CN110358630B - Spice with fresh and spicy flavor for cigarettes, preparation method of spice and application of spice in cigarettes - Google Patents

Spice with fresh and spicy flavor for cigarettes, preparation method of spice and application of spice in cigarettes Download PDF

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CN110358630B
CN110358630B CN201910553195.5A CN201910553195A CN110358630B CN 110358630 B CN110358630 B CN 110358630B CN 201910553195 A CN201910553195 A CN 201910553195A CN 110358630 B CN110358630 B CN 110358630B
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cigarettes
flavor
clear
preparation
prickly ash
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CN110358630A (en
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王宝林
姚倩
孙九喆
王新中
王二彬
许衡
刘超
张书伟
马一琼
贾国涛
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China Tobacco Henan Industrial Co Ltd
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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
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery by solvent extraction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Tobacco Products (AREA)
  • Fats And Perfumes (AREA)

Abstract

本发明属于烟草加工技术领域,具体涉及一种清辛香型烟用香料、其制备方法及在卷烟中的应用。本发明所述清辛香型烟用香料,由如下质量百分比的原料组成:20%‑30%花椒芽叶、30%‑60%紫苏叶以及20%‑40%碰碰香,在卷烟制备过程中,将溶解有所述清辛香型烟用香料的有机溶剂均匀喷洒在烟丝上,当清辛香型烟用香料的添加量占烟丝重量的0.01~0.1%时,可以丰富卷烟烟气,对卷烟制品起着有效的增香作用,该提取物还可赋予卷烟独特的香韵,突出卷烟特色,整体提升卷烟内在品质。该提取物作为烟用香料,效果明显,对具有特色风格的卷烟制品有很好的应用前景,适用于卷烟工业化生产。The invention belongs to the technical field of tobacco processing, and in particular relates to a clear and spicy flavor type tobacco flavor, a preparation method thereof and its application in cigarettes. The spice-flavored tobacco flavor of the present invention is composed of the following raw materials by mass percentage: 20%-30% prickly ash sprouts, 30%-60% perilla leaves, and 20%-40% touch-pump incense, prepared in cigarettes During the process, the organic solvent in which the clear and spicy flavor type tobacco flavor is dissolved is evenly sprayed on the cut tobacco, and when the added amount of the clear and spicy flavor type tobacco flavor accounts for 0.01-0.1% of the weight of the cut tobacco, the cigarette smoke can be enriched. , plays an effective aroma-enhancing effect on cigarette products, the extract can also impart a unique aroma to cigarettes, highlight the characteristics of cigarettes, and improve the internal quality of cigarettes as a whole. The extract has obvious effect as tobacco flavor, has good application prospect for cigarette products with characteristic style, and is suitable for the industrial production of cigarettes.

Description

一种清辛香型烟用香料、其制备方法及在卷烟中的应用A clear and spicy flavor type tobacco flavor, its preparation method and its application in cigarettes

技术领域technical field

本发明属于烟草加工技术领域,具体涉及一种清辛香型烟用香料、其制备方法及在卷烟中的应用。The invention belongs to the technical field of tobacco processing, and in particular relates to a clear and spicy flavor type tobacco flavor, a preparation method thereof and an application in cigarettes.

背景技术Background technique

烟用香料是卷烟品牌培育中的重要组成部分,也是突出卷烟产品的个性化风格的重要手段,在降低卷烟焦油的同时,存在于焦油中的烟草本身固有的香味物质难免会有损失,导致卷烟香气损失、感官舒适度下降等风格特征弱化的问题,而天然香料具有香韵独特、自然,香气协调丰满,留香持久等特点,因此从天然植物中寻找有效香味成分作为低焦油烟用香料,已成为卷烟发展的必然趋势。Tobacco flavor is an important part of cigarette brand cultivation, and it is also an important means to highlight the personalized style of cigarette products. While reducing cigarette tar, the inherent aroma substances of tobacco itself in tar will inevitably be lost, resulting in cigarettes. The problem of the weakening of style characteristics such as the loss of aroma and the decline of sensory comfort, while the natural flavor has the characteristics of unique and natural aroma, harmonious and full aroma, and long-lasting fragrance. It has become an inevitable trend in the development of cigarettes.

花椒是芸香科花椒属植物,落叶灌木或小乔木,产于东亚和北美,全球约有250种,我国有近60种,广布我国南北各省区。花椒具有芳香和麻辣特性,可食用和药用,能促进唾液分泌,增加食欲,有抗溃疡、抗腹泻、保肝、保护心脏、降血压、抗凝血、抑制病原微生物、抗癌等作用。国内外学者对花椒的化学成分进行了系列研究,发现其含有挥发油、生物碱、黄酮类物质、有机酸等成分。Zanthoxylum bungeanum is a deciduous shrub or small tree of the Rutaceae family. It is produced in East Asia and North America. There are about 250 species in the world, and there are nearly 60 species in my country, which are widely distributed in the north and south provinces of my country. Zanthoxylum bungeanum has aromatic and spicy properties, edible and medicinal, can promote saliva secretion, increase appetite, anti-ulcer, anti-diarrhea, liver protection, heart protection, blood pressure lowering, anti-coagulation, inhibition of pathogenic microorganisms, anti-cancer and other effects. Scholars at home and abroad have conducted a series of studies on the chemical components of Zanthoxylum bungeanum, and found that it contains volatile oils, alkaloids, flavonoids, organic acids and other components.

