CN102952638A - Preparation method and application of tobacco endogenous spice of Boshan aromatic tobacco - Google Patents
Preparation method and application of tobacco endogenous spice of Boshan aromatic tobaccoDownload PDFInfo
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Abstract
Description
Translated fromChinese技术领域technical field
本发明属于卷烟生产技术领域，具体涉及一种保山香料烟烟草内源性香料的制备方法和应用。 The invention belongs to the technical field of cigarette production, and in particular relates to a preparation method and application of endogenous spices of Baoshan oriental tobacco. the
背景技术Background technique
目前卷烟行业制备烟用香料，基本都是使用常用的溶剂提取，将得到的提取物添加在梗丝、烟纸浆或烟叶中，以达到增进吃味，提升香气的作用。这种传统的提取方法工艺繁琐，耗时长，有效成分遭到破坏且提取物价值低。因此，开发一种提取效率高、减少有效成分破坏、能将提取物精细化分离且附加值高的烟草香料制备方法成为新的研究方向。 At present, the tobacco flavors prepared by the cigarette industry are basically extracted with commonly used solvents, and the obtained extracts are added to cut stems, tobacco pulp or tobacco leaves to improve taste and aroma. This traditional extraction method is cumbersome and time-consuming, the active ingredients are destroyed and the value of the extract is low. Therefore, it has become a new research direction to develop a tobacco spice preparation method with high extraction efficiency, reduced destruction of active ingredients, fine separation of extracts and high added value. the
香料烟（茄科，烟草属），为一年生草本植物，其株型紧凑，叶片小， 茎秆细，易燃烧，填充力强，芳香气味好，香浓味醇，故有“香料烟”之称。香料烟又称土耳其烟、东方型烟，原产于地中海沿岸国家，是红花烟草（Nicotianatobacum）的一种特殊烟草类型。由于香料烟具有浓郁芳香和纯净吃味的品质特点，在烟草制品中有着特殊的应用价值，是生产混合型、外香型和东方型卷烟及斗烟丝的重要原料之一。尤其是混合型卷烟具有劲足、味浓、用料广泛、可有效降低焦油含量从而减轻吸烟对人体健康的危害特点，深受吸烟者的青睐，成为当今世界流行的卷烟类型。目前，中国香料烟主要在云南保山、新疆、浙江、湖北进行规模生产。 Oriented tobacco (Solanaceae, Nicotiana) is an annual herb with compact plant type, small leaves, thin stems, easy to burn, strong filling power, good aroma, strong fragrance and mellow taste, so it has the name of "Oriental Tobacco". say. Oriented tobacco, also known as Turkish tobacco and oriental tobacco, originates in countries along the Mediterranean Sea and is a special tobacco type of Nicotianatobacum. Because of its rich aroma and pure taste, oriental tobacco has special application value in tobacco products, and is one of the important raw materials for the production of mixed, outer-flavored and oriental cigarettes and pipe tobacco. In particular, the blended cigarette has the characteristics of strong strength, strong flavor, wide range of materials, and can effectively reduce the tar content and reduce the harm of smoking to human health. It is favored by smokers and has become a popular type of cigarette in the world today. At present, Chinese oriental tobacco is mainly produced on a large scale in Baoshan, Yunnan, Xinjiang, Zhejiang, and Hubei. the
目前采用香料烟制备烟草内源性香料的方法都是采用溶剂提取的方法。提取方法工艺繁琐，耗时长，提取物不澄清，应用效果不佳，价值低。 At present, the methods for preparing tobacco endogenous spices from oriental tobacco all adopt the method of solvent extraction. The extraction method is cumbersome and time-consuming, the extract is not clear, the application effect is not good, and the value is low. the
发明内容Contents of the invention
本发明的目的是针对现有烟草香料制备技术的不足，尤其是烟草内源性香料的制备技术不足，提供保山香料烟烟草内源性香料的制备方法。 The object of the present invention is to provide a method for preparing endogenous tobacco flavors of Baoshan oriental tobacco aiming at the deficiencies in the existing technology for preparing tobacco flavors, especially the technology for preparing endogenous tobacco flavors. the
本发明的另一个目的是提供所述制备方法制备得到的保山香料烟烟草内源性香料。Another object of the present invention is to provide the endogenous flavor of Baoshan oriental tobacco prepared by the preparation method.
