟使用之溶劑,第二萃取步驟使用之溶劑的介電率高,藉此,可於第二萃取步驟萃取在第一萃取步驟未被萃取出之菸葉材料中之成分。第二萃取步驟所得到之萃取液係不倒回萃取殘渣中。 In the first extraction step and the second extraction step, the solvent used in the second extraction step has a higher dielectric constant than the solvent used in the first extraction step, whereby the second extraction step can be extracted in the first extraction step. An ingredient in the tobacco material that has not been extracted. The extract obtained in the second extraction step is not poured back into the extraction residue.

第二萃取步驟中,可從第一萃取步驟所得到之萃取殘渣除去菸葉材料所含有之不必要的成分。 In the second extraction step, unnecessary components contained in the tobacco leaf material can be removed from the extraction residue obtained in the first extraction step.

不必要的成分係可舉例如高極性之成分,例如包含低分子之有機酸或氨等。 The unnecessary components are, for example, highly polar components such as organic acids or ammonia containing a low molecular weight.

本發明之製造方法係採用第一萃取步驟及第二萃取步驟之順序,亦即最初之萃取使用的溶劑為比較低極性者,在其次之萃取步驟使用的溶劑,相較於第一萃取步驟使用的溶劑,使用介電率為比較大的高極性之溶劑乃很重要。若此順序相反,則無法得到香吸味良好的菸原料。 The manufacturing method of the present invention adopts the sequence of the first extraction step and the second extraction step, that is, the solvent used in the initial extraction is relatively low polarity, and the solvent used in the second extraction step is used in comparison with the first extraction step. For the solvent, it is important to use a solvent having a relatively high dielectric polarity. If the order is reversed, a tobacco material having a good scent is not obtained.

可使第一萃取步驟進行複數次之後使第二萃取步驟進行複數次,亦可反複使第一萃取步驟及第二萃取步驟連續進行,其後,又進行第一萃取步驟,而進一步進行第二萃取步驟。 After the first extraction step is performed plural times, the second extraction step is performed plural times, and the first extraction step and the second extraction step may be repeated continuously, and then the first extraction step is performed, and the second extraction step is further performed. Extraction step.

第一萃取步驟及第二萃取步驟之合計之步驟次數,從製造步驟之簡略化觀點而言,較佳為較少者。 The number of steps of the total of the first extraction step and the second extraction step is preferably from the viewpoint of simplification of the production step.

本發明之製造方法係包含:經過第二萃取步驟之後,於經過第二萃取步驟所得到之萃取殘渣中,倒 回第一萃取步驟所得到之萃取液而作為菸葉原料之步驟。 The manufacturing method of the present invention comprises: after the second extraction step, in the extraction residue obtained through the second extraction step, pouring The step of returning the extract obtained in the first extraction step as a raw material of tobacco leaves.

此步驟係將第一萃取步驟所得到之萃取液倒回於第二萃取步驟所得到之萃取殘渣,藉此在第一萃取步驟所萃取之使菸原料香吸味良好的成分被返回菸原料。 In this step, the extract obtained in the first extraction step is poured back to the extraction residue obtained in the second extraction step, whereby the components extracted in the first extraction step to make the tobacco raw material have good taste are returned to the tobacco raw material.

將萃取液倒回萃取殘渣之時,從保持菸原料之品質之均一性的觀點而言,較佳為使萃取液均等地遍佈於萃取殘渣之方式。 When the extract is poured back to the extraction residue, from the viewpoint of maintaining the uniformity of the quality of the tobacco raw material, it is preferred to uniformly distribute the extract to the extraction residue.

第一萃取步驟所得到之萃取液,係可直接倒回,亦可倒回只濃縮溶劑者。又,對於萃取液係亦可實施塩析處理。 The extract obtained in the first extraction step can be directly poured back, or can be poured back to the solvent only. Further, a decanting treatment may be performed on the extract liquid system.

將萃取液倒回萃取殘渣之後,係以適當方法除去溶劑。 After the extract is poured back to the extraction residue, the solvent is removed by an appropriate method.

藉此,可得到本發明之菸原料。 Thereby, the tobacco raw material of the present invention can be obtained.

藉本發明之製造方法所得到之菸原料,就其使用態樣而言,可舉例如在常溫使用之態樣,及以加溫之状態使用的態樣,其任一之使用態樣香吸味皆優異。 The tobacco raw material obtained by the production method of the present invention may be used in a state of use at room temperature or in a state of being heated, for example, in any aspect of use. The taste is excellent.

在常溫或加熱之條件下使用的態樣,係可舉例如於直徑0.7mm之管,填充經上述處理之菸葉而使用的態樣。 The aspect to be used under normal temperature or heating conditions is, for example, a tube having a diameter of 0.7 mm and filled with the tobacco leaf treated as described above.

以經加溫之状態使用的態樣,可舉例如加溫至例如40至70℃左右而使用之態樣。 The aspect used in the state of being heated may be, for example, a state in which it is heated to, for example, about 40 to 70 ° C.