由于花椒具有特殊的强烈芳香,添加在卷烟中,能赋予卷烟特别的香气风格。但花椒味辛、麻而持久,在丰富烟香的同时,也会增加卷烟对口腔和鼻腔的刺激,破坏卷烟的口感。公告号为CN102499433B的中国专利公开了一种花椒醇提取物在卷烟加香加料中的应用,通过提取花椒醇,使花椒提取物既保留了花椒中的主要香味成分,又去除了木质纤维等杂质,不仅方法简单而且可以提高卷烟的吸食质感。Since Sichuan pepper has a special strong aroma, it can give cigarettes a special aroma style when added to cigarettes. However, prickly ash is spicy, numb and long-lasting. While enriching the aroma of the cigarette, it will also increase the stimulation of the cigarette to the oral cavity and nasal cavity, and destroy the taste of the cigarette. The Chinese patent with the publication number CN102499433B discloses the application of an alcohol extract of Zanthoxylum in cigarette flavoring. By extracting the alcohol from Zanthoxylum, the extract of Zanthoxylum can retain the main aroma components in Zanthoxylum bungeanum, and remove impurities such as wood fibers. , not only the method is simple but also can improve the smoking texture of cigarettes.

紫苏别名:桂荏、白苏、赤苏等,为唇形科一年生草本植物,中国华北、华中、华南、西南及台湾省均有野生种和栽培种。其具有特异的芳香,叶片多皱缩卷曲,嫩枝紫绿色,断面中部有髓,气清香,味微辛。Perilla aliases: Guiren, Baisu, Chisu, etc. It is an annual herb of the Lamiaceae family. There are wild and cultivated species in North China, Central China, South China, Southwest China and Taiwan Province. It has a specific aroma, the leaves are mostly shriveled and curled, the twigs are purple-green, the middle of the section has marrow, the air is fragrant, and the taste is slightly acrid.

紫苏叶中含有丰富的挥发油、糖甙类、黄酮类、有机酸类、甾醇类等物质,由紫苏叶制备的紫苏提取物(或紫苏油等)是GB-2760允许使用的食品添加剂,也是食品、日化、烟草中常用的香料品种之一。根据“相似相溶”原理,紫苏提取物一般采用水提或醇提工艺。但是简单的水提或醇提工艺,只能提取极性与提取溶剂类似或相近的成分,其他极性与提取溶剂差别较大的成分无法有效提取出来,无法实现紫苏叶的有效综合利用。Perilla leaves are rich in volatile oils, glycosides, flavonoids, organic acids, sterols and other substances. The perilla extract (or perilla oil, etc.) prepared from perilla leaves is a food allowed by GB-2760. Additives are also one of the spice varieties commonly used in food, daily chemicals and tobacco. According to the principle of "similar compatibility", the perilla extract is generally extracted by water or alcohol. However, the simple water extraction or alcohol extraction process can only extract the components with similar or similar polarity to the extraction solvent, and other components with large differences in polarity and extraction solvent cannot be effectively extracted, and the effective comprehensive utilization of perilla leaves cannot be realized.

碰碰香也称绒毛香茶菜,是一种会散发淡淡清香的盆栽植物。因触碰后可散发出令人舒适的香气而得名,又因其香味浓甜,颇似苹果香味,故又享有"苹果香"美誉,闻之令人神清气爽;可清热解暑,驱避蚊虫。Pengpengxiang, also known as fluffy tea vegetable, is a potted plant that emits a light fragrance. It is named after the pleasant aroma it emits after being touched, and because of its strong and sweet aroma, it is similar to the aroma of apples, so it also enjoys the reputation of "apple aroma", which is refreshing to smell; it can clear away heat and relieve summer heat. , repelling mosquitoes.

发明内容SUMMARY OF THE INVENTION

本发明的目的在于提供一种清辛香型烟用香料,并将其作为低焦油烟用香料添加剂加入卷烟中,以解决现有卷烟制备工艺中由于降低焦油量含量,而导致香气损失的问题。The object of the present invention is to provide a clear and spicy flavor type tobacco flavor, and add it to cigarettes as a low-tar flavor flavor additive to solve the problem of aroma loss due to reducing the tar content in the existing cigarette preparation process .