本发明还有一目的是提供所述保山香料烟烟草内源性香料在卷烟生产方面的应用。Another object of the present invention is to provide the application of the endogenous spices of Baoshan oriental tobacco in cigarette production.
本发明的目的通过以下技术方案予以实现： The purpose of the present invention is achieved through the following technical solutions:
提供一种保山香料烟烟草内源性香料的制备方法，其特征在于包括以下步骤：A method for preparing Baoshan oriental tobacco tobacco endogenous flavor is provided, which is characterized by comprising the following steps:
（1）将保山香料烟碎末放入超高压提取罐，加入8～12倍量的提取溶剂，室温浸泡后加压至100MPa～600MPa ，保压1～10min 后，立即卸压，放出提取液，过滤，取滤液浓缩得到浓缩液待用；(1) Put the minced Baoshan flavored tobacco into an ultra-high pressure extraction tank, add 8 to 12 times the amount of extraction solvent, soak at room temperature, pressurize to 100MPa to 600MPa, keep the pressure for 1 to 10min, release the pressure immediately, and release the extract , filtered, and the filtrate was concentrated to obtain a concentrated solution for later use;
（2）大孔树脂进行装柱预处理，将步骤（1）制备得到的浓缩液作为上样液上样，流速控制为5mL/min，用体积比浓度为30～80%的乙醇作为洗脱液洗脱，流速控制在3mL/min，洗致流出液基本无色，收集乙醇洗脱液，将乙醇洗脱液浓缩即得。(2) The macroporous resin is pretreated for column packing, the concentrated solution prepared in step (1) is used as the sample solution, the flow rate is controlled at 5mL/min, and ethanol with a volume ratio concentration of 30-80% is used as the eluent elution, the flow rate is controlled at 3mL/min, the effluent is basically colorless after washing, the ethanol eluate is collected, and the ethanol eluate is concentrated.
优选地，步骤（1）所述保山香料烟碎末的粒度为50～200目。包括将保山香料烟叶粉碎得到的碎片和/或卷烟生产过程收集的废弃烟末。 Preferably, the particle size of the Baoshan spice powder in step (1) is 50-200 mesh. Including shreds obtained by crushing Baoshan oriental tobacco leaves and/or waste tobacco dust collected during the cigarette production process. the
更为优选地，所述保山香料烟为云南保山地区种植的芳香型香料烟品种“巴斯玛”（“柯玛蒂尼”或“克撒锡”系列）。通常分为A1（顶部一级）、A2（中部一级）、A3（中下部一级）、B1（顶部二级）、B2（中部二级）、B3（中下部二级）、K1（顶部三级）、K2（中部三级）、K3（下部三级）9个等级，9个等级的都可以采用本发明方法制备烟草香料。 More preferably, the Baoshan oriental tobacco is an aromatic oriental tobacco variety "Basma" ("Komatini" or "Kesarxi" series) grown in Baoshan, Yunnan. Usually divided into A1 (top level one), A2 (middle level one), A3 (middle and lower level one), B1 (top level two), B2 (middle level two), B3 (middle level two), K1 (top level Three grades), K2 (the third grade in the middle), and K3 (the third grade in the lower part) 9 grades, all of which can adopt the method of the present invention to prepare tobacco spices. the
优选地，步骤（1）所述提取溶剂为乙醇或水，或者乙醇和水的混合溶液，混合比例不做严格限定； Preferably, the extraction solvent in step (1) is ethanol or water, or a mixed solution of ethanol and water, and the mixing ratio is not strictly limited;
步骤（1）所述室温浸泡的浸泡时间为30～60min；The soaking time of the room temperature soaking in step (1) is 30-60 minutes;
步骤（1）所述浓缩是将滤液浓缩至香料烟原料重1.5～2.5倍；可采用50～60℃、真空度0.04～0.06Mpa的条件下浓缩。The concentration in the step (1) is to concentrate the filtrate to 1.5-2.5 times the weight of the oriental tobacco raw material; it can be concentrated under the conditions of 50-60°C and a vacuum degree of 0.04-0.06Mpa.
