技术领域Technical field
本发明属于电子烟生产技术领域，具体涉及一种特征香型的电子烟烟液微胶囊制备方法。The invention belongs to the technical field of electronic cigarette production, and specifically relates to a method for preparing characteristically fragrant electronic cigarette liquid microcapsules.
背景技术Background technique
电子烟通过电子控制加热烟液产生可抽吸的气溶胶，具有不燃烧、不产生二手烟危害等优点，具有广阔的市场前景。电子烟口味繁多，烟液一般呈透明或半透明，色彩丰富，曾满足了不同消费者需求。随着烟草行业的进一步规范化，对非烟风格的电子烟准入收紧，市售电子烟必然回归烟草口味风格。E-cigarettes generate smokeable aerosols by electronically controlling the heating of smoke liquid. They have the advantages of not burning and not producing the hazards of second-hand smoke, and have broad market prospects. E-cigarettes come in a variety of flavors, and the e-cigarette liquid is generally transparent or translucent and rich in color, which has met the needs of different consumers. With the further standardization of the tobacco industry and the tightening of access to non-smoking style e-cigarettes, commercially available e-cigarettes will inevitably return to tobacco-flavored styles.
目前，电子烟液中添加的烟草源物质以烟草精油、烟草花蕾油为主，油类赋以烟草风格的同时，仍能保持烟液的物理性状，但也造成抽吸口感不佳的现象，主要是因为精油及花蕾油以易挥发性烟草头香物质为主，并不能表达烟草完整香气风格。At present, the tobacco-derived substances added to e-cigarette liquid are mainly tobacco essential oil and tobacco bud oil. The oils give the tobacco style while still maintaining the physical properties of the e-cigarette liquid, but they also cause poor smoking taste. Mainly because essential oils and bud oils are mainly volatile tobacco top aroma substances and cannot express the complete aroma style of tobacco.
烟草浸膏作为另一种烟草再加工产物，一般采取水或乙醇作为溶剂，其中单独水提后，提取率一般大于90%，所得浸膏可具备较为全面的烟草风格特征。但浸膏在电子烟液中应用受限，一方面是因为其中的糖类、蛋白质、淀粉等大分子物质易沉淀，烟液外观不佳，另一方面，在电子烟加热过程中反应，上述物质产生的焦糊气味，会造成吸食感官品质不佳，还会影响电子烟雾化能力与雾化效果，从而限制了烟草浸膏的进一步应用。Tobacco extract, as another tobacco reprocessing product, generally uses water or ethanol as the solvent. After water extraction alone, the extraction rate is generally greater than 90%, and the resulting extract can have relatively comprehensive tobacco style characteristics. However, the application of extract in e-cigarette liquid is limited. On the one hand, it is because the sugars, proteins, starches and other macromolecular substances in it are easy to precipitate and the appearance of the e-cigarette liquid is not good. On the other hand, they react during the heating process of the e-cigarette. The above-mentioned The burnt smell produced by the substance will cause poor smoking sensory quality, and will also affect the vaporization ability and atomization effect of electronic cigarettes, thus limiting the further application of tobacco extract.
烟草浸膏原料来源广泛，主要包括碎片、烟末及烟叶，其中烟叶主要是因为烟叶等级不高，或自身化学成分失衡导致不适宜烟草加工使用，一般存在燃烧性、杂气、刺激性等负面影响。因此，对烟叶的合理使用目前仍是烟草行业研究的重要方向。Tobacco extract raw materials come from a wide range of sources, mainly including fragments, tobacco powder and tobacco leaves. Among them, tobacco leaves are mainly not suitable for tobacco processing and use because the tobacco leaves are not of high grade or their own chemical composition is imbalanced. They generally have negative effects such as flammability, miscellaneous gas, and irritation. Influence. Therefore, the rational use of tobacco leaves is still an important research direction in the tobacco industry.