本发明还提供了上述清辛香型烟用香料的制备方法,以及所述清辛香型烟用香料在卷烟调香中的应用。The invention also provides the preparation method of the above-mentioned clear and spicy flavor type tobacco flavor, and the application of the clear and spicy flavor type tobacco flavor in cigarette flavoring.

为了实现上述目的,本发明采用以下技术方案:In order to achieve the above object, the present invention adopts the following technical solutions:

一种清辛香型烟用香料,由如下质量百分比的原料组成:20%-30%花椒芽叶、30%-60%紫苏叶以及20%-40%碰碰香。A clear and spicy flavor type tobacco flavor is composed of the following raw materials by mass percentage: 20%-30% of prickly ash bud leaves, 30%-60% of perilla leaves and 20%-40% of pumice incense.

优选的,所述的清辛香型烟用香料,由如下质量百分比的原料组成:20%花椒芽叶、40%紫苏叶以及40%碰碰香。Preferably, the clear and spicy flavor type tobacco flavor is composed of the following raw materials by mass percentage: 20% Zanthoxylum bungeanum bud leaves, 40% perilla leaves and 40% bump incense.

所述清辛香型烟用香料的制备方法,包括以下步骤:The preparation method of the spice-flavored tobacco flavor comprises the following steps:

(1)预处理:摘取新鲜花椒芽叶、紫苏叶和碰碰香叶用清水洗净,沥干,放入烘箱中,50-70℃条件下烘干,将烘干后的三种植物叶子研磨粉碎后过60目筛;(1) Pretreatment: Pick fresh prickly ash sprouts, perilla leaves and pumice leaves, wash them with clean water, drain them, put them in an oven, and dry them at 50-70°C. The plant leaves are ground and crushed and passed through a 60-mesh sieve;

(2)蒸馏萃取:取花椒芽、紫苏叶和碰碰香粉末进行混合,加入重量为粉末总重量10-20倍的蒸馏水,水浴3-5h;再用乙醚在水浴环境下萃取香气物质,得到一次料液;(2) Distillation extraction: Mix Chinese prickly ash buds, perilla leaves, and fragrant fragrant powder, add distilled water with a weight of 10-20 times the total weight of the powder, and bath for 3-5 hours; then use ether to extract aroma substances in a water bath environment, get a feed liquid;

(3)浓缩提纯:向步骤(2)萃取得到的一次料液中加入无水硫酸钠,干燥6-8 h,取上清液,得到二次料液;将二次料液在水浴的条件下进行旋转蒸发并浓缩,浓缩后的物质即为所述清辛香型烟用香料。(3) Concentration and purification: add anhydrous sodium sulfate to the primary feed solution obtained by extraction in step (2), dry for 6-8 h, and take the supernatant to obtain a secondary feed solution; place the secondary feed solution in a water bath under conditions Rotary evaporation and concentration are carried out under the following conditions, and the concentrated substance is the clear and spicy flavor for cigarettes.

具体的,步骤(2)中每50g花椒芽、紫苏叶和碰碰香的混合粉末中加入30-50 mL乙醚进行萃取;Specifically, in step (2), 30-50 mL of ether is added to each 50 g of the mixed powder of prickly ash buds, perilla leaves and incense sticks for extraction;

具体的,步骤(3)中每50g花椒芽、紫苏叶和碰碰香的混合粉末经萃取后得到的一次料液中加入10-30 g无水硫酸钠。Specifically, in step (3), 10-30 g of anhydrous sodium sulfate is added to the primary feed solution obtained by extracting the mixed powder of 50 g of Chinese prickly ash buds, perilla leaves and incense sticks.

优选的,步骤(2)中所述水浴温度为55-65℃。Preferably, the temperature of the water bath in step (2) is 55-65°C.

优选的,步骤(3)中所述水浴温度为35-50℃。Preferably, the temperature of the water bath in step (3) is 35-50°C.

所述清辛香型烟用香料在卷烟调香中的应用,应用时,在卷烟制备过程中,将清辛香型烟用香料溶于有机溶剂中得到调香溶液,并将调香溶液均匀喷洒在烟丝上,使清辛香型烟用香料的添加量占烟丝重量的0.01~0.1%。The application of the clear and spicy flavor type tobacco flavor in cigarette flavoring. During the application, in the cigarette preparation process, the clear and spicy flavor type tobacco flavor is dissolved in an organic solvent to obtain a flavoring solution, and the flavoring solution is uniformly distributed. It is sprayed on the cut tobacco, so that the added amount of the spice-flavored tobacco flavor accounts for 0.01-0.1% of the weight of the cut tobacco.

具体的,所述有机溶剂为体积分数90-95%的乙醇。Specifically, the organic solvent is ethanol with a volume fraction of 90-95%.