步骤（2）所述大孔吸附树脂优选为AB-8、D101、ADS-17、ADS-F8、ADS-7、NKA-9等，最为优选是AB-8和D101；装柱预处理的操作方法参照市购的大孔树脂的产品说明书。 The macroporous adsorption resin in step (2) is preferably AB-8, D101, ADS-17, ADS-F8, ADS-7, NKA-9, etc., most preferably AB-8 and D101; the operation of column packing pretreatment The method refers to the product manual of the commercially available macroporous resin. the
步骤（2）所述的洗脱液为体积比浓度是30～80%的乙醇水溶液，优选30%、40%、50%、60%、65%、70%、75%的体积比浓度。 The eluent in step (2) is an aqueous ethanol solution with a volume concentration of 30-80%, preferably 30%, 40%, 50%, 60%, 65%, 70%, or 75%. the
步骤（2）所述将乙醇洗脱液浓缩是浓缩至原料（香料烟原料）质量的10%。可采用50～60℃、真空度0.04～0.06Mpa条件下浓缩。 Concentrating the ethanol eluent in step (2) is to concentrate to 10% of the mass of the raw material (oriental tobacco raw material). It can be concentrated under the conditions of 50-60°C and vacuum degree of 0.04-0.06Mpa. the
本发明同时提供所述制备方法制备得到的烟草内源性香料。 The invention also provides the tobacco endogenous flavor prepared by the preparation method. the
本发明提供了所述制备得到的烟草香料在卷烟方面的应用。 The invention provides the application of the prepared tobacco flavor in cigarettes. the
本发明方法的有益效果： The beneficial effect of the inventive method:
与烟用香料息息相关的香味和吃味可以说是卷烟的生命，是消费者赖以识别卷烟品牌的重要依据，改变香味和吃味意味着改变卷烟的生命表征指标，影响的是一个品牌的象征，所以长久以来，在烟用香料的制备方面一直沿用的是溶剂提取的技术手段，没有根本性的改进。虽然自20世纪90年代以来，国外许多学者利用超高压（Ultra high pressure，UHP）技术在改善食品的香味方面取得了较好的效果；大孔吸附树脂技术是近年来国内外新发展的处理技术，最早用于废水处理、医药工业、化学工业、分析化学、临床检定和治疗等领域，近年来在我国广泛用于中草药有效成分的提取、分离、纯化工作中，在医药领域特别是天然药物精制中广为应用。超高压和大孔吸附树脂技术的优越性已被认识和运用已久，但从未有报道将超高压或大孔吸附树脂技术应用于烟草香料的制备中，更未见将二者联用于烟草生产技术领域产生显著技术效果的技术方案。The aroma and taste closely related to tobacco flavors can be said to be the life of cigarettes and an important basis for consumers to identify cigarette brands. Changing the aroma and taste means changing the vital signs of cigarettes, which affects the symbol of a brand , so for a long time, the technical means of solvent extraction has been used in the preparation of tobacco flavors, without fundamental improvement. Although since the 1990s, many foreign scholars have achieved good results in improving the aroma of food by using Ultra high pressure (UHP) technology; macroporous adsorption resin technology is a newly developed processing technology at home and abroad in recent years. It was first used in the fields of wastewater treatment, pharmaceutical industry, chemical industry, analytical chemistry, clinical testing and treatment. In recent years, it has been widely used in the extraction, separation and purification of active ingredients of Chinese herbal medicines in my country. In the field of medicine, especially in the refining of natural medicines widely used in China. The superiority of ultra-high pressure and macroporous adsorption resin technology has been recognized and used for a long time, but there has never been any report on the application of ultra-high pressure or macroporous adsorption resin technology to the preparation of tobacco flavors, let alone the combination of the two. Technical solutions that produce significant technical effects in the field of tobacco production technology.