杨梅浸膏是由杨梅干燥、发酵后，破碎并水提或醇提得到的棕红色膏体，具有典型的浓郁甜果香特征，是一种重要的烟用添加剂。杨梅浸膏的挥发性成分在电子烟中可赋予产品独特的杨梅醇化特征，丰富烟香；但杨梅浸膏中主要成分，比如大量糖类物质和氨基酸并没有起到传统卷烟中的应用效果，比如丰富香气、减轻刺激性、醇和烟气等作用。美拉德反应产物中含有大量与烟草协调的致香成分，且具有天然感强、香气饱满等优点，在改善烟草制品品质方面取得了良好的应用效果，因而美拉德反应成为制备烟用香料的重要途径。微胶囊技术是将小液滴、固体颗粒等包埋在微胶囊壁材中，成为流动性的颗粒。微胶囊化可以防止储存过程中芯材的挥发损失，并且可以保证芯材均匀释放。Bayberry extract is a brown-red paste obtained by drying and fermenting bayberries, then crushing and extracting with water or alcohol. It has a typical rich, sweet and fruity aroma and is an important tobacco additive. The volatile components of bayberry extract can give the product unique bayberry alcoholization characteristics in e-cigarettes and enrich the flavor of tobacco. However, the main components of bayberry extract, such as a large amount of sugars and amino acids, do not have the same effect as in traditional cigarettes. Such as enriching aroma, reducing irritation, alcohol and smoke. The Maillard reaction product contains a large number of aroma-causing ingredients that are coordinated with tobacco, and has the advantages of strong natural feeling and full aroma. It has achieved good application results in improving the quality of tobacco products. Therefore, the Maillard reaction has become a popular choice for the preparation of tobacco flavors. important ways. Microcapsule technology embeds small droplets, solid particles, etc. in microcapsule wall materials to become fluid particles. Microencapsulation can prevent the volatilization loss of the core material during storage and ensure uniform release of the core material.
目前有一些关于微胶囊技术制备电子烟烟液的相关专利。如专利CN201410402403.9公开了一种带微胶囊缓释的装置电子烟及微胶囊，通过烟液微胶囊化，隔绝了环境接触，保证烟液成分不受污染，并可感受不同味道。专利CN202111036865.X公开了一种用于电子烟烟液的微胶囊，壁材为β-环糊精或羟丙基-β-环糊精，芯材为烟草精油。专利CN201810929445.6提供了一种电子烟烟液，以环糊精为囊壁，以香精和烟碱为芯材，将香精和烟碱制成微胶囊型电子烟液。但目前尚未见到有将烟叶和杨梅的美拉德反应物微胶囊化后应用于电子烟的相关报道。基于此，研发了本申请。There are currently some patents related to the preparation of e-cigarette liquid using microcapsule technology. For example, patent CN201410402403.9 discloses an electronic cigarette with a microcapsule sustained release device and microcapsules. By microencapsulating the smoke liquid, it is isolated from environmental contact, ensuring that the components of the smoke liquid are not polluted, and different flavors can be experienced. Patent CN202111036865. Patent CN201810929445.6 provides an electronic cigarette liquid, which uses cyclodextrin as the capsule wall, essence and nicotine as core materials, and the essence and nicotine are made into microcapsule electronic cigarette liquid. However, there have been no reports on the microencapsulation of Maillard reactants from tobacco leaves and bayberry and their application in electronic cigarettes. Based on this, this application was developed.
发明内容Contents of the invention
本发明目的在于克服现有技术缺陷，提供一种特征香型的电子烟烟液微胶囊制备方法，其利用烟叶和杨梅浸膏中含有的大量蛋白质、糖类物质，通过美拉德反应进一步制备香气量丰富、香气品质更高的烟用香料并通过微胶囊技术包埋制备电子烟烟液微胶囊，不仅减少了烟叶浪费，同时制备的电子烟烟液微胶囊不仅具有浓郁的烟草香和杨梅的特征香气，同时增加了美拉德反应产物特征香韵，且保质期长、稳定性好，抽吸时烟雾量释放均匀稳定。The object of the present invention is to overcome the shortcomings of the existing technology and provide a method for preparing characteristic-flavor electronic cigarette liquid microcapsules, which utilizes a large amount of protein and sugar substances contained in tobacco leaves and bayberry extract to further prepare through the Maillard reaction. Tobacco spices with rich aroma and higher aroma quality are encapsulated by microencapsulation technology to prepare e-cigarette liquid microcapsules, which not only reduces the waste of tobacco leaves, but also prepares e-cigarette liquid microcapsules with rich tobacco aroma and bayberry. It also adds the characteristic aroma of the Maillard reaction product, has a long shelf life, good stability, and the smoke is released evenly and stably when inhaled.