本发明的有益效果是:The beneficial effects of the present invention are:

1、所得香料含有花椒芽特有的辛香特征香气成分,并具有紫苏和碰碰香的清香感,香味醇和饱满,持香性能好。1. The obtained spice contains the peculiar pungent characteristic aroma components of Zanthoxylum bungeanum buds, and has the fragrance sense of perilla and bump incense, the aroma is mellow and full, and the aroma holding performance is good.

2、所得香料用在卷烟加香上,可以丰富卷烟烟气,对卷烟制品起着有效的增香作用,该提取物还可赋予卷烟独特的香韵,突出卷烟特色,整体提升卷烟内在品质。2. The obtained spice is used in cigarette flavoring, which can enrich cigarette smoke and play an effective flavoring effect on cigarette products. The extract can also give cigarettes a unique aroma, highlight the characteristics of cigarettes, and improve the internal quality of cigarettes as a whole.

3、成本低廉,工艺简便,安全健康,原材料及加工工艺均广泛应用于食品领域,不存在毒物残留问题。3. Low cost, simple process, safe and healthy, raw materials and processing technology are widely used in the field of food, and there is no problem of toxic residues.

4、本发明为清辛香型烟用香料提取物开辟了一个新的应用领域,增加了花椒芽、紫苏和碰碰香新的功效和作用。该提取物作为烟用香料,效果明显,对具有特色风格的卷烟制品有很好的应用前景,适用于卷烟工业化生产。4. The present invention opens up a new application field for the spice-flavored tobacco spice extract, and increases the new efficacy and function of Zanthoxylum bungeanum bud, basil and Pengpengxiang. The extract has obvious effect as tobacco flavor, has good application prospect for cigarette products with characteristic style, and is suitable for the industrial production of cigarettes.

具体实施方式Detailed ways

下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式不限于此。下述实施例中旋转蒸发时使用的设备为LC-RE-52A型旋转蒸发仪。以下实施方式中采用长度为1-2cm的花椒芽叶。The present invention will be described in further detail below with reference to the examples, but the embodiments of the present invention are not limited thereto. The equipment used in the rotary evaporation in the following examples is a LC-RE-52A rotary evaporator. In the following embodiments, sprouts and leaves of Chinese prickly ash with a length of 1-2 cm are used.

实施例1Example 1

一种清辛香型烟用香料,由以下重量份的原料制成:花椒芽10 g、紫苏20 g、碰碰香20 g。所述复合天然植物提取液的制备方法包括以下步骤:A clear and spicy-flavor tobacco spice is prepared from the following raw materials by weight: 10 g of Chinese prickly ash buds, 20 g of perilla, and 20 g of fragrant incense. The preparation method of the composite natural plant extract comprises the following steps:

(1)预处理:摘取新鲜花椒芽叶、紫苏叶和碰碰香叶用清水洗净,沥干,放入烘箱中,60℃条件下烘干,将烘干后的三种植物叶子研磨粉碎后过60目筛;(1) Pretreatment: Pick fresh prickly ash sprouts, basil leaves and pumice leaves, wash them with water, drain, put them in an oven, and dry them at 60°C. Dry the three kinds of plant leaves after drying. After grinding and pulverizing, pass through a 60-mesh sieve;

(2)蒸馏萃取:取花椒芽、紫苏叶、碰碰香粉末混合,取花椒芽、紫苏和碰碰香混合粉末,加入1000 mL蒸馏水,水浴55℃加热4h,用30 mL乙醚溶剂在60℃水浴环境下萃取香气物质,得到一次料液;(2) Distillation extraction: Mix the prickly ash buds, basil leaves, and Pangpangxiang powder, take the mixed powder of prickly ash buds, basil, and Pangpangxiang, add 1000 mL of distilled water, heat in a water bath at 55 °C for 4 hours, and use 30 mL of ether solvent in Extract aroma substances in a water bath environment of 60 °C to obtain a feed liquid;

(3)浓缩提纯:向步骤(2)萃取得到的一次料液中加入15 g无水硫酸钠,干燥6 h,取上清液,得到二次料液;将二次料液在水浴温度为45℃条件下,进行旋转蒸发,浓缩后的物质即为提取物A。(3) Concentration and purification: add 15 g of anhydrous sodium sulfate to the primary feed solution obtained by extraction in step (2), dry for 6 h, and take the supernatant to obtain a secondary feed solution; set the secondary feed solution at a water bath temperature of Under the condition of 45°C, rotary evaporation is performed, and the concentrated substance is the extract A.