<本發明之菸原料> <The raw material of tobacco of the present invention>

本發明之菸原料係藉由使用正己烷作為溶劑的萃取所得到之萃取物(以下,亦稱為己烷萃取物)、及其萃取後進一步藉由使用水作為溶劑的萃取所得到之萃取物(以下,稱為水萃取物)之重量之比,就水萃取物重量/己烷萃取物重量之數值(亦稱為W/H比)而言,為0以上1.5以下。 The tobacco raw material of the present invention is an extract obtained by extraction using n-hexane as a solvent (hereinafter, also referred to as a hexane extract), and an extract obtained by extraction using water as a solvent after extraction. The ratio of the weight of the water extract (hereinafter referred to as water extract) is 0 or more and 1.5 or less in terms of the value of the water extract weight/hexane extract weight (also referred to as W/H ratio).

菸原料具有如上述之W/H比,藉此成為香吸味良好的菸原料。若W/H比超過1.5,亦即若水萃取物之含量變得太多,於菸原料之香吸味會混入雜味。 The tobacco raw material has a W/H ratio as described above, whereby it becomes a smoke raw material having a good scent. If the W/H ratio exceeds 1.5, that is, if the content of the water extract becomes too much, the flavor of the tobacco material will be mixed with the taste.

又,W/H比係可舉例如0.3以上0.6以下之態樣。 Further, the W/H ratio may be, for example, 0.3 or more and 0.6 or less.

又,本發明之菸原料中的己烷萃取物及水萃取物之合計之重量,相對於萃取前之菸原料之重量,可舉例如5至17重量%之態樣。又,可舉例如5至14重量%之態樣。 Further, the total weight of the hexane extract and the water extract in the tobacco raw material of the present invention may be, for example, 5 to 17% by weight based on the weight of the raw material of the tobacco before extraction. Further, for example, it is 5 to 14% by weight.

為製造具有如上述之W/H比的菸原料,可使用例如上述本發明的菸原料之製造方法。 In order to produce a tobacco raw material having a W/H ratio as described above, for example, a method for producing a tobacco raw material of the present invention described above can be used.

又,藉由菸原料中使用正己烷作為溶劑的萃取所得到之萃取物量、及藉由其後以水作為溶劑所使用的萃取所得到之萃取物量之測定方法係使用以下之方法。具體上係使用高速溶劑萃取裝置(DIONEX公司、ASE200),使22ml之體積裝入於耐壓金屬製萃取格室以菸原料成為1.0g/cell之方式,準備填充有試料之格室。將當該格室具備於前述高速溶劑萃取裝置上,以如下之表所示的條件進行萃取。 In addition, the following method is used for the measurement method of the amount of the extract obtained by the extraction using the hexane as a solvent and the amount of the extract obtained by the extraction using the water as a solvent. Specifically, a high-speed solvent extraction apparatus (DIONEX Co., Ltd., ASE 200) was used, and a volume of 22 ml was placed in a pressure-resistant metal extraction cell so that the raw material of the sample was 1.0 g/cell, and a cell filled with the sample was prepared. When the cell was provided on the aforementioned high-speed solvent extraction apparatus, extraction was carried out under the conditions shown in the following table.

在上述之萃取中,萃取液係被移送至裝置專用之玻璃製小瓶,但萃取此後進行回收,使用於萃取量之測定(方法係參照下述)。溶劑萃取係以溶劑之加壓填充、加溫、靜置、除氣(將溶劑移送至小瓶)、再度之溶劑的加壓填充為1循環,正己烷之情形係重複3循環,從1個格室所得到之全液量回收至1個小瓶中。繼而實施之水萃取之情形係合計重複9循環,將從3循環所得到之全液量回收至1個小瓶,可從1個格室得到合計3小瓶。 In the above extraction, the extract is transferred to a glass vial for the device, but after the extraction, it is recovered and used for the measurement of the extraction amount (the method is as follows). Solvent extraction is filled with solvent, heated, allowed to stand, degassed (transfer the solvent to the vial), and the pressurized filling of the solvent is 1 cycle, and the case of n-hexane is repeated for 3 cycles, from 1 grid. The total amount of liquid obtained in the chamber was recovered into one vial. The water extraction which was carried out was repeated for 9 cycles in total, and the total liquid amount obtained from the 3 cycles was recovered to 1 vial, and a total of 3 vials were obtained from one cell.

正己烷萃取物量之測定係依以下之方法進行。 The amount of n-hexane extract was measured by the following method.

