TW201500013A - Method for manufacturing tobacco material - Google Patents
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Description
本發明係關於煙草原料之製造方法。 The present invention relates to a method of producing a tobacco material.
長久以來都嘗試改善原料葉煙草之香味。例如專利文獻1中記載在葉煙草之裝桶熟成步驟前於葉煙草添加乙醇之方法。 It has long been tried to improve the aroma of raw leaf tobacco. For example, Patent Document 1 describes a method of adding ethanol to leaf tobacco before the barrel baking step of leaf tobacco.
根據該技術,藉由吸附於葉煙草之乙醇的化學作用,活化葉煙草中之蛋白質系高分子化合物、含氮化合物、糖類等之氧化反應、分解、去胺基化等,一邊釋出大量碳酸氣體一邊進行熟成。接著記載使用經如此發酵所得之葉煙草的香煙在吸煙時之煙中含有較多甲酸、乙酸之類之有機酸。此外亦記載會降低在吸煙時造成異臭、刺激之乙醛、丙酮、丙烯醛、丙酮醇等。 According to this technique, a large amount of carbonic acid is released by activating the oxidation reaction, decomposition, deamination, etc. of a protein-based polymer compound, a nitrogen-containing compound, a saccharide or the like in leaf tobacco by chemical action of ethanol adsorbed on leaf tobacco. The gas is cooked on one side. Next, it is described that a cigarette using the leaf tobacco obtained by such fermentation contains a large amount of an organic acid such as formic acid or acetic acid in the smoke at the time of smoking. In addition, it is also reported that acetaldehyde, acetone, acrolein, acetol, and the like which cause odor and irritation during smoking are reduced.
專利文獻1:日本特開昭56-51976號公報 Patent Document 1: Japanese Patent Laid-Open No. 56-51976
根據專利文獻1所記載之方法,雖然記載藉由對葉煙草賦予乙醇,而使使用賦予乙醇之葉煙草的香煙增加吸煙時之 煙中所含的有機酸含量,但增加之化合物係僅關於有機酸。 According to the method described in Patent Document 1, it is described that when ethanol is added to leaf tobacco, cigarettes using leaf tobacco to which ethanol is added are increased in smoking. The organic acid content contained in the smoke, but the added compound is only related to the organic acid.
對此,本發明係著眼於賦予煙草原料香味之成分的酯類化合物。提供藉由增加煙草原料中的如此香味成分,而增強煙草原料之香味之方法。 In this regard, the present invention is directed to an ester compound which imparts a component which imparts aroma to the tobacco raw material. A method of enhancing the aroma of a tobacco material by increasing such aroma components in the tobacco material is provided.
本案發明者精心檢討,結果發現在藉由包括燻製處理乾燥煙草葉之步驟、在經燻製處理之乾燥煙草葉添加醇類之步驟、將添加醇類之煙草葉藏置之步驟的製造方法所獲得之煙草原料中,會增加增強香味之酯類的含量,從而完成本發明。 The inventors of the present invention carefully reviewed and found that the method was obtained by the steps of the steps of drying the tobacco leaves by smoking, the steps of adding the alcohol to the dried tobacco leaves by the smoked treatment, and the step of placing the tobacco leaves with the alcohol added. In the tobacco raw material, the content of the ester which enhances the flavor is increased, thereby completing the present invention.
亦即,本發明係如下。 That is, the present invention is as follows.
[1].一種煙草原料之製造方法,係包括燻製處理乾燥煙草葉之步驟、在經燻製處理之乾燥煙草葉添加醇類之步驟、將添加醇類後之煙草葉藏置之步驟。 [1] A method for producing a tobacco raw material, comprising the steps of: treating a dried tobacco leaf by smoking, adding an alcohol to the dried tobacco leaf by the smoked treatment, and storing the tobacco leaf after adding the alcohol.
[2].如[1]所述之製造方法,其中,在前述藏置步驟後,又包括於煙草葉添加多元醇之步驟。 [2] The production method according to [1], wherein, after the hiding step, the step of adding a polyol to the tobacco leaf is further included.
[3].如[1]或[2]所述之製造方法,其中,前述藏置步驟係在室溫至70℃進行,其期間為1週以上。 [3] The production method according to [1], wherein the storing step is performed at room temperature to 70 ° C for a period of one week or longer.