本发明克服本技术领域的技术定势和思维局限，彻底改变了烟草技术领域传统的烟草香料的溶剂提取制备路线，提供了高压提取和柱分离的整体联用技术方案，成功利用高压提取和大孔树脂柱的分离技术，简单易行地制备得到理想的烟草香料，获得了意想不到的技术效果。本发明方法简单实用，操作方便，成本较低，树脂可反复使用，并大大节省时间，提取的有效致香成分价值高，更为充分地利用了烟草原料。 The present invention overcomes the technical stereotypes and thinking limitations in this technical field, completely changes the traditional solvent extraction preparation route of tobacco spices in the field of tobacco technology, provides an overall combined technical scheme of high-pressure extraction and column separation, and successfully utilizes high-pressure extraction and large-scale The separation technology of the porous resin column can easily prepare ideal tobacco spices and obtain unexpected technical effects. The method of the invention is simple and practical, easy to operate, low in cost, the resin can be used repeatedly, and greatly saves time, the extracted effective aroma components are of high value, and the tobacco raw material is more fully utilized. the
本发明在原料的选择方面，优选了云南保山生产的香料烟作为制备原料。保山香料烟的叶片小而厚，香气量足，香气质好，香气风格突出，化学成分协调，吃味醇和，余味舒适，燃烧性好，现有技术用来生产混合型卷烟。但现有技术采用溶剂提取保山香料烟的方法制备烟用香料，得到的提取物不澄清，应用效果不佳，价值偏低，虽然卷烟抽吸品质有所提升，但存在着有刺激、有残留、欠谐调的缺陷。本发明总结发现高压提取和柱分离的整体联用技术方案特别适合保山香料烟原料，制备的烟用香料，加入卷烟后，能更加显著地能增加烟草本香和香气饱满度，谐调烟气，使烟气细腻柔和，增加甜润感，提高卷烟的吸味品质，说明本发明制备方法很好地获取了保山香料烟烟草内源性的增香成分。 In terms of raw material selection in the present invention, oriental tobacco produced in Baoshan, Yunnan Province is preferably used as the raw material for preparation. Baoshan oriental tobacco has small and thick leaves, sufficient aroma, good aroma, outstanding aroma style, coordinated chemical composition, mellow taste, comfortable aftertaste, and good combustibility. The existing technology is used to produce mixed cigarettes. However, in the prior art, the method of solvent extraction of Baoshan oriental tobacco is used to prepare tobacco spices. The obtained extract is not clear, the application effect is not good, and the value is low. Although the smoking quality of cigarettes has improved, there are irritation and residues. , Less harmonious defects. According to the summary of the present invention, it is found that the overall combined technical scheme of high-pressure extraction and column separation is particularly suitable for Baoshan oriental tobacco raw materials, and the tobacco spices prepared by adding them to cigarettes can more significantly increase the original aroma and aroma fullness of tobacco, and harmonize the smoke. The smoke is fine and soft, the sweetness is increased, and the smoking quality of the cigarette is improved, which shows that the preparation method of the present invention can obtain the endogenous aroma-enhancing components of Baoshan oriental tobacco. the
具体实施方式Detailed ways
下面结合具体实施例进一步详细说明本发明。除非特别说明，本发明实施例采用的试剂和原料均为市购的试剂和原料。 The present invention will be further described in detail below in conjunction with specific examples. Unless otherwise specified, the reagents and raw materials used in the examples of the present invention are commercially available reagents and raw materials. the
实施例1 Example 1
（1）取保山香料烟（烟叶购于云南保山柯玛蒂尼-巴斯玛，包括将保山香料烟叶粉碎得到的碎片和/或卷烟生产过程收集的废弃烟末，为了方便说明本实施例此采用中部一级，但并不因此限定本实施例）烟叶300g，粉碎后（约50～200目）放入超高压提取罐（本实施例采用UHP900ⅹ2超高压装置），加入10倍量体积比浓度为95% 的乙醇水溶液，室温浸泡保山香料烟碎末30min，加压至100MPa，保压1min后立即卸压，反复3次，将提取液过滤，将滤液浓缩至450g。(1) Take Baoshan oriental tobacco (tobacco leaves purchased from Komartini-Basma in Baoshan, Yunnan, including fragments obtained by crushing Baoshan oriental tobacco leaves and/or waste tobacco dust collected during cigarette production, for the convenience of describing this example The first grade in the middle is used, but this example is not limited thereto) 300g of tobacco leaves are crushed (about 50-200 mesh) and put into an ultra-high pressure extraction tank (UHP900ⅹ2 ultra-high pressure device is used in this example), and 10 times the volume ratio concentration is added It is 95% ethanol aqueous solution, soak Baoshan spice powder at room temperature for 30 minutes, pressurize to 100MPa, keep the pressure for 1 minute, and immediately release the pressure, repeat 3 times, filter the extract, and concentrate the filtrate to 450g.