使用正己烷、醋酸乙酯、乙醇,將1小瓶/1格室之正己烷萃取液移至預先秤量之100ml茄型燒杯中,進一步洗入小瓶,將全部之萃取物回收至茄型燒杯中。使茄型燒杯以旋轉蒸發器減壓濃縮後,進一步以3小時減壓油封幫浦在常溫、減壓下乾燥。濃縮係使用安裝有捕集球之旋轉蒸發器,水槽之液溫係設定為25℃以下。測定乾燥後之茄型燒杯之重量,以差分作為正己烷萃取物量。 Using n-hexane, ethyl acetate, and ethanol, 1 vial/1 compartment of the n-hexane extract was transferred to a pre-weighed 100 ml eggplant type beaker, further washed into a vial, and the entire extract was recovered into an eggplant type beaker. The eggplant type beaker was concentrated under reduced pressure on a rotary evaporator, and further dried under reduced pressure at a normal temperature and reduced pressure for 3 hours under reduced pressure. The concentrating system uses a rotary evaporator equipped with a collecting ball, and the liquid temperature of the water tank is set to 25 ° C or lower. The weight of the dried eggplant beaker was measured, and the difference was used as the amount of n-hexane extract.

有關水萃取物量之測定係依以下之方法進行。 The measurement of the amount of the water extract was carried out in the following manner.

使用超純水而將3小瓶/1格室之水萃取液移至預先秤量之500ml凍結乾燥用共通匹配茄型燒杯,進一步洗入小瓶,將全部之萃取物回收至茄型燒杯。將茄型燒杯以凍結乾燥裝置之預備凍結槽凍結後,連接至凍結乾燥裝置並乾燥。測定乾燥後之茄型燒杯之重量,以差分作為水萃取物收量。 The ultra-pure water was used to transfer the 3 vials/1 cell water extract to a pre-weighed 500 ml freeze-drying common matching eggplant beaker, further washed into the vial, and the entire extract was recovered to the eggplant beaker. The eggplant type beaker was frozen in a preliminary freezing tank of the freeze-drying apparatus, and then connected to a freeze-drying apparatus and dried. The weight of the dried eggplant beaker was measured, and the difference was taken as the water extract.

[實施例] [Examples]

藉實施例而更具體地說明本發明,但本發明係只要不超出其要旨,並不受以下之實施例之記載所限定。 The present invention will be more specifically described by the examples, but the present invention is not limited by the description of the examples below.

以下,藉實施例而進一步具體地說明本發明,但本發明係只要不超出其要旨,並不受以下之實施例之記載所限定。 Hereinafter, the present invention will be specifically described by way of examples, but the present invention is not limited by the description of the examples below.

<實施例1> <Example 1>

以粉碎機粉碎菸葉材料(國產Barley種)。 The tobacco leaf material (made by domestic Barley species) was pulverized by a pulverizer.

粉碎機係使用協立理工(股)製之試樣研磨機SK-M10。 The pulverizer was a sample grinder SK-M10 manufactured by Kyoritsu Seiko Co., Ltd.

繼而經過篩網,可得到粒徑成為0.425mm至1.18mm之粉碎菸葉材料。正確量取此粉碎菸葉材料2g,填充於金屬製之格室中。 Then, through the screen, a pulverized tobacco material having a particle diameter of 0.425 mm to 1.18 mm can be obtained. The 2 g of the pulverized tobacco leaf material was accurately weighed and filled in a metal cell.

填充時所產生之空隙係使用不銹鋼製之珠粒而填入。格室係使用DIONEX(股)製之22mL萃取格室,珠粒係使用中央科學貿易之粒徑2.2mm。因於此格室送入溶劑,進行 粉碎菸葉材料之萃取,故使用高速溶劑萃取機。 The voids generated during filling are filled with beads made of stainless steel. The cell system used a 22 mL extraction cell made of DIONEX (shares), and the beads used a central scientific trade size of 2.2 mm. Because the cell is fed with solvent, The pulverized tobacco leaf material is extracted, so a high speed solvent extraction machine is used.

萃取器係使用DIONEX(股)製之高速溶劑萃取裝置ASE-200。 The extractor was a high-speed solvent extraction apparatus ASE-200 manufactured by DIONEX.

萃取係使用正己烷(介電率:2)、乙醇(介電率:24)之介電率為1以上、未達25之溶劑。 The extraction system used a solvent having a dielectric constant of 1 or more and a ratio of not more than 25 in n-hexane (dielectric ratio: 2) and ethanol (dielectric ratio: 24).

以使用此等溶劑之上述萃取機之萃取係以首先於格室中填充溶劑,加溫後靜置,將押出格室內的溶劑之順序重複進行三次。又,各溶劑在加溫時之溫度及靜置時之壓力條件係如以下般。 The extraction system of the above extraction machine using these solvents is first filled with a solvent in a cell, and after standing, it is allowed to stand, and the solvent in the cell chamber is repeated three times in this order. Further, the temperature at the time of heating and the pressure conditions at the time of standing are as follows.