[4].如[1]至[3]中任一項所述之製造方法,其中,前述藏置步驟係在密閉條件下進行。 [4] The production method according to any one of [1] to [3] wherein the storing step is performed under a sealed condition.
[5].如[1]至[4]中任一項所述之製造方法,其中,前述燻製處理係藉由冷燻法進行者。 [5] The production method according to any one of [1] to [4] wherein the smoking treatment is performed by a cold smoking method.
[6].一種煙草製品,係包括以[1]至[5]中任一項之製造方法所製造之煙草原料。 [6] A tobacco product comprising the tobacco raw material produced by the production method according to any one of [1] to [5].
根據本發明可提供增強香味成分之酯類化合物的含量之煙草原料之製造方法。 According to the present invention, a method for producing a tobacco raw material which enhances the content of an ester compound of a flavor component can be provided.
第1圖係表示煙草葉之燻製處理次數與有機酸含量之關係,(a)為乙酸之含量,(b)為異丁酸,丁酸,異戊酸,2-甲基丁酸,戊酸之含量。 Figure 1 shows the relationship between the number of smoked treatments of tobacco leaves and the content of organic acids. (a) is the content of acetic acid, and (b) is isobutyric acid, butyric acid, isovaleric acid, 2-methylbutyric acid, valeric acid. The content.
第2圖係表示變更燻製處理煙草葉時所使用之木材種類時,所得之有機酸組成的差異。 Fig. 2 is a view showing the difference in the organic acid composition obtained when the type of wood used in the tobacco leaf treatment is changed.
第3圖係表示在僅進行燻製處理步驟之情形、在燻製處理步驟後又經添加乙醇步驟之情形、在進行燻製處理步驟後又經添加薄荷醇步驟之情形、以及在燻製處理步驟後又經添加乙醇及薄荷醇步驟之情形中,各煙草原料中之有機酸含量。 Fig. 3 is a view showing a case where only the smoking treatment step is carried out, a case where the ethanol is added after the smoking treatment step, a step of adding the menthol after the smoking treatment step, and a case after the smoking treatment step. In the case of the ethanol and menthol steps, the organic acid content of each tobacco material.
第4圖(a)至(h)表示在經燻製處理之乾燥煙草葉添加醇類之步驟後(圖中之横軸之1)、以及將添加醇類之煙草葉每經藏置1週之步驟後(圖中之横軸之2至4)添加各濃度之丙二醇時,其煙草原料中之有機酸酯的變化量。 Figure 4 (a) to (h) show the steps of adding alcohol to the smoked dried tobacco leaves (1 on the horizontal axis in the figure), and the tobacco leaves to which the alcohol is added are stored for 1 week. The amount of change in the organic acid ester in the tobacco raw material when propylene glycol of each concentration is added after the step (2 to 4 on the horizontal axis in the figure).
以下表示實施形態及例示物等詳細說明本發明,但本發明並不限定以下實施形態及例示物等,在不脫離本發明主旨之範圍可任意變更後實施。 The present invention is described in detail below with reference to the accompanying drawings, and the embodiments of the invention.
本發明之煙草原料之製造方法係包括燻製處理乾燥煙草葉之步驟、在經燻製處理之乾燥煙草葉添加醇類之步驟、將添加醇類之煙草葉藏置之步驟。 The method for producing the tobacco raw material of the present invention comprises the steps of: smoking the dried tobacco leaves, adding the alcohol to the dried tobacco leaves by the smoked treatment, and placing the tobacco leaves added with the alcohol.
本發明之製造方法中實施燻製處理之煙草葉係經乾燥處理者。乾燥處理可舉出公知方法。本發明所述之經乾燥處理之煙草葉,是指乾燥至煙草葉之含水率概略未滿15重量%者。 In the manufacturing method of the present invention, the tobacco leaf which is subjected to the smoking treatment is subjected to a drying treatment. A well-known method is mentioned as a drying process. The dried tobacco leaf of the present invention means that the moisture content of the dried tobacco leaves is less than 15% by weight.
乾燥處理並無特別限定,可使用公知方法。 The drying treatment is not particularly limited, and a known method can be used.
所使用之煙草葉無特別限制,可舉出煙草屬之紅花煙草(Nicotiana tabacum)之黄色種或白肋種、黃花煙草(Nicotiana rustica)之巴西利亞種等。 The tobacco leaf to be used is not particularly limited, and examples thereof include a yellow or rib type of Nicotiana tabacum, a Brasilia species of Nicotiana rustica, and the like.