为实现上述目的，本发明采用如下技术方案：In order to achieve the above objects, the present invention adopts the following technical solutions:
一种特征香型的电子烟烟液微胶囊制备方法，其具体包括以下步骤：A method for preparing characteristically fragrant electronic cigarette liquid microcapsules, which specifically includes the following steps:
1）在烟叶中加入果胶酶、蛋白酶、淀粉酶进行酶解反应，将酶解后的烟叶用水提取，提取液经离心、膜分离后，负压浓缩成烟草浸膏；1) Add pectinase, protease, and amylase to the tobacco leaves for enzymatic hydrolysis reaction, and extract the enzymatically hydrolyzed tobacco leaves with water. After centrifugation and membrane separation, the extract is concentrated under negative pressure into tobacco extract;
2）将烟草浸膏、杨梅浸膏、还原糖、氨基酸和溶剂混合均匀，调节反应体系的pH值为7-10，补水至体系中水分含量为12%-15%，搅拌均匀，控制体系温度为90-150℃反应1-3h，冷却后离心除杂，即得到美拉德反应物；2) Mix tobacco extract, bayberry extract, reducing sugar, amino acid and solvent evenly, adjust the pH value of the reaction system to 7-10, replenish water until the moisture content in the system is 12%-15%, stir evenly, and control the system temperature. React at 90-150°C for 1-3 hours, cool and then centrifuge to remove impurities to obtain the Maillard reactant;
3）将微胶囊包膜原料用水溶解后，缓慢加入美拉德反应物，对混合物进行高速分散，得到乳液微胶囊，喷雾干燥，得到电子烟烟液微胶囊，或按现有常规方法制备微胶囊。所得的电子烟具有浓郁的烟草香和杨梅的特征香型，且保质期长、稳定性好，抽吸时香气释放均匀稳定。3) After the microcapsule coating raw materials are dissolved in water, Maillard reactants are slowly added, and the mixture is dispersed at high speed to obtain emulsion microcapsules, which are spray-dried to obtain e-cigarette liquid microcapsules, or microcapsules can be prepared according to existing conventional methods. capsule. The obtained electronic cigarette has a rich tobacco aroma and the characteristic aroma of bayberry, and has a long shelf life and good stability, and the aroma is released evenly and stably when smoked.
具体的，步骤1）中，果胶酶、蛋白酶、淀粉酶添加量均为烟叶质量的0.1-0.8%。Specifically, in step 1), the added amounts of pectinase, protease, and amylase are 0.1-0.8% of the tobacco leaf mass.
进一步的，步骤1）中，酶解温度可以为40-50℃，酶解时间可以为5-12h。Further, in step 1), the enzymatic hydrolysis temperature can be 40-50°C, and the enzymatic hydrolysis time can be 5-12 hours.
进一步的，步骤1）中，酶解后的烟叶中可以加入烟叶质量5-10倍的水进行提取，提取温度50-75℃，提取时间1-2.5h。膜分离时，可以选用孔径为0.05-2.0μm的碳化硅管式膜，主要阻留分子量为20万-100万的物质，以及微细纤维、颗粒等悬浮物杂质。Further, in step 1), water with 5-10 times the mass of the tobacco leaves can be added to the enzymatically hydrolyzed tobacco leaves for extraction. The extraction temperature is 50-75°C and the extraction time is 1-2.5 hours. For membrane separation, you can choose a silicon carbide tubular membrane with a pore size of 0.05-2.0 μm, which mainly blocks substances with a molecular weight of 200,000-1 million, as well as suspended impurities such as fine fibers and particles.
具体的，步骤2）中，所述还原糖可以为木糖、阿拉伯糖、葡萄糖、果糖、甘露糖、半乳糖等中的一种或两种以上的混合物；所述氨基酸可以为脯氨酸、亮氨酸、色氨酸、苏氨酸、丝氨酸、苯丙氨酸等中的一种或两种以上的混合物。Specifically, in step 2), the reducing sugar can be one or a mixture of two or more of xylose, arabinose, glucose, fructose, mannose, galactose, etc.; the amino acid can be proline, One or a mixture of two or more of leucine, tryptophan, threonine, serine, phenylalanine, etc.