实施例2Example 2

一种清辛香型烟用香料,由以下重量份的原料制成:花椒芽12.5 g、紫苏25 g、碰碰香12.5 g。所述清辛香型烟用香料的制备方法包括以下步骤:A clear and spicy-flavor tobacco spice is prepared from the following raw materials by weight: 12.5 g of prickly ash buds, 25 g of perilla, and 12.5 g of fragrant incense. The preparation method of the clear and spicy flavor type tobacco flavor comprises the following steps:

(1)预处理步骤与实施例1相同;(1) The preprocessing steps are the same as those in Example 1;

(2)蒸馏萃取:取花椒芽、紫苏和碰碰香混合粉末,加入1000 mL蒸馏水,水浴65℃加热3.5小时,用40 mL乙醚溶剂在水浴60℃环境下萃取香气物质,得到一次料液;(2) Distillation extraction: Take the mixed powder of Zanthoxylum bungeanum bud, Perilla frutescens and Pangpangxiang, add 1000 mL of distilled water, heat in a water bath at 65°C for 3.5 hours, and extract the aroma substances with 40 mL of ether solvent in a water bath at 60°C to obtain a primary feed solution ;

(3)浓缩提纯:向步骤(2)萃取得到的一次料液中加入20 g无水硫酸钠,干燥7 h,取上清液,得到二次料液;将二次料液在水浴温度为48℃条件下,进行旋转蒸发,浓缩后的物质即为提取物B。(3) Concentration and purification: add 20 g of anhydrous sodium sulfate to the primary feed solution obtained by extraction in step (2), dry for 7 h, and take the supernatant to obtain a secondary feed solution; the secondary feed solution is kept at a water bath temperature of Under the condition of 48°C, rotary evaporation was performed, and the concentrated substance was the extract B.

实施例3Example 3

一种清辛香型烟用香料,由以下重量份的原料制成:花椒芽15 g、紫苏20 g、碰碰香15 g。所述清辛香型烟用香料的制备方法包括以下步骤:A clear and spicy-flavor tobacco spice is prepared from the following raw materials by weight: 15 g of prickly ash buds, 20 g of perilla, and 15 g of fragrant incense. The preparation method of the clear and spicy flavor type tobacco flavor comprises the following steps:

(1)预处理步骤与实施例1相同;(1) The preprocessing steps are the same as those in Example 1;

(2)蒸馏萃取:取花椒芽、紫苏和碰碰香混合粉末,加入1000 mL蒸馏水,水浴60℃加热5小时,用40 mL乙醚溶剂在水浴60℃环境下萃取香气物质,得到一次料液;(2) Distillation extraction: take the mixed powder of Zanthoxylum bungeanum, basil, and incense sticks, add 1000 mL of distilled water, heat in a water bath at 60°C for 5 hours, and use 40 mL of ether solvent to extract aroma substances in a water bath at 60°C to obtain a primary feed solution ;

(3)浓缩提纯:向步骤(2)萃取得到的一次料液中加入约30 g无水硫酸钠,干燥7.5h,取上清液,得到二次料液;将二次料液在水浴温度为47℃以下条件下,进行旋转蒸发,浓缩后的物质即为提取物C。(3) Concentration and purification: add about 30 g of anhydrous sodium sulfate to the primary feed solution obtained by extraction in step (2), dry for 7.5 hours, and take the supernatant to obtain a secondary feed solution; the secondary feed solution is heated at the temperature of a water bath. Under the condition of below 47°C, rotary evaporation is performed, and the concentrated substance is the extract C.

对比例1Comparative Example 1

取50 g预处理过的花椒芽粉末,加入1000 mL蒸馏水,水浴55℃加热4小时,用30mL乙醚溶剂在60℃水浴环境下萃取香气物质,得到一次料液。向萃取后的一次料液中加入约15 g无水硫酸钠,干燥6 h,取上清液,得到二次料液;将二次料液在水浴温度为45℃条件下,进行旋转蒸发,浓缩后的物质即为提取物D。Take 50 g of pretreated prickly ash bud powder, add 1000 mL of distilled water, heat in a water bath at 55 °C for 4 hours, and extract aroma substances with 30 mL of ether solvent in a 60 °C water bath to obtain a primary feed solution. About 15 g of anhydrous sodium sulfate was added to the primary feed solution after extraction, dried for 6 h, and the supernatant was taken to obtain a secondary feed solution; the secondary feed solution was subjected to rotary evaporation under the condition of a water bath temperature of 45 °C, The concentrated substance is the extract D.

对比例2Comparative Example 2

取50 g预处理过的紫苏粉末,加入1000 mL蒸馏水,水浴55℃加热4小时,用30 mL乙醚溶剂在60℃水浴环境下萃取香气物质,得到一次料液。向萃取后的一次料液中加入约15 g无水硫酸钠,干燥6 h,取上清液,得到二次料液;将二次料液在水浴温度为45℃条件下,进行旋转蒸发,浓缩后的物质即为提取物E。Take 50 g of pretreated perilla powder, add 1000 mL of distilled water, heat in a water bath at 55°C for 4 hours, and extract aroma substances with 30 mL of ether solvent in a 60°C water bath to obtain a primary feed solution. About 15 g of anhydrous sodium sulfate was added to the primary feed solution after extraction, dried for 6 h, and the supernatant was taken to obtain a secondary feed solution; the secondary feed solution was subjected to rotary evaporation under the condition of a water bath temperature of 45 °C, The concentrated substance is the extract E.