該等煙草葉係藉由公知方法裁切並製作煙草細絲。 The tobacco leaves are cut and made into tobacco filaments by known methods.
燻製處理煙草葉之方法可舉出公知方法,例如可舉出熱燻處理或溫燻處理、冷燻處理。 The method of the tobacco-treated tobacco leaf can be exemplified by a known method, and examples thereof include a hot smoke treatment, a warm smoke treatment, and a cold smoke treatment.
熱燻處理係以品溫60至120℃左右燻製煙草葉之處理。處理時間可根據必需之有機酸賦予量而任意設定,例如為10分鐘至1小時左右。 The hot smoke treatment is a treatment of smoking tobacco leaves at a temperature of about 60 to 120 °C. The treatment time can be arbitrarily set according to the amount of the organic acid to be required, and is, for example, about 10 minutes to 1 hour.
溫燻處理係以品溫30至60℃左右燻製煙草葉之處理。處理時間可根據必需之有機酸賦予量而任意設定,例如為10分鐘至1天左右。 The warm smoke treatment is a treatment of smoking tobacco leaves at a temperature of about 30 to 60 ° C. The treatment time can be arbitrarily set depending on the amount of organic acid required to be added, and is, for example, about 10 minutes to 1 day.
冷燻處理係以品溫15至30℃左右燻製煙草葉之處理。處理時間可根據必需之有機酸賦予量而任意地設定,但例如為10分鐘至4週左右。 The cold smoke treatment is a treatment of smoking tobacco leaves at a temperature of about 15 to 30 °C. The treatment time can be arbitrarily set according to the amount of the organic acid to be required, but it is, for example, about 10 minutes to 4 weeks.
為了產生燻煙而使用之木材種類並無特別限定,例如可舉出白橡木、櫻、胡桃、蘋果、櫸、櫟、山核桃。此外,為了產生燻煙可燃燒或加熱木材。加熱溫度可為350℃至650℃,較佳為450℃至500℃。 The type of wood to be used for generating smoke is not particularly limited, and examples thereof include white oak, cherry, walnut, apple, alfalfa, alfalfa, and pecan. In addition, wood can be burned or heated in order to produce smoke. The heating temperature may be from 350 ° C to 650 ° C, preferably from 450 ° C to 500 ° C.
任一種燻製處理皆可用公知燻製器等進行。 Any of the smoking treatments can be carried out by a known smoker or the like.
藉由對煙草葉實施燻製處理,可於煙草葉賦予乙酸、丁酸、異丁酸、戊酸、異戊酸、2-甲基丁酸等有機酸。 Organic acids such as acetic acid, butyric acid, isobutyric acid, valeric acid, isovaleric acid, and 2-methylbutyric acid can be imparted to tobacco leaves by smoking treatment on tobacco leaves.
使用上述燻製處理之任一者皆可對煙草葉賦予有機酸。以製造裝置之操作性(洗淨之容易性)之觀點來看,燻製處理可舉出以冷燻處理進行之態樣。此時之燻製處理時間較佳為10分鐘至1日,更佳為1小時至3小時。 An organic acid can be imparted to the tobacco leaves using any of the above-described smoking treatments. From the viewpoint of the operability of the manufacturing apparatus (ease of washing), the smoking treatment can be carried out by a cold smoking treatment. The smoking treatment time at this time is preferably from 10 minutes to 1 day, more preferably from 1 hour to 3 hours.
在經燻製處理所得之煙草葉添加之醇類並無特別限定,可舉出乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、2,2-二甲基乙醇、環己醇之類之一價脂肪族醇類;苄醇類、苯乙醇等具有芳香族取代基之一價醇類;山梨醇、麥芽糖醇、木糖醇、赤藻糖醇、乳糖醇、山梨糖醇酐、木糖、阿拉伯糖、甘露糖、海藻糖之類之糖醇類。 The alcohol to be added to the tobacco leaf obtained by the smoked treatment is not particularly limited, and examples thereof include ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, and 2-methyl-1-propane. a monovalent aliphatic alcohol such as alcohol, 2,2-dimethylethanol or cyclohexanol; a valent alcohol having an aromatic substituent such as benzyl alcohol or phenylethyl alcohol; sorbitol, maltitol, xylose Alcohols such as alcohol, erythritol, lactitol, sorbitol, xylose, arabinose, mannose, trehalose.