正己烷:70℃、2000psi Hexane: 70 ° C, 2000 psi

乙醇:80℃、2000psi Ethanol: 80 ° C, 2000 psi

所得到之以上述溶劑的萃取液係約為40mL,但使用蒸發器進行濃縮,使用與萃取時使用之溶劑相同的溶劑而以懸濁状定溶成為6.25mL。繼而以溶劑之水(介電率:80)進行萃取。萃取之時,係採取與介電率為1以上、未達25之溶劑之萃取同樣之順序,但加溫時之溫度及靜置時之壓力條件係100℃、2000psi,將以介電率為1以上、未達25之溶劑之萃取時係3次之循環,改為以水進行之萃取係9次之循環。萃取液之総量係大概為120mL。 The extract obtained by the above solvent was about 40 mL, but it was concentrated using an evaporator, and dissolved in a suspension in the same solvent as the solvent used for the extraction to 6.25 mL. Extraction was then carried out with water of a solvent (dielectric ratio: 80). At the time of extraction, the same procedure as the extraction of a solvent having a dielectric constant of 1 or more and less than 25 is adopted, but the temperature at the time of heating and the pressure condition at the time of standing are 100 ° C, 2000 psi, and the dielectric ratio is When the extraction of the solvent of 1 or more and less than 25 is carried out for 3 cycles, the extraction by water is changed to 9 cycles. The amount of the extract is approximately 120 mL.

殘留於萃取後之格室的萃取殘渣係無殘留地回收,預備凍結之後,供應至凍結乾燥。預備凍結及凍結乾燥係使用EYELA製之FREEZE DRYER FD-81。 The extraction residue remaining in the cells after the extraction is recovered without residue, and after preliminary freezing, it is supplied to freeze-drying. The pre-freeze and freeze-drying system uses FREEZE DRYER FD-81 made by EYELA.

以上述作成的低極性溶劑所產生的萃取液全量無結塊地倒回於乾燥後之萃取殘渣,可得到本發明之菸原料。 The tobacco raw material of the present invention can be obtained by pouring the entire amount of the extract produced by the above-described low-polarity solvent to the extracted residue after drying without agglomeration.

於各實施例所使用的溶劑係如下。 The solvents used in the respective examples are as follows.

使用正己烷之例:實施例1 Example using n-hexane: Example 1

使用乙醇的例:實施例2 Example of using ethanol: Example 2

又,以在第一萃取步驟中使用甲醇(介電率:33)作為溶劑所得到的菸原料之例作為比較例1。 Further, as an example of the comparative example 1, a tobacco raw material obtained by using methanol (dielectric ratio: 33) as a solvent in the first extraction step was used.

對於實施例1、2及比較例1之菸原料,測定氨之含量。菸原料中之氨之含量之測定係依以下之順序而進行。 For the tobacco materials of Examples 1, 2 and Comparative Example 1, the content of ammonia was measured. The determination of the content of ammonia in the raw material of the tobacco is carried out in the following order.

<氨分析> <Ammonia analysis>

未處理原料(180mg)或處理原料(處理未處理原料180mg時之重量)以純水5mL浸透萃取30分鐘。其後,藉10KDa之極限過濾膜過濾萃取液。使濾液以Agilent Technologies製毛細管電氣泳動色層分析儀進行分析。吸光度係設為波長280nm,氨係使用氯化銨水溶液稀釋成適當濃度之標準溶液而定量成銨離子。 The untreated raw material (180 mg) or the treated raw material (the weight at which 180 mg of the untreated raw material was treated) was soaked in 5 mL of pure water for 30 minutes. Thereafter, the extract was filtered through a 10 KDa limit filter membrane. The filtrate was analyzed by a capillary electrophoresis chromatography analyzer manufactured by Agilent Technologies. The absorbance was set to a wavelength of 280 nm, and ammonia was diluted with an aqueous solution of ammonium chloride to a standard solution of an appropriate concentration to quantify ammonium ions.

所定量之值換算成每原料重量之結果表示於表2。又,處理原料係使用未處理時之原料重量而換算出。(起因於處理所造成的重量減少之差異的影響除外。) The results of the quantified values converted to the weight per raw material are shown in Table 2. Further, the raw material to be treated was converted into the weight of the raw material at the time of untreated. (Except for the effect of the difference in weight reduction caused by the treatment.)

從上述表2之結果,可知於第一萃取步驟使用介電率1以上、未達25的溶劑,於經過第二萃取步驟之後,在第一萃取步驟所得到之萃取液倒回萃取殘渣中之情形,係相較於第一萃取步驟使用介電率為25以上之溶劑之情形,很多氨被選擇性地除去。 From the results of the above Table 2, it is understood that the first extraction step uses a solvent having a dielectric constant of 1 or more and less than 25, and after the second extraction step, the extract obtained in the first extraction step is poured back into the extraction residue. In the case where a solvent having a dielectric constant of 25 or more is used as compared with the first extraction step, a large amount of ammonia is selectively removed.