（2）AB-8大孔树脂500g，按说明书要求装柱预处理，（可参见http://www.tech-sep.com/a/techprofile/2011/1011/189.html），将步骤（1）所得450g样品上样，流速控制在5mL/min，再用体积比浓度为30%的乙醇水溶液洗脱，流速控制在3mL/min，洗致流出液基本无色，收集乙醇洗脱液，浓缩至30g，即得保山香料烟烟草内源性香料。 (2) AB-8 macroporous resin 500g, according to the requirements of the instructions for column packing pretreatment, (see http://www.tech-sep.com/a/techprofile/2011/1011/189.html), the step ( 1) The obtained 450g sample is loaded, the flow rate is controlled at 5mL/min, and then eluted with an ethanol aqueous solution with a volume ratio concentration of 30%, and the flow rate is controlled at 3mL/min. The effluent is basically colorless after washing, and the ethanol eluate is collected. Concentrate to 30g to obtain the endogenous flavor of Baoshan oriental tobacco. the
实施例2 Example 2
（1）取保山香料烟（品种同实施例1）烟叶300g，粉碎后（约50～200目）放入超高压提取罐（同实施例1），加入10倍量体积比浓度为95% 的乙醇水溶液，室温浸泡保山香料烟碎末30min，加压至100MPa，保压1min后立即卸压，反复3次，将提取液过滤，将滤液浓缩至450g。(1) Take 300g of Baoshan oriental tobacco leaves (the variety is the same as in Example 1), crush them (about 50-200 mesh) and put them into an ultra-high pressure extraction tank (same as in Example 1), add 10 times the volume ratio of 95% Ethanol aqueous solution, soak Baoshan flavor tobacco powder at room temperature for 30 minutes, pressurize to 100MPa, hold the pressure for 1 minute, release the pressure immediately, repeat 3 times, filter the extract, and concentrate the filtrate to 450g.
（2）D101大孔树脂500g，按说明要求（http://www.sep-bj.com/news/html/?456.html）装柱预处理，将步骤（1）所得450g样品上样，流速控制在5mL/min，再用体积比浓度为30%的乙醇水溶液洗脱，流速控制在3mL/min，洗致流出液基本无色，收集乙醇洗脱液，浓缩至30g，既得保山香料烟烟草内源性香料。 (2) 500g of D101 macroporous resin, according to the instructions (http://www.sep-bj.com/news/html/?456.html) for column pretreatment, and 450g of the sample obtained in step (1) was loaded, The flow rate was controlled at 5mL/min, and then eluted with an ethanol aqueous solution with a concentration of 30% by volume. The flow rate was controlled at 3mL/min. Tobacco endogenous flavours. the
实施例3 Example 3
（1）取保山香料烟（品种同实施例1，顶部一级）烟叶300g，粉碎后（约50～200目）放入超高压提取罐（UHP900ⅹ2超高压装置），加入8倍量水，室温浸泡60min，加压至600MPa ，保压10min后立即卸压，反复3次，将提取液过滤，将滤液浓缩至450g。(1) Take 300g of Baoshan oriental tobacco leaves (the variety is the same as in Example 1, the top grade), crush them (about 50-200 mesh) and put them into an ultra-high pressure extraction tank (UHP900ⅹ2 ultra-high pressure device), add 8 times the amount of water, and leave at room temperature Soak for 60 minutes, pressurize to 600MPa, release the pressure immediately after holding the pressure for 10 minutes, repeat 3 times, filter the extract, and concentrate the filtrate to 450g.
（2）ADS-17大孔树脂500g，按说明要求装柱预处理，将步骤（1）所得450g样品上样，流速控制在5mL/min，再用体积比浓度为40%的乙醇水溶液洗脱，流速控制在3mL/min，洗致流出液基本无色，收集乙醇洗脱液，浓缩至30g，即得保山香料烟烟草内源性香料。 (2) 500g of ADS-17 macroporous resin, according to the requirements of the instructions, pre-pack the column, load the 450g sample obtained in step (1), control the flow rate at 5mL/min, and then elute with ethanol water solution with a volume ratio concentration of 40% , the flow rate is controlled at 3mL/min, the effluent is basically colorless after washing, the ethanol eluate is collected, concentrated to 30g, and the endogenous flavor of Baoshan oriental tobacco is obtained. the
实施例4 Example 4
（1）取保山香料烟（顶部二级）烟叶300g，粉碎后（约50 ～200目）放入超高压提取罐（UHP900ⅹ2超高压装置），加入11倍量体积比浓度为70%的乙醇水溶液，室温浸泡40min，加压至400MPa，保压8min后立即卸压，反复3次，将提取液过滤，将滤液浓缩至450g。(1) Take 300g of Baoshan oriental tobacco (top grade 2) tobacco leaves, crush them (about 50 to 200 mesh) and put them into an ultra-high pressure extraction tank (UHP900ⅹ2 ultra-high pressure device), add 11 times the volume ratio of ethanol aqueous solution with a concentration of 70% , soak at room temperature for 40 minutes, pressurize to 400MPa, release the pressure immediately after holding the pressure for 8 minutes, repeat 3 times, filter the extract, and concentrate the filtrate to 450g.