該等醇類可單獨使用或組合兩種以上使用。 These alcohols may be used singly or in combination of two or more.
在經燻製處理之煙草葉如上述賦予有機酸,並在煙草葉添加醇類,然後將其藏置,藉此可使有機酸與醇類反應而產生酯化。藉此增強所得煙草原料中之酯化合物含量。 The tobacco leaves treated with the smoked are given an organic acid as described above, and an alcohol is added to the tobacco leaves, and then stored, whereby the organic acid is reacted with the alcohol to cause esterification. Thereby, the content of the ester compound in the obtained tobacco raw material is enhanced.
添加於煙草葉之醇類相對於煙草葉之1重量單位,可以0.000001至0.1單位之比例添加。 The alcohol added to the tobacco leaf may be added in a ratio of 0.000001 to 0.1 unit per 1 weight unit of the tobacco leaf.
醇類之添加係以對煙草葉之細絲盡可能均勻塗布之方式,使用噴霧之類之一般方法進行。 The addition of the alcohol is carried out by a general method such as spraying in such a manner that the filament of the tobacco leaf is coated as uniformly as possible.
此外,添加醇類之步驟中,除了上述醇類也可添加其他香料。如此香料可舉出由薄荷醇,萊姆,胡椒薄荷油,綠薄荷油,薄荷 油,迷迭香油,甘草萃取物,貫葉連翹萃取物,可可等之精油或萃取物香料選出之1種以上。 Further, in the step of adding an alcohol, other fragrances may be added in addition to the above alcohols. Such spices can be exemplified by menthol, lime, peppermint oil, spearmint oil, mint One or more selected from the essential oils of oil, rosemary oil, licorice extract, St. John's wort extract, cocoa, and the like.
添加於煙草葉之香料相對於煙草葉之1重量單位,可以0.000001至0.1單位之比例添加。 The flavor added to the tobacco leaf may be added in a ratio of 0.000001 to 0.1 unit per 1 weight unit of the tobacco leaf.
將添加醇類之煙草葉藏置之步驟,較佳為在藏置中所生成之酯化合物不會揮散之條件下進行。如此條件可舉出密閉條件。 The step of depositing the tobacco leaf to which the alcohol is added is preferably carried out under the condition that the ester compound formed in the storage is not volatilized. Such a condition can be exemplified by a sealing condition.
密閉條件可舉出藉由使用密閉容器所形成之條件。此外,密閉條件可舉出使低分子酯化合物之類之揮發性成分不會揮散之程度的條件。 The sealing condition can be exemplified by the use of a closed container. Further, the sealing condition is a condition in which the volatile component such as the low molecular ester compound is not volatilized.
藏置期間只要是用以生成酯化合物之充分期間則無特別限制,但為了充分產生反應較佳為1週以上。 The storage period is not particularly limited as long as it is a sufficient period for producing an ester compound, but it is preferably one week or more in order to sufficiently generate a reaction.
藏置時之期間上限基本上無制限,但考慮製作之煙草原料至出貨之期間而可舉出30週左右。 There is basically no upper limit on the upper limit of the period of storage, but it can be considered for about 30 weeks from the time of production of the tobacco raw materials to the time of shipment.
藏置時之溫度較佳為使酯化合物充分生成之溫度。 The temperature at the time of storage is preferably a temperature at which the ester compound is sufficiently formed.
如此溫度較佳為使煙草葉所含之促進酯化反應之酵素活化,並容易產生化學酯化反應之溫度。 Such a temperature is preferably such that the enzyme which promotes the esterification reaction contained in the tobacco leaf is activated and the temperature of the chemical esterification reaction is easily generated.
具體溫度可舉出在室溫至70℃之範圍適宜調整之態樣,也可舉出在30至80℃之範圍適宜設定之態樣。 The specific temperature may be appropriately adjusted in the range of room temperature to 70 ° C, and may be suitably set in the range of 30 to 80 ° C.
除了燻製處理所賦予之有機酸以外,煙草葉也含有原本即含有之有機酸,例如肉豆蔻酸、棕櫚酸、硬脂酸、油酸、亞麻油酸、蘇子油酸等。由此來看,藉由經過上述添加醇類之步驟與藏置步驟,也會生成該等煙草葉原本含有之有機酸與所添加醇類之酯類。 In addition to the organic acid imparted by the smoking treatment, the tobacco leaves also contain organic acids originally contained, such as myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, uric acid, and the like. From this point of view, the ester of the organic acid originally contained in the tobacco leaves and the added alcohol is also produced by the step of adding the alcohol and the hiding step.