<官能評價> <Functional evaluation>

對於依本發明之製造方法所得到之菸原料,以與實施例1相同的條件所製作者(實施例3)、於實施例1中只進行倒回經過第一萃取步驟所得到之萃取液的操作所得到之(無第二萃取步驟)比較例2、在實施例1中除了使用巴西產黄色種作為菸葉材料以外係進行相同的操作所得到之實施例4、在實施例4中只進行倒回經過第一萃取步驟所得到之萃取液的操作所得到之(無第二萃取步驟)比較例3、以與實施例3相同的菸葉材料及經過操作所得到之實施例5,及以與比較例2相同的菸葉材料及經過操作所得到之比較例4,進行如以下之官能評價。官能評價之期間,進行以下之操作。 The raw material of the tobacco obtained by the production method of the present invention was produced under the same conditions as in Example 1 (Example 3), and in Example 1, only the extract obtained by the first extraction step was poured back. The operation was carried out (without the second extraction step). In Comparative Example 2, Example 4 obtained by performing the same operation except that the yellow species produced in Brazil was used as the tobacco leaf material in Example 1 was only poured in Example 4. Back to the operation of the extract obtained by the first extraction step (without the second extraction step), Comparative Example 3, the same tobacco material as in Example 3, and Example 5 obtained by operation, and comparison with In the same tobacco material of Example 2 and Comparative Example 4 obtained by the operation, the following functional evaluation was carried out. During the period of functional evaluation, the following operations were performed.

(實施例3、4及比較例2、3) (Examples 3 and 4 and Comparative Examples 2 and 3)

將進行粉碎並篩選之未處理材料(粒徑0.425mm至1.18mm)及各菸原料(實施例3、4、比較例2、3)填充至石英管(外徑9mm×內徑7mm×長55mm)。 The untreated material (particle diameter 0.425 mm to 1.18 mm) and each of the tobacco materials (Examples 3, 4, Comparative Examples 2, and 3) which were pulverized and sieved were filled into a quartz tube (outer diameter 9 mm × inner diameter 7 mm × length 55 mm) ).

填充量,無未處理原料以及萃取物之除去時係180mg,於步驟包含萃取物之除去之處理原料時,係考量不倒回水萃取分之重量減少分,為109mg(處理180mg之原料時所得到之原料重量)。石英管之兩端係以不銹鋼製之網密封,避免伴隨抽吸之評價時的試樣飛濺。對於此等之石英管,加熱至60℃,從石英管之一端抽吸,調查與未處理之原料比較的結果。 The filling amount is 180 mg when there is no untreated raw material and the extract is removed. When the raw material containing the extract is removed in the step, the weight reduction of the non-returned water extract is considered to be 109 mg (when processing 180 mg of the raw material) The weight of the raw material obtained). The ends of the quartz tube are sealed with a stainless steel mesh to avoid splashing of the sample accompanying the evaluation of the suction. For these quartz tubes, heat to 60 ° C, suction from one end of the quartz tube, and investigate the results compared with the untreated raw materials.

<官能評價之方法> <Method of Functional Evaluation>

官能評價(吸感之變化)之基準係如以下。變化比率係與未處理之原料比較而以下述之文字表現的7段階評價進行判斷。又在全部之評價中被驗者數為10名。評價結果係利用最小有意義差法(LSD),判斷以處理方法進行官能評價結果差異之有意義性。結果表示於第1及2圖中。 The basis for the functional evaluation (change in sensation of sensation) is as follows. The change ratio is judged by the 7-stage evaluation expressed by the following text in comparison with the untreated raw material. In addition, the number of subjects examined was 10 in all evaluations. The evaluation results were judged by the least significant difference method (LSD) to judge the significance of the difference in the results of the functional evaluation by the treatment method. The results are shown in Figures 1 and 2.

(1)非常強:+3 (1) Very strong: +3

(2)強:+2 (2) Strong: +2

(3)略強:+1 (3) Slightly strong: +1

(4)不變:±0 (4) unchanged: ±0

(5)稍弱:-1 (5) slightly weaker: -1

(6)弱:-2 (6) Weak: -2

(7)非常弱:-3 (7) Very weak: -3

從第1及2圖之結果,可看到以最小有意義差法之檢定,係於實施例及比較例之間有95%有意義差,可看到本發明之製造方法所產生的效果。 From the results of Figs. 1 and 2, it can be seen that the test with the least significant difference method is 95% meaningful difference between the examples and the comparative examples, and the effect produced by the manufacturing method of the present invention can be seen.

從此事,可知無關於國內產Barley種及巴西產黄色種之菸葉材料的品種之差,依本發明之製造方法所得到之菸原料係發揮優異之香吸味。 From this, it can be seen that the difference in the variety of the domestically produced Barley species and the tobacco leaf material produced in Brazil is excellent in the flavor of the tobacco material obtained by the production method of the present invention.

(實施例5及比較例4) (Example 5 and Comparative Example 4)

將進行粉碎並篩選之未處理原料(粒徑0.425mm至1.18mm)及各菸原料(實施例5及比較例4)填充至塑膠管(外徑9mm×內徑7mm×長110mm)。 The untreated raw materials (particle diameter: 0.425 mm to 1.18 mm) and each of the tobacco materials (Examples 5 and 4) which were pulverized and sieved were filled in a plastic tube (outer diameter 9 mm × inner diameter 7 mm × length 110 mm).