对比例3Comparative Example 3

取50 g预处理过的碰碰香粉末,加入1000 mL蒸馏水,水浴55℃加热4小时,用30mL乙醚溶剂在60℃水浴环境下萃取香气物质,得到一次料液。向萃取后的一次料液中加入约15 g无水硫酸钠,干燥6 h,取上清液,得到二次料液;将二次料液在水浴温度为45℃条件下,进行旋转蒸发,浓缩后的物质即为提取物F。Take 50 g of pretreated touch-flavoured incense powder, add 1000 mL of distilled water, heat in a water bath at 55 °C for 4 hours, and extract aroma substances with 30 mL of ether solvent in a 60 °C water bath to obtain a primary feed solution. About 15 g of anhydrous sodium sulfate was added to the primary feed solution after extraction, dried for 6 h, and the supernatant was taken to obtain a secondary feed solution; the secondary feed solution was subjected to rotary evaporation under the condition of a water bath temperature of 45 °C, The concentrated substance is the extract F.

试验例1Test Example 1

将实施例1-3得到的清辛香型烟用香料提取物与对比例1-3的提取物,将其溶于体积分数95%的乙醇中得到调香溶液,并将调香溶液均匀喷洒在烟丝上,使提取物的添加量占烟丝重量的0.05%,依照常规加料工艺程序,平衡水分至14%,在其它条件一致的情况下,烟丝经卷烟机卷制成检测样品香烟,评吸专家对加香卷烟进行感官质量评价。将未加提取物的烟丝卷制成的卷烟作为对照,结果见下表1。Dissolve the clear and spicy cigarette flavor extract obtained in Example 1-3 and the extract of Comparative Example 1-3 in ethanol with a volume fraction of 95% to obtain a flavoring solution, and spray the flavoring solution evenly On the cut tobacco, the added amount of the extract is 0.05% of the weight of the cut tobacco. According to the conventional feeding process, the moisture content is balanced to 14%. When other conditions are the same, the cut tobacco is rolled by a cigarette machine to make a test sample cigarette, and the smoking is evaluated. Sensory quality evaluation of flavored cigarettes by experts. The cigarettes made from the tobacco cut without the extract were used as a control, and the results are shown in Table 1 below.

表1提取物对卷烟感官质量的影响。Table 1 Effects of extracts on the sensory quality of cigarettes.

Figure DEST_PATH_IMAGE002
Figure DEST_PATH_IMAGE002

结果表明单独使用紫苏和花椒芽提取物的卷烟,辛香突出,但余味舒适性较差,刺激性明显。单独使用碰碰香提取物的卷烟,清香稍有,余味清凉,口感净润,刺激性较小。添加花椒芽、紫苏和碰碰香三种物质提取物的卷烟,香气饱满丰富,协调性好,清辛香突出,余味有所改善。The results showed that the cigarettes using the extracts of perilla and prickly ash buds alone had outstanding spice, but the aftertaste was less comfortable and irritating. Cigarettes using Pangpangxiang extract alone have a slight fragrance, a cool aftertaste, a clean taste and less irritation. Cigarettes added with three kinds of extracts of pepper bud, basil and pengpengxiang have full and rich aroma, good coordination, prominent clear and spicy aroma, and improved aftertaste.

试验例2Test Example 2

检测上述得到的A、B和C三个清辛香型烟用香料提取物,分析主要化学成分含量,结果见下表2。Detect the above-obtained A, B and C three clear and spicy flavor tobacco flavor extracts, analyze the content of the main chemical components, and the results are shown in Table 2 below.

表2不同配比清辛香提取物主要化学成分含量比较(%)。Table 2 Comparison (%) of the main chemical components of the clear spice extracts with different proportions.

Figure DEST_PATH_IMAGE004
Figure DEST_PATH_IMAGE004

紫苏醛具有辛香香味;柠檬烯具有独特的清香味;芳樟醇具有浓青带甜的木青气息,似玫瑰木香气,香气柔和,轻扬透发;罗勒烯具有草香、花香并伴有橙花油气息,香气清新透发;月桂烯存在于花椒芽中,有清淡的香脂气味;乙酸芳樟酯具有花香和果香;紫苏醇具有草香,稍有木香和花香;柠檬醛具有柠檬香味。结果表明,花椒芽叶、紫苏叶和碰碰香叶的配比不同,所含香气物质的含量也不同。Perillaldehyde has a spicy fragrance; limonene has a unique fragrance; linalool has a strong blue and sweet woody green smell, like rosewood, with a soft aroma, light and transparent; basilene has grassy, floral and orange fragrances The scent of flower oil is fresh and clear; myrcene exists in the buds of Chinese prickly ash and has a light balsamic scent; linalyl acetate has floral and fruity aromas; perillyl alcohol has grassy, slightly woody and floral aromas; citral has lemony aromas fragrance. The results showed that the content of aroma substances in different proportions of prickly ash bud leaves, perilla leaves and fragrant leaves was different.