此外,煙草葉也含有甲醇、苄基醇類、苯乙醇等醇類,故認為該等醇類也在藉由上述本發明步驟生成酯類之過程提供貢獻。 Further, since tobacco leaves also contain alcohols such as methanol, benzyl alcohol, and phenylethyl alcohol, it is considered that these alcohols also contribute to the process of producing esters by the above-described steps of the present invention.
經過本發明之製造方法所得之煙草原料中被增強之有機酸酯,例如可舉出乙酸乙酯、戊酸乙酯、巴豆酸乙酯、己酸乙酯、肉豆蔻酸乙酯、棕櫚酸乙酯、硬脂酸乙酯、油酸乙酯、琥珀酸乙酯。 The organic acid ester to be reinforced in the tobacco raw material obtained by the production method of the present invention may, for example, be ethyl acetate, ethyl valerate, ethyl crotonate, ethyl hexanoate, ethyl myristate or palmitic acid. Ester, ethyl stearate, ethyl oleate, ethyl succinate.
本發明之製造方法中,在藏置步驟之後亦可包含在煙草葉細絲添加多元醇之步驟。多元醇可使用丙二醇、甘油、或該等之混合物。多元醇相對於煙草葉細絲可以0.1至5重量%之量添加。 In the production method of the present invention, the step of adding a polyol to the tobacco leaf filament may be included after the hiding step. The polyol may be propylene glycol, glycerin, or a mixture of these. The polyol may be added in an amount of 0.1 to 5% by weight relative to the tobacco leaf filament.
多元醇之添加較佳為藉由噴霧等煙草製造步驟所使用之一般方法,而以使多元醇遍佈於煙草葉細絲整體之方式進行為佳。 The addition of the polyol is preferably carried out by a general method used in a tobacco production step such as spraying, and is preferably carried out in such a manner that the polyol is spread over the entire tobacco leaf filament.
多元醇係如後述實驗例所示,具有抑制所添加之醇類與有機酸之酯化反應的功能。因此,藉由在藏置步驟後添加多元醇,可抑制所添加之醇類再產生反應而生成酯化合物,藉此使本發明之藏置步驟所生成之酯化合物的組成不易經時變化。 The polyol has a function of suppressing the esterification reaction between the added alcohol and the organic acid as shown in the experimental examples described later. Therefore, by adding a polyol after the hiding step, it is possible to suppress the re-generation reaction of the added alcohol to form an ester compound, whereby the composition of the ester compound produced in the hiding step of the present invention is not easily changed over time.
此現象被認為是因添加之多元醇比醇類更優先與有機酸形成酯類之故。 This phenomenon is considered to be because the added polyol preferentially forms an ester with an organic acid more than an alcohol.
經添加多元醇之步驟後,由充分抑制添加之醇類與有機酸之酯化反應的觀點萊看,較佳為藏置約1週以上。此外,該藏置較佳為在密封條件下進行。 After the step of adding a polyol, it is preferable to store it for about one week or more from the viewpoint of sufficiently suppressing the esterification reaction between the added alcohol and the organic acid. Furthermore, the storage is preferably carried out under sealed conditions.
本發明之製造方法中,可在任意步驟中以任意量添加上述精油或萃取物香料等添加物。 In the production method of the present invention, an additive such as the above-mentioned essential oil or extract perfume may be added in an arbitrary amount in any step.
本發明之煙草原料為例如口腔煙草製品時,可舉例口含煙(Snus)。此時係將上述製造方法所製作之煙草原料以公知方法充填於使用不織布之類原料的包裝材而得。例如調整煙草原料量而充填,並藉由熱封等手段進行密封而得口含煙。 When the tobacco raw material of the present invention is, for example, an oral tobacco product, it may be exemplified by a cigarette (Snus). In this case, the tobacco raw material produced by the above-described production method is obtained by filling a packaging material using a raw material such as a nonwoven fabric by a known method. For example, the amount of the tobacco raw material is adjusted and filled, and sealed by means of heat sealing or the like to obtain a mouth-containing smoke.