填充量,無未處理原料以及萃取物之除去時為360mg,於步驟包含萃取物之除去的處理原料時,係考量不倒回水萃取分之重量減少分,為218mg(處理360mg之原料時所得到之原料重量)。石英管之兩端係以不織布之網密封,避免伴隨抽吸之評價時的試樣飛濺。使此塑膠管於室溫,從塑膠管之一端抽吸,調查與未處理之原料比較的結果。結果表示於第3圖。 The filling amount is 360 mg when there is no untreated raw material and the removal of the extract, and when the processing raw material including the removal of the extract is included in the step, the weight reduction of the non-returned water extract is considered to be 218 mg (when processing 360 mg of the raw material) The weight of the raw material obtained). Both ends of the quartz tube are sealed with a non-woven net to avoid splashing of the sample accompanying the evaluation of suction. The plastic tube was suctioned from one end of the plastic tube at room temperature to investigate the results compared with the untreated material. The results are shown in Figure 3.

與實施例3及4、比較例2及3同樣地,對於實施例5及比較例4亦進行評價。其結果,以最小有意義差法進行檢定,於實施例5及比較例4之間有95%有意義差,可看到本發明之製造方法所產生的效果。 Similarly to Examples 3 and 4 and Comparative Examples 2 and 3, Example 5 and Comparative Example 4 were also evaluated. As a result, the test was carried out by the least significant difference method, and 95% of the difference between Example 5 and Comparative Example 4 was significant, and the effect produced by the production method of the present invention can be seen.

<實施例6> <Example 6>

於第一萃取步驟使用於萃取之溶劑,除使用四氫呋喃(介電率:8)以外係藉由與實施例1同樣之順序,製作菸原 料。 In the first extraction step, the extraction solvent was used, and the tobacco was produced in the same order as in Example 1 except that tetrahydrofuran (dielectric ratio: 8) was used. material.

對於實施例6之菸原料(104.94mg)及於比較例1製作之菸原料(第一萃取步驟使用於萃取之溶劑,係使用甲醇)(134.55mg),以與實施例3、4及比較例2、3相同的方法進行官能評價(吸感之變化)。 The tobacco raw material of Example 6 (104.94 mg) and the raw material of the tobacco produced in Comparative Example 1 (the first extraction step used in the extraction solvent, methanol was used) (134.55 mg), and Examples 3, 4 and Comparative Examples 2, 3 The same method for functional evaluation (change in sorption).

結果表示於第4圖中。 The results are shown in Figure 4.

<比較例5及6> <Comparative Examples 5 and 6>

與實施例1相同地進行粉碎處理國產Barley種之菸葉材料,不進行第一萃取步驟,而只進行第二萃取步驟(只以水進行萃取),依其第二萃取步驟所得到之萃取液倒回萃取殘渣,製作比較例5之菸原料。 In the same manner as in Example 1, the tobacco leaf material of the domestic Barley species was pulverized, and the first extraction step was not carried out, but only the second extraction step (extraction with water only) was carried out, and the extract obtained by the second extraction step was poured. The residue was extracted back to prepare a tobacco raw material of Comparative Example 5.

又,與實施例1相同地粉碎處理國產Barley種之菸葉材料,最初進行第二萃取步驟(以水進行萃取),然後,進行第一萃取步驟(以正己烷進行萃取)後,僅將水進行萃取所得到之萃取液倒回萃取殘渣,製作比較例6之菸原料。 Further, the tobacco leaf material of the domestic Barley species was pulverized and treated in the same manner as in Example 1, and the second extraction step (extraction with water) was first performed, and then, the first extraction step (extraction with n-hexane) was carried out, and only water was allowed to proceed. The extract obtained by the extraction was poured back to the extraction residue to prepare a tobacco raw material of Comparative Example 6.

對於比較例5及6之菸原料,以與上述相同的方法進行官能評價(吸感之變化)。於官能評價所使用的比較例5之菸原料之重量係180mg,比較例6之菸原料之重量係172.9mg。 For the tobacco materials of Comparative Examples 5 and 6, the sensory evaluation (change in sorption) was carried out in the same manner as above. The weight of the tobacco raw material of Comparative Example 5 used for the sensory evaluation was 180 mg, and the weight of the tobacco raw material of Comparative Example 6 was 172.9 mg.

結果表示於第5圖中。 The results are shown in Figure 5.

<比較例7> <Comparative Example 7>

與實施例1相同地進行粉碎處理國產Barley種之菸葉材料,先進行第二萃取步驟,(先以水進行萃取),其後進行第一萃取步驟(其後進行以正己烷之萃取),將所得到之 萃取液(只有以正己烷之萃取液)倒回萃取殘渣,製作比較例7之菸原料。 The pulverization treatment of the tobacco material of the domestic Barley species is carried out in the same manner as in the first embodiment, and the second extraction step is first performed (extraction with water first), followed by the first extraction step (subsequent extraction with n-hexane), Obtained The extract (only the extract of n-hexane) was poured back to the residue to prepare a tobacco material of Comparative Example 7.