（2）ADS-17大孔树脂500g，按说明要求（http://cn.diytrade.com/china/pd/7290015/ADS_17大孔吸附树脂.html）装柱预处理，将步骤（1）所得450g样品上样，流速控制在5mL/min，再用体积比浓度为50%的乙醇水溶液洗脱，流速控制在3mL/min，洗致流出液基本无色，收集乙醇洗脱液，浓缩至30g，即得保山香料烟烟草内源性香料。 (2) ADS-17 macroporous resin 500g, according to the instructions (http://cn.diytrade.com/china/pd/7290015/ADS_17 macroporous resin.html) pretreatment column, the step (1) 450g sample was loaded, the flow rate was controlled at 5mL/min, and then eluted with ethanol aqueous solution with a volume ratio concentration of 50%, the flow rate was controlled at 3mL/min, the effluent was basically colorless after washing, and the ethanol eluate was collected and concentrated to 30g , that is, the endogenous flavor of Baoshan oriental tobacco tobacco. the
实施例5 Example 5
（1）取保山香料烟烟叶300g，粉碎后（约50～200目）放入超高压提取罐（UHP900ⅹ2超高压装置），加入12倍量体积比浓度为85%的乙醇水溶液，室温浸泡50min，加压至300MPa，保压5min，立即卸压，反复3次，将提取液过滤，将滤液浓缩至450g。(1) Take 300g of Baoshan oriental tobacco leaves, crush them (about 50-200 meshes), put them into an ultra-high pressure extraction tank (UHP900ⅹ2 ultra-high pressure device), add 12 times the volume ratio of ethanol solution with a concentration of 85%, soak at room temperature for 50 minutes, Pressurize to 300MPa, keep the pressure for 5min, release the pressure immediately, repeat 3 times, filter the extract, and concentrate the filtrate to 450g.
（2）ADS-7大孔树脂500g，按说明要求（郑州勤实科技有限公司出品）装柱预处理，将步骤（1）所得450g样品上样，流速控制在5mL/min，再用体积比浓度为60%的乙醇洗脱，流速控制在3mL/min，洗致流出液基本无色，收集乙醇洗脱液，浓缩至30g，即得保山香料烟烟草内源性香料。 (2) ADS-7 macroporous resin 500g, according to the instructions (produced by Zhengzhou Qinshi Technology Co., Ltd.) for column pretreatment, load 450g of the sample obtained in step (1), control the flow rate at 5mL/min, and then use the volume ratio Elute with 60% ethanol and control the flow rate at 3mL/min until the effluent is basically colorless. Collect the ethanol eluate and concentrate it to 30g to obtain the endogenous flavor of Baoshan oriental tobacco tobacco. the
实施例6 Example 6
（1）取保山香料烟烟叶300g，粉碎后（约50～200目）放入超高压提取罐（UHP900ⅹ2超高压装置），加入9倍量水，室温浸泡60min，加压至500MPa，保压5min后立即卸压，反复3次，将提取液过滤，将滤液浓缩至450g。(1) Take 300g of Baoshan oriental tobacco leaves, crush them (about 50-200 mesh), put them into an ultra-high pressure extraction tank (UHP900ⅹ2 ultra-high pressure device), add 9 times the amount of water, soak at room temperature for 60 minutes, pressurize to 500MPa, and hold the pressure for 5 minutes Immediately after that, the pressure was released, and repeated 3 times, the extract was filtered, and the filtrate was concentrated to 450g.