包裝材之使用並無特別限制,但較佳為使用纖維素系之不織布等。 The use of the packaging material is not particularly limited, but a cellulose-based nonwoven fabric or the like is preferably used.
口腔煙草製品例如為膠時,可將使用本發明之製造方法所得之上述煙草原料以公知方法與公知之膠基混合而得。有關嚼式煙草或聞式煙草、壓縮煙草,除了使用以本發明之製造方法所得之上述煙草原料以外,可使用公知方法製得。此外,有關可食用薄膜,除了使用以本發明之製造方法所得之上述煙草原料以外,可使用公知之材料或方法製得。 When the oral tobacco product is, for example, a gum, the above-mentioned tobacco raw material obtained by the production method of the present invention can be obtained by mixing a known gum base with a known method. The chewing tobacco, the tobacco, and the compressed tobacco can be produced by a known method in addition to the above-mentioned tobacco raw material obtained by the production method of the present invention. Further, the edible film can be obtained by using a known material or method in addition to the above-mentioned tobacco raw material obtained by the production method of the present invention.
本發明之煙草原料可於一般煙草細絲以任意比例混合,並以其製造香煙。此外,本發明之煙草原料亦可配置於公知香煙之過濾器部分。過濾器部分之配置例如可為配置在空腔內或分散配置於過濾器纖維。 The tobacco raw material of the present invention can be mixed in a usual ratio in a general tobacco filament and used to produce a cigarette. Further, the tobacco raw material of the present invention may be disposed in a filter portion of a known cigarette. The configuration of the filter portion can be, for example, disposed within the cavity or dispersedly disposed in the filter fibers.
本發明之煙草原料亦可使用於加溫或非加熱型之香煙代替製品。 The tobacco material of the present invention can also be used in a warm or non-heated type of cigarette instead of the article.
根據本發明之製造方法,可提供香味成分增強之煙草原料。此外,以本發明之方法所製造之煙草原料,可使用作為煙草製品中之煙草原料全部,也可使用作為煙草製品中之煙草原料之一部分。使用本發明所得之煙草原料作為煙草製品中之煙草原料之一部分時,可以任意比例使用。 According to the manufacturing method of the present invention, a tobacco material having enhanced flavor component can be provided. Further, the tobacco raw material produced by the method of the present invention can be used as the tobacco raw material in the tobacco product, and can also be used as a part of the tobacco raw material in the tobacco product. When the tobacco raw material obtained by the present invention is used as a part of the tobacco raw material in the tobacco product, it can be used in any ratio.
藉由實施例更具體說明本發明,但本發明在不超過其主旨之範圍係不限定於以下實施例之記載。 The present invention will be more specifically described by the examples, but the scope of the present invention is not limited to the description of the following examples.
在鋁箔上秤取白橡木的木屑20g,並敷於燻製器底部。 20 g of white oak wood chips were weighed on aluminum foil and applied to the bottom of the smoker.
將煙草細絲20g載置於燻製器內之網上。關閉燻製器的蓋子,將加熱器調為ON(600W)。在產生煙起5分鐘間直接以600W持續加熱,然後將加熱器電源調為OFF。至產生煙為止之時間大約為6至7分鐘。使燻製器的蓋子為關閉狀態下放置30分鐘(冷卻)。 20 g of tobacco filaments were placed on the net in the smoker. Close the lid of the smoker and turn the heater to ON (600W). The battery was continuously heated at 600 W for 5 minutes from the generation of the smoke, and then the heater power was turned OFF. The time until the smoke is generated is approximately 6 to 7 minutes. Place the lid of the smoker in the closed state for 30 minutes (cooling).
將處理之煙草細絲再燻製處理時,係重複上述操作。 The above operation is repeated when the treated tobacco filament is re-smoked.
上述之處理中品溫為100℃左右,木屑之溫度為600℃左右。 In the above treatment, the product temperature is about 100 ° C, and the temperature of the wood chips is about 600 ° C.
依照以下順序測定經燻製處理之煙草葉所含乙酸之濃度。 The concentration of acetic acid contained in the smoked tobacco leaves was determined in the following order.
於經燻製處理之煙草細絲0.5g加入超純水10mL,振搖30分鐘進行萃取。 To the tobacco-treated tobacco filament 0.5 g, 10 mL of ultrapure water was added, and the mixture was shaken for 30 minutes for extraction.