對於比較例7之菸原料,以與實施例3、4及比較例2、3相同的方法進行官能評價(吸感之變化)。於官能評價所使用的比較例7之菸原料之重量係83.86g。 For the tobacco material of Comparative Example 7, the sensory evaluation (change in sorption) was carried out in the same manner as in Examples 3 and 4 and Comparative Examples 2 and 3. The weight of the tobacco raw material of Comparative Example 7 used for the sensory evaluation was 83.86 g.

結果表示於第6圖中。 The results are shown in Figure 6.

<各菸原料之W/H比> <W/H ratio of each tobacco raw material>

測定實施例1(於第一萃取步驟使用正己烷者)、實施例2(於第一萃取步驟使用乙醇者)及實施例6(於第一步驟使用四氫呋喃者)、比較例1(於第一步驟使用甲醇者)之各菸原料之W/H比。又,就參考而言,對於未處理之菸原料(Barley種)仍測定W/H比作為參考例。 Measurement Example 1 (using n-hexane in the first extraction step), Example 2 (using ethanol in the first extraction step), and Example 6 (using tetrahydrofuran in the first step), Comparative Example 1 (in the first The step uses the W/H ratio of each of the tobacco raw materials. Further, as for the reference, the W/H ratio was measured for the untreated tobacco material (Barley species) as a reference example.

其測定方法係如上述記載。 The measurement method is as described above.

使用於萃取之試料之填充係依以下之順序進行。 The filling of the sample used for the extraction is carried out in the following order.

將純正濾紙安置於耐壓金屬製萃取格室,填充預先洗浄且已秤量之不銹鋼球10g。然後,對於實施例1、2、6、比較例1及參考例之各菸原料,以上皿天秤於藥包紙上秤量1.0g/格室,使用粉末用漏斗等之適當補助具,於預先置入濾紙及不銹鋼球且於已準備之22ml之格室,置入已秤量之試料,將殘留於藥包紙上之試料以不銹鋼球擦拭數次而加入於格室中。進一步,於空隙以不銹鋼球塞入直到格室上部而填滿。成為填滿後,密閉格室之上側部,於桌上敲擊來填充隙間使其均勻,再於空處塞入不銹鋼球。 The pure filter paper was placed in a pressure-resistant metal extraction cell, and 10 g of pre-washed and weighed stainless steel balls were filled. Then, for each of the tobacco materials of Examples 1, 2, 6, and Comparative Example 1 and the reference examples, the above-mentioned dish scale was weighed 1.0 g/cell on the medicine wrap, and a suitable aid such as a powder funnel was used, and the pre-insertion was carried out. The filter paper and the stainless steel ball were placed in the prepared 22 ml cell, the sample was weighed, and the sample remaining on the drug wrap was wiped several times with a stainless steel ball and added to the cell. Further, the gap is filled with a stainless steel ball until the upper portion of the cell is filled. After filling, the upper part of the cell is sealed, tapped on the table to fill the gap to make it uniform, and then the stainless steel ball is inserted into the space.

其次,以表1所示之條件,將以正己烷與水(MilliQ水) 進行之萃取,分別進行3循環及9循環,求出藉由各別之溶劑所萃取的萃取物之重量。測定係對於各菸原料各進行2次,萃取物之重量係表示其平均值。 Next, under the conditions shown in Table 1, hexane and water (MilliQ water) will be used. The extraction was carried out for 3 cycles and 9 cycles, respectively, and the weight of the extract extracted by the respective solvent was determined. The measurement system was performed twice for each of the tobacco materials, and the weight of the extract was expressed as an average value.

從所得到之萃取物重量求出W/H比及萃取物重量對萃取處理前之菸原料比率。結果表示於表3。 The ratio of the W/H ratio and the weight of the extract to the smoke raw material before the extraction treatment was determined from the weight of the obtained extract. The results are shown in Table 3.

有關實際使用之裝置、溶劑、物品係如以下。 The devices, solvents, and articles actually used are as follows.

<使用裝置> <Usage device>

高速溶劑萃取裝置(DIONEX社、ASE200) High-speed solvent extraction device (DIONEX, ASE200)

上皿天秤(METTLER、PM2500) Dish scales (METTLER, PM2500)

附預備凍結槽之凍結乾燥裝置(東京理科機械(股).FD-81) Freeze drying device with preparatory freezing tank (Tokyo Science Machinery Co., Ltd.. FD-81)

減壓油封幫浦(ULVAC KIKO Inc.、ULVAC GCD-051X) Decompression oil seal pump (ULVAC KIKO Inc., ULVAC GCD-051X)

<使用溶劑> <Use solvent>

正己烷(和光純藥工業(股)、高速液體色層分析用(HPLC)) Hexane (Wako Pure Chemical Industries Co., Ltd., High Speed Liquid Chromatography (HPLC))

水(超純水製造裝置MQ Gradient所得之MilliQ水、日 本Millipore(股)) Water (MilliQ water, day from MQ Gradient, ultra pure water manufacturing equipment) Ben Millipore (share))

醋酸乙酯(和光純藥工業(股)、高速液體色層分析用(HPLC)) Ethyl acetate (Wako Pure Chemical Industries, Ltd., high-speed liquid chromatography (HPLC))

乙醇(和光純藥工業(股)、高速液體色層分析用(HPLC)) Ethanol (Wako Pure Chemical Industries Co., Ltd., High Speed Liquid Chromatography (HPLC))

*醋酸乙酯及乙醇係將正己烷所得之萃取液移至茄型燒杯之際使用 *Ethyl acetate and ethanol are used to transfer the extract from n-hexane to the eggplant beaker.