试验例3Test Example 3

取50 g花椒芽、紫苏和碰碰香混合粉末(花椒芽10 g、紫苏20 g、碰碰香20 g)制备清辛香提取物,其具体实施步骤与实施例1相同,只将萃取溶剂换为乙醇,制得的浓缩物为提取物G,检测提取物A和提取物G香气物质(紫苏醛、柠檬烯、罗勒烯、芳樟醇和月桂烯)的含量,并将两个提取物溶于体积分数95%的乙醇中得到调香溶液,并将调香溶液均匀喷洒在烟丝上,使提取物的添加量占烟丝重量的0.05%,依照常规加料工艺程序,平衡水分至14%,在其它条件一致的情况下,烟丝经卷烟机卷制成检测样品香烟,评吸专家对加香卷烟进行感官质量评价,结果见下表3。Take 50 g of Chinese prickly ash buds, basil and Pangpangxiang mixed powder (10 g of prickly ash buds, 20 g of basil, and 20 g of Pangpangxiang) to prepare a clear spice extract. The specific implementation steps are the same as those in Example 1, except that The extraction solvent was changed to ethanol, and the obtained concentrate was extract G. The contents of aroma substances (perillaldehyde, limonene, basilene, linalool and myrcene) in extract A and extract G were detected, and the two were extracted. The substance is dissolved in ethanol with a volume fraction of 95% to obtain a flavoring solution, and the flavoring solution is evenly sprayed on the cut tobacco, so that the addition amount of the extract accounts for 0.05% of the weight of the cut tobacco. According to the conventional feeding process, the moisture content is balanced to 14%. , under the same conditions as other conditions, the cut tobacco was rolled by the cigarette machine to make the test sample cigarette, and the evaluation experts carried out the sensory quality evaluation of the flavored cigarette. The results are shown in Table 3 below.

表3 不同萃取剂提取清辛香物质对卷烟感官质量的影响。Table 3 Effects of different extractants on the sensory quality of cigarettes.

Figure DEST_PATH_IMAGE006
Figure DEST_PATH_IMAGE006

结果表明,采用乙醚溶剂得到的提取物主要香气物质含量多于采用乙醇溶剂得到的香气物质,结合感官评吸结果,表明添加提取物A的卷烟烟气香味饱满丰富,清辛香突出,增加特色香味效果明显。The results showed that the content of main aroma substances in the extract obtained by using ether solvent was more than that obtained by using ethanol solvent. Combined with the sensory evaluation results, it showed that the cigarette smoke added with extract A had full and rich aroma, prominent clear and spicy aroma, and increased characteristics. The fragrance effect is obvious.

试验例4Test Example 4

将实施例1得到的提取物A,将提取物A溶于体积分数95%的乙醇中得到调香溶液,并将调香溶液均匀喷洒在烟丝上,使提取物的添加量占烟丝重量的0.02%、0.04%、0.06%和0.08%,依照常规加料工艺程序,平衡水分至14%,在其它条件一致的情况下,烟丝经卷烟机卷制成检测样品香烟,评吸专家对加香卷烟进行感官质量评价,结果见下表4。The extract A obtained in Example 1 was dissolved in ethanol with a volume fraction of 95% to obtain a flavoring solution, and the flavoring solution was evenly sprayed on the cut tobacco, so that the addition amount of the extract accounted for 0.02 of the weight of the cut tobacco. %, 0.04%, 0.06% and 0.08%, according to the conventional feeding process, the moisture content is balanced to 14%. Under the condition that other conditions are the same, the shredded tobacco is rolled into the test sample cigarette by the cigarette machine. Sensory quality evaluation, the results are shown in Table 4 below.

其中,感官总分(T)=(A+B)×2.0+(C+D)×1.5+E+F+G+H。Among them, the total sensory score (T)=(A+B)×2.0+(C+D)×1.5+E+F+G+H.

表4 清辛香提取物不同添加量对卷烟感官质量的影响。Table 4 The effect of different addition amounts of clear spice extracts on the sensory quality of cigarettes.

Figure DEST_PATH_IMAGE008
Figure DEST_PATH_IMAGE008

结果表明,从香气质(A)、香气量(B)、浓度(C)、柔细度(D)、余味(E)、杂气(G)、刺激性(H)、劲头(F)8个方面打分,添加0.04%和0.06%时感官质量均较好,得分分别为68.25和68.75,整体而言,添加0.06%时感官质量最佳。The results show that there are 8 factors including aroma quality (A), aroma quantity (B), concentration (C), softness (D), aftertaste (E), miscellaneous gas (G), irritation (H) and energy (F). In terms of scores, the sensory quality was better when 0.04% and 0.06% were added, and the scores were 68.25 and 68.75, respectively. Overall, the sensory quality was the best when 0.06% was added.