（2）NKA-9大孔树脂500g，按说明要求（http://baike.baidu.com/view/6355904.htm）装柱预处理，将上一步450g样品上样，流速控制在5mL/min，再用体积比浓度为75%的乙醇水溶液洗脱，流速控制在3mLmin，洗致流出液基本无色，收集乙醇洗脱液，浓缩至30g，即得保山香料烟烟草内源性香料。 (2) NKA-9 macroporous resin 500g, according to the instructions (http://baike.baidu.com/view/6355904.htm) for column pretreatment, load the 450g sample in the previous step, and control the flow rate at 5mL/min , and then eluted with an aqueous ethanol solution with a volume ratio concentration of 75%, and the flow rate was controlled at 3mLmin. the
实施例7 Example 7
取保山香料烟（同实施例1和2）烟叶300g，粉碎后（约50～200目）放入超高压提取罐（UHP900ⅹ2超高压装置），加入10倍量体积比浓度为95% 的乙醇水溶液，室温浸泡保山香料烟碎末30min，加压至100MPa，保压1min后立即卸压，反复3次，将提取液过滤，将滤液浓缩至450g。AB-8大孔树脂500g，按说明要求（http://www.tech-sep.com/a/techprofile/2011/1011/189.htTake 300g of Baoshan oriental tobacco leaves (same as in Examples 1 and 2), crush them (about 50-200 mesh) and put them into an ultra-high pressure extraction tank (UHP900ⅹ2 ultra-high pressure device), add 10 times the volume ratio of ethanol aqueous solution with a concentration of 95% , Soak Baoshan spice powder at room temperature for 30 minutes, pressurize to 100MPa, keep the pressure for 1 minute and then release the pressure immediately, repeat 3 times, filter the extract, and concentrate the filtrate to 450g. AB-8 macroporous resin 500g, according to the instructions (http://www.tech-sep.com/a/techprofile/2011/1011/189.ht
ml）装柱预处理，将步骤（1）所得450g样品上样，流速控制在5mL/min，再用体积比浓度为30%的乙醇水溶液洗脱，流速控制在3mL/min，洗致流出液基本无色，收集乙醇洗脱液，浓缩至30g，即得保山香料烟烟草内源性香料。ml) column pretreatment, load the 450g sample obtained in step (1), control the flow rate at 5mL/min, and then elute with ethanol aqueous solution with a volume ratio concentration of 30%, control the flow rate at 3mL/min, and wash the effluent It is basically colorless, and the ethanol eluate is collected and concentrated to 30 g to obtain the endogenous flavor of Baoshan oriental tobacco tobacco.
作为对比，取保山香料烟（同上）烟叶300g，加入10倍量体积比95%乙醇，热回流提取，每次提取2小时，提取2次，两次提取液合并，过滤，浓缩至60克，即得对比香料。 As a comparison, take 300g of Baoshan oriental tobacco (same as above) tobacco leaves, add 10 times the volume ratio of 95% ethanol, heat reflux extraction, each extraction is 2 hours, extraction is 2 times, the two extractions are combined, filtered, and concentrated to 60 grams, Get contrasting spices. the
本发明制得的保山香料烟烟草内源性香料与对比香料相比较，外观上的区别是： Compared with the comparison spices, the endogenous spices of Baoshan oriental tobacco produced by the present invention have the following differences in appearance:
实施例8应用实验Embodiment 8 application experiment
粘稠状的烟用香料的质量及应用效果评价主要通过评吸结果进行。将本发明实施例1～6制备得到的烟用香料和实施例7制备得到的对比香料按照本技术领域常规用适量的水稀释后喷洒于烟丝上（按照添加重量比例为5‰为例），经相同的卷烟制备处理后由七人专业评吸小组进行评吸，以香气、协调、杂气、刺激性和余味五个指标，进行感官质量评价。实验结果见表1所示：The evaluation of the quality and application effect of viscous flavorings for tobacco is mainly carried out through the evaluation of smoking results. The flavors for tobacco prepared in Examples 1-6 of the present invention and the comparative flavor prepared in Example 7 were diluted with an appropriate amount of water according to the conventional techniques in the technical field, and then sprayed on shredded tobacco (according to the addition weight ratio of 5‰ as an example), After the same cigarette preparation and treatment, a seven-person professional smoking evaluation team conducts smoking evaluation, and evaluates sensory quality based on five indicators: aroma, coordination, miscellaneous smell, irritation and aftertaste. The experimental results are shown in Table 1:
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