對萃取液進行超過濾(分子量劃分3000)並回收濾液。以成為在檢量線範圍之方式以超純水稀釋濾液,並以毛細管電泳(DAD檢測器)實施定量分析。 The extract was subjected to ultrafiltration (molecular weight division 3000) and the filtrate was recovered. The filtrate was diluted with ultrapure water in such a manner as to be in the range of the calibration line, and quantitative analysis was carried out by capillary electrophoresis (DAD detector).
接著,其他有機酸類之分析係藉由SPE-GCMS進行。 Next, analysis of other organic acids was carried out by SPE-GCMS.
在經燻製處理之煙草細絲0.5g加入超純水50mL,並振搖30分鐘進行萃取。 50 mL of ultrapure water was added to 0.5 g of the smoked tobacco filaments, and the mixture was shaken for 30 minutes for extraction.
將萃取液過濾、回収後,加入鹽酸調整為pH2。 After the extract was filtered and recovered, hydrochloric acid was added to adjust to pH 2.
使萃取液通過經二乙醚、甲醇、0.01N鹽酸水溶液各約20mL調節後之固相萃取匣(OasisHLB),將匣以氮氣流乾燥。以二乙醚溶出吸附於匣之有機酸類,並以GCMS分析定量。 The extract was passed through a solid phase extraction crucible (Oasis HLB) adjusted to about 20 mL each of diethyl ether, methanol and 0.01 N aqueous hydrochloric acid, and the hydrazine was dried under a nitrogen stream. The organic acids adsorbed on hydrazine were dissolved in diethyl ether and quantified by GCMS analysis.
燻製處理前後之有機酸分析值之比較資料表示於第1圖。 The comparative data of the organic acid analysis values before and after the smoked treatment are shown in Fig. 1.
由第1圖之結果可確認藉由對煙草葉實施燻製處理,可增加煙草葉所含之有機酸含量。此外也可確認藉由增加燻製處理次數,使賦予之有機酸量增加。 From the results of Fig. 1, it was confirmed that the tobacco leaf can be smoked to increase the organic acid content of the tobacco leaves. Further, it was confirmed that the amount of organic acid to be added was increased by increasing the number of times of smoking treatment.
此外調查變更燻製所使用木材之素材時所得乙酸濃度之差異。 In addition, the difference in acetic acid concentration obtained when the material used for smoking was changed was investigated.
對各素材進行之順序係依照與上述白橡木相同之順序。 The order of the materials is in the same order as the white oak described above.
結果示於第2圖。 The results are shown in Figure 2.
由第2圖之結果可知,變更燻製處理所使用木材之種類也會增加煙草葉中之有機酸含量。 As can be seen from the results of Fig. 2, changing the type of wood used in the smoking treatment also increases the organic acid content in the tobacco leaves.
將以白橡木進行8次燻製處理之煙草葉細絲10g、及各種醇類素材(乙醇0.5g、薄荷醇0.5g、乙醇0.5g+薄荷醇0.5g)放入50mL容量之旋口瓶並密封。將其於預定溫度(70℃)、預定期間(1週)在密閉容器中一邊加溫一邊藏置。 10 g of tobacco leaf filaments which were subjected to 8 times of smoking treatment in white oak, and various alcohol materials (0.5 g of ethanol, 0.5 g of menthol, 0.5 g of ethanol + 0.5 g of menthol) were placed in a 50 mL capacity screw bottle and sealed. This was stored at a predetermined temperature (70 ° C) for a predetermined period of time (one week) while being heated in a sealed container.
有關上述酯化處理,係分別調查僅進行燻製處理(白橡木8次燻製)、燻製處理後添加乙醇、燻製處理後添加薄荷醇、燻製處理後添加乙醇及薄荷醇各者之有機酸組成。結果示於第3圖。 Regarding the above-mentioned esterification treatment, the organic acid composition in which only the smoked treatment (white oak 8 smoked), the smoked treatment, the ethanol addition, the smoked treatment, the menthol, the smoked treatment, and the addition of ethanol and menthol were investigated. The results are shown in Figure 3.
有機酸含量之測定係以與上述實驗例1同樣之方法進行。 The measurement of the organic acid content was carried out in the same manner as in Experimental Example 1 described above.
由第3圖之結果來看,添加醇類並以密封容器加溫者其有機酸含量減少,可推知產生酯化反應。 From the results of Fig. 3, it can be inferred that an esterification reaction is produced by adding an alcohol and heating the sealed container to reduce the organic acid content.