进一步的，步骤2）中，所述溶剂可以为丙二醇、甘油、乙二醇等中的一种或两种以上的混合物。Further, in step 2), the solvent may be one or a mixture of two or more of propylene glycol, glycerin, ethylene glycol, etc.
具体的，步骤2）中，以重量份计，可以将20份烟草浸膏、20-30份杨梅浸膏、10-15份还原糖、0.6-2.0份氨基酸和17-20份溶剂混合均匀。Specifically, in step 2), 20 parts of tobacco extract, 20-30 parts of bayberry extract, 10-15 parts of reducing sugar, 0.6-2.0 parts of amino acids and 17-20 parts of solvent can be mixed evenly by weight.
进一步的，步骤2）中，调节反应体系的pH值时，采用的酸性化合物可以为食用盐酸、醋酸、柠檬酸等中的一种或多种，采用的碱性化合物为氨水、Na0H、KOH等中的一种或多种。Further, in step 2), when adjusting the pH value of the reaction system, the acidic compound used can be one or more of edible hydrochloric acid, acetic acid, citric acid, etc., and the alkaline compound used is ammonia, NaOH, KOH, etc. one or more of them.
进一步的，步骤3）中，所述微胶囊包膜原料可以包括聚乙烯醇、环糊精、瓜尔胶、纤维素衍生物等中一种或两种以上的混合物。微胶囊包膜原料用水溶解后，获得质量浓度2-8%的微胶囊包膜原料溶液，微胶囊包膜原料溶液与美拉德反应物的质量比在1：5 -10之间。Further, in step 3), the microcapsule coating raw material may include one or a mixture of two or more of polyvinyl alcohol, cyclodextrin, guar gum, cellulose derivatives, etc. After the microcapsule coating raw material is dissolved in water, a microcapsule coating raw material solution with a mass concentration of 2-8% is obtained. The mass ratio of the microcapsule coating raw material solution and the Maillard reactant is between 1:5-10.
和现有技术相比，本发明制备方法的有益效果如下：Compared with the prior art, the beneficial effects of the preparation method of the present invention are as follows:
通过本发明方法制备所得的电子烟烟液微胶囊不仅具有浓郁的烟草香和杨梅的特征香气，同时增加了美拉德反应产物特征香韵，且保质期长、稳定性好，抽吸时烟雾量释放均匀稳定。另外，本发明反应条件温和，要求的设备相对简单，易于工业化生产。The electronic cigarette liquid microcapsules prepared by the method of the present invention not only have rich tobacco aroma and the characteristic aroma of bayberry, but also increase the characteristic aroma of the Maillard reaction product, and have a long shelf life, good stability, and low smoke volume during smoking. The release is even and stable. In addition, the reaction conditions of the present invention are mild, the required equipment is relatively simple, and it is easy for industrial production.
具体实施方式Detailed ways
以下结合实施例对本发明的技术方案作进一步地详细介绍，但本发明的保护范围并不局限于此。The technical solution of the present invention will be described in further detail below with reference to the examples, but the protection scope of the present invention is not limited thereto.
下述实施例中，所用原料均为可以直接购买到的普通市售产品、或者采用本领域常规方法制备获得。如，果胶酶和淀粉酶购买厂家为山东拢科特酶制剂有限公司，果胶酶活性为30000u/g，淀粉酶活性为50000 u/g；蛋白酶购买厂家为南宁庞博生物工程有限公司，蛋白酶活性为200000 u/g。In the following examples, the raw materials used are all common commercial products that can be purchased directly, or prepared by conventional methods in this field. For example, the purchasing manufacturer of pectinase and amylase is Shandong Pongke Enzyme Preparation Co., Ltd., the pectinase activity is 30000 u/g, and the amylase activity is 50000 u/g; the purchasing manufacturer of protease is Nanning Pangbo Bioengineering Co., Ltd. Protease activity is 200000 u/g.
实施例中，如无详细，涉及的操作或工艺采用本领域常规技术即可。In the embodiments, if there are no details, the operations or processes involved may adopt conventional techniques in the art.