综上所述,本发明作为一种具有清辛香型的天然植物提取物,用在卷烟加香中可以明显的增加卷烟清辛香特点,值得在卷烟创新性生产中应用推广。To sum up, the present invention, as a natural plant extract with a clear and spicy flavor, can significantly increase the clear and spicy flavor of cigarettes when used in cigarette flavoring, and is worthy of application and promotion in innovative cigarette production.

上述实施例为本发明实施方式的举例说明,本发明的实施方式并不受上述实施例的限制,其它任何未背离本发明精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。The above examples are examples of the embodiments of the present invention, and the embodiments of the present invention are not limited by the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principle of the present invention are all Should be equivalent replacement manners, all are included within the protection scope of the present invention.

Claims (6)

1.一种清辛香型烟用香料的制备方法,其特征在于,包括以下步骤:1. a preparation method of clear and spicy flavor type tobacco flavor, is characterized in that, comprises the following steps: (1)预处理:摘取新鲜花椒芽叶、紫苏叶和碰碰香叶清洗,在50-70℃条件下烘干,研磨后过筛;(1) Pretreatment: pick fresh prickly ash sprouts, perilla leaves and pumice leaves, wash, dry at 50-70°C, grind and sieve; (2)蒸馏萃取:取花椒芽、紫苏叶和碰碰香粉末进行混合,加入重量为粉末总重量10-20倍的蒸馏水,水浴3-5h;再用乙醚在水浴环境下萃取香气物质,得到一次料液;(2) Distillation extraction: Mix Chinese prickly ash buds, perilla leaves, and fragrant fragrant powder, add distilled water with a weight of 10-20 times the total weight of the powder, and bath for 3-5 hours; then use ether to extract aroma substances in a water bath environment, get a feed liquid; (3)浓缩提纯:向步骤(2)萃取得到的一次料液中加入无水硫酸钠,干燥6-8 h,取上清液,得到二次料液;将二次料液在水浴的条件下进行旋转蒸发并浓缩,浓缩后的物质即为所述清辛香型烟用香料;(3) Concentration and purification: add anhydrous sodium sulfate to the primary feed solution extracted in step (2), dry for 6-8 h, and take the supernatant to obtain a secondary feed solution; place the secondary feed solution in a water bath under conditions Rotary evaporation is carried out down and concentrated, and the concentrated material is the clear spicy flavor type tobacco flavor; 所述清辛香型烟用香料,由如下质量百分比的原料制成:20%-30%花椒芽叶、30%-60%紫苏叶以及20%-40%碰碰香。The clear and spicy flavor type tobacco flavor is prepared from the following raw materials by mass percentage: 20%-30% of prickly ash sprouts, 30%-60% of perilla leaves and 20%-40% of pumice incense. 2.如权利要求1所述的制备方法,其特征在于,步骤(2)中每50g花椒芽、紫苏叶和碰碰香的混合粉末中加入30-50 mL乙醚进行萃取。2 . The preparation method according to claim 1 , wherein in step (2), 30-50 mL of ether is added to the mixed powder of each 50 g of Chinese prickly ash buds, perilla leaves and incense sticks for extraction. 3 . 3.如权利要求1所述的制备方法,其特征在于,步骤(3)中每50g花椒芽、紫苏叶和碰碰香的混合粉末经萃取后得到的一次料液中加入10-30 g无水硫酸钠。3. preparation method as claimed in claim 1 is characterized in that, in step (3), every 50g mixed powder of Chinese prickly ash sprouts, perilla leaves and incense sticks is added to the primary feed liquid obtained after extraction by adding 10-30 g Anhydrous sodium sulfate. 4.如权利要求1所述的制备方法,其特征在于,步骤(2)中所述水浴温度为55-65℃。4 . The preparation method according to claim 1 , wherein the temperature of the water bath in step (2) is 55-65° C. 5 . 5.如权利要求1所述的制备方法,其特征在于,步骤(3)中所述水浴温度为35-50℃。5 . The preparation method of claim 1 , wherein the temperature of the water bath in step (3) is 35-50° C. 6 . 6.如权利要求1所述的制备方法,其特征在于,所述的清辛香型烟用香料,由如下质量百分比的原料制成:20%花椒芽叶、40%紫苏叶以及40%碰碰香。6. preparation method as claimed in claim 1 is characterized in that, described clear and spicy flavor type tobacco flavor, is made by the raw material of following mass percentage: 20% prickly ash sprouts, 40% perilla leaves and 40% Touch the fragrance.
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