添加乙醇(相對於燻製處理後之煙草葉細絲重量為5%),在40℃放入旋口瓶密封1週,在藏置1週之時間點以預定濃度(相對於煙草葉為1重量%、2重量%、5重量%)添加丙二醇。 Add ethanol (5% of the weight of the tobacco leaf filament after the smoked treatment), put it in a screw bottle at 40 ° C for 1 week, and set it at a predetermined concentration for 1 week (1 weight relative to the tobacco leaf) 5%, 2% by weight, 5% by weight) propylene glycol was added.
在經過0週時(未處理)、添加乙醇後經過一週時(添加丙二醇前)、之後(添加丙二醇後)再經過一週時,藉由以下所示操作進行各有機酸酯之分析。 The analysis of each organic acid ester was carried out by the following procedure after 0 weeks (untreated), one week after the addition of ethanol (before the addition of propylene glycol), and then (after the addition of propylene glycol).
由以下方式進行酯化合物之分析。 The analysis of the ester compound was carried out in the following manner.
精確秤取煙草細絲0.5g放入SPME試樣瓶(20mL容量),蓋上試樣瓶蓋密封,藉由附有SPME自動導入裝置之GCMS進行分析。 0.5 g of tobacco filaments were accurately weighed into a SPME sample bottle (20 mL capacity), sealed with a sample bottle cap, and analyzed by GCMS with an SPME automatic introduction device.
此外,對在其他SPME試樣瓶加入對溴苯乙基醇類之乙腈溶液(1mg/mL)25μL之樣品同樣進行分析,求取分析對象成分與對溴苯乙基醇類之波峰面積比,以求得之值與各細絲樣品中所含分析對象成分之量比較。 In addition, a sample of 25 μL of a p-bromophenethyl alcohol acetonitrile solution (1 mg/mL) was added to other SPME sample vials to obtain a peak area ratio of the component to be bromophenylethyl alcohol. The value obtained is compared with the amount of the analyte component contained in each filament sample.
裝置:Agilent公司製氣相層析分析裝置(6890A)Agilent公司製質量檢測器(5973N) Device: Gas chromatographic analyzer (6890A) manufactured by Agilent Co., Ltd. Quality detector manufactured by Agilent (5973N)
注入量:1μL(以脈衝不分流模式注入) Injection volume: 1μL (injection in pulse splitless mode)
管柱:INNOWAX Column: INNOWAX
加熱室:40℃→250℃(3℃/min) Heating chamber: 40 ° C → 250 ° C (3 ° C / min)
質量檢測器:TIC模式(質量數29至550) Quality detector: TIC mode (mass 29 to 550)
酯化合物:乙酸乙酯、戊酸乙酯、己酸乙酯、巴豆酸乙酯、己酸乙酯、肉豆蔻酸乙酯、棕櫚酸乙酯、硬脂酸乙酯、油酸乙酯。 Ester compound: ethyl acetate, ethyl valerate, ethyl hexanoate, ethyl crotonate, ethyl hexanoate, ethyl myristate, ethyl palmitate, ethyl stearate, ethyl oleate.
將實驗例3之結果示於第4圖(a)至(h)。另外,第4圖中縱軸之數值並非有機酸酯之濃度,而是表示GCMS分析所得之波峰面積值。此外,第4圖横軸數值係表示經過週數。 The results of Experimental Example 3 are shown in Figures 4(a) to (h). Further, the value of the vertical axis in Fig. 4 is not the concentration of the organic acid ester, but the peak area value obtained by GCMS analysis. In addition, the horizontal axis numerical value of Fig. 4 indicates the number of weeks passed.
由第4圖可明瞭,藏置1週後之添加醇類之煙草葉中生成有機酸酯。此外可知,隨後添加丙二醇者與未添加者相比,前者會抑制經時之有機酸酯之生成。 As can be seen from Fig. 4, an organic acid ester was formed in the tobacco leaf to which the alcohol was added after one week of storage. Further, it was found that the subsequent addition of propylene glycol inhibited the formation of the organic acid ester over time as compared with the unadded one.
根據本發明之製造方法,可提供增強有機酸酯之類之香味成分之煙草原料。 According to the production method of the present invention, a tobacco raw material which enhances a flavor component such as an organic acid ester can be provided.
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