<使用物品> <Use items>

藥包紙10公分×10公分 Medicine wrap 10 cm × 10 cm

共通匹配茄型燒杯/100ml(柴田科學(股)) Common match eggplant beaker / 100ml (Shibata Science Co., Ltd.)

凍結乾燥用共通匹配茄型燒杯/500ml(EYELA(股)) Freeze-drying common matching eggplant beaker / 500ml (EYELA)

耐壓金屬製萃取格室22mL(DIONEX社(股)) Pressure-resistant metal extraction cell 22mL (DIONEX Co., Ltd.)

萃取格室用純正濾紙(DIONEX社(股)) Pure filter paper for extraction chamber (DIONEX Co., Ltd.)

不銹鋼球粒徑2.3mm(中央科學貿易(股)) Stainless steel ball size 2.3mm (Central Science Trade (share))

本案申請專利範圍所請為一種菸原料及其製造方法,而本案之圖式為實施例與比較例之官能評價結果,不足以代表本案技術特徵。 The scope of the patent application in this case is a kind of tobacco raw material and its manufacturing method, and the drawing of the present case is the functional evaluation result of the embodiment and the comparative example, which is not enough to represent the technical features of the present invention.

Claims (7)

一種菸原料,其係藉由使用正己烷作為溶劑的萃取所得到之萃取物之重量、及其萃取後進一步藉由使用水作為溶劑的萃取所得到之萃取物的重量之比,就水萃取物重量/己烷萃取物重量比,為0以上1.5以下。 A tobacco raw material which is a weight ratio of an extract obtained by extraction using n-hexane as a solvent, and a weight ratio of an extract obtained by extraction using water as a solvent after extraction, and an aqueous extract The weight/hexane extract weight ratio is 0 or more and 1.5 or less. 如申請專利範圍第1項所述之菸原料,其中,藉由使用正己烷作為溶劑的萃取所得到之萃取物之重量、及其萃取後進一步藉由使用水作為溶劑的萃取所得到之萃取物的重量之合計量為萃取前之菸原料的重量之5至17重量%。 The tobacco raw material according to claim 1, wherein the weight of the extract obtained by extraction using n-hexane as a solvent, and the extract obtained by further extracting by using water as a solvent after extraction The total weight is 5 to 17% by weight based on the weight of the raw material of the tobacco before extraction. 一種菸原料之製造方法,其係包含如下步驟:第一萃取步驟,其係使用介電率1以上、未達25之溶劑而萃取菸葉材料以得到萃取液及萃取殘渣;第二萃取步驟,其係於第一萃取步驟之後,將第一萃取步驟所得到之萃取殘渣使用介電率25以上之溶劑進行萃取而得到萃取殘渣;及,於經過第二萃取步驟所得到之萃取殘渣,倒回第一萃取步驟所得到之萃取液而作為菸葉原料之步驟。 A method for producing a tobacco raw material, comprising: a first extraction step of extracting a tobacco leaf material using a solvent having a dielectric constant of 1 or more and less than 25 to obtain an extract liquid and a extraction residue; and a second extraction step After the first extraction step, the extraction residue obtained in the first extraction step is extracted with a solvent having a dielectric constant of 25 or more to obtain an extraction residue; and the extraction residue obtained after the second extraction step is returned to the first The step of extracting the extract obtained as the raw material of the tobacco leaf. 如申請專利範圍第3項所述之製造方法,其中,於第一萃取步驟使用之溶劑為介電率1至20之溶劑,於第二萃取步驟使用之溶劑為水。 The manufacturing method according to claim 3, wherein the solvent used in the first extraction step is a solvent having a dielectric constant of 1 to 20, and the solvent used in the second extraction step is water. 如申請專利範圍第3項或第4項所述之製造方法,其中,於第一萃取步驟使用之溶劑為選自正己烷、四氫呋喃及乙醇之1種以上。 The production method according to the third or fourth aspect of the invention, wherein the solvent used in the first extraction step is one or more selected from the group consisting of n-hexane, tetrahydrofuran and ethanol. 一種菸原料,其係藉由如申請專利範圍第3至5項中任 一項所述之製造方法所得到者。 a raw material for tobacco, which is exemplified by items 3 to 5 of the scope of the patent application The one obtained by the manufacturing method described. 一種菸製品,其係使用如申請專利範圍第1項、第2項或第6項所述之菸原料。 A smoking article which uses the tobacco material as described in claim 1, item 2 or item 6.
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