实施例1Example 1
一种特征香型的电子烟烟液微胶囊制备方法，其具体包括以下步骤：A method for preparing characteristically fragrant electronic cigarette liquid microcapsules, which specifically includes the following steps:
1）在烟叶中加入果胶酶、蛋白酶、淀粉酶调制成的酶解溶液进行酶解反应，将酶解后的烟叶用水提取。其中果胶酶、蛋白酶、淀粉酶添加量分别为烟叶质量的0.2%、0.2%和0.5%。酶解温度为40℃，酶解时间6h。酶解后的烟叶中加入烟叶质量5倍的水提取，提取温度为50℃，提取时间1.5h；1) Add an enzymatic solution prepared by pectinase, protease and amylase to tobacco leaves to perform an enzymatic hydrolysis reaction, and extract the enzymatically hydrolyzed tobacco leaves with water. The addition amounts of pectinase, protease and amylase were 0.2%, 0.2% and 0.5% of the tobacco leaf mass respectively. The enzymatic hydrolysis temperature was 40°C and the enzymatic hydrolysis time was 6 hours. Add water 5 times the mass of the tobacco leaves to the enzymatically hydrolyzed tobacco leaves for extraction. The extraction temperature is 50°C and the extraction time is 1.5 hours;
2）将提取液离心和膜分离，其中膜分离采用碳化硅管式膜（浙江坚膜科技有限公司，型号JMtech-SICT-30-4-19-1016），孔径为1.0 μm；2) Centrifuge and membrane separate the extract. The membrane separation uses a silicon carbide tubular membrane (Zhejiang Jian Membrane Technology Co., Ltd., model JMtech-SICT-30-4-19-1016) with a pore size of 1.0 μm;
3）将提取液负压浓缩成烟草浸膏，把烟草浸膏、市售乙醇提取杨梅浸膏（购自郑州捷士化工有限公司）与还原糖、氨基酸、溶剂混合均匀，调节反应体系的pH值为7，补水至体系中水分含量为12%，搅拌均匀，控制体系反应温度为100℃，反应时间为1h，冷却后离心除杂，即得到美拉德反应物。其中，溶剂为丙二醇，还原糖为质量比3:1的葡萄糖、果糖两种。氨基酸为质量比1:2:2:2的脯氨酸、亮氨酸、苏氨酸、苯丙氨酸。烟草浸膏的质量份为20时，杨梅浸膏的质量份为20，还原糖的质量份为10，氨基酸的质量份为0.6、溶剂的质量份为18。调节反应体系的pH值采用的化合物是氨水；3) Concentrate the extract into tobacco extract under negative pressure, mix the tobacco extract, commercially available ethanol-extracted bayberry extract (purchased from Zhengzhou Jiesh Chemical Co., Ltd.) with reducing sugar, amino acids, and solvents, and adjust the pH of the reaction system. The value is 7. Add water until the moisture content in the system is 12%. Stir evenly. Control the reaction temperature of the system to 100°C and the reaction time to 1 hour. After cooling, centrifuge to remove impurities to obtain the Maillard reactant. Among them, the solvent is propylene glycol, and the reducing sugars are glucose and fructose with a mass ratio of 3:1. The amino acids are proline, leucine, threonine, and phenylalanine in a mass ratio of 1:2:2:2. When the mass parts of tobacco extract are 20, the mass parts of bayberry extract are 20, the mass parts of reducing sugar are 10, the mass parts of amino acids are 0.6, and the mass parts of solvent are 18. The compound used to adjust the pH value of the reaction system is ammonia;
4）将聚乙烯醇缓慢加入水中，加热到90℃搅拌溶解（聚乙烯醇溶液浓度约5%）后，缓慢加入美拉德反应物（聚乙烯醇溶液与美拉德反应物的质量比为1：10），对混合物进行高速分散，得到乳液微胶囊，喷雾干燥，即得到所需电子烟烟液微胶囊。4) Slowly add polyvinyl alcohol to water, heat to 90°C, stir and dissolve (polyvinyl alcohol solution concentration is about 5%), then slowly add Maillard reactant (the mass ratio of polyvinyl alcohol solution to Maillard reactant is 1:10), the mixture is dispersed at high speed to obtain emulsion microcapsules, and spray-dried to obtain the required e-cigarette liquid microcapsules.
对照样为烟液，具体制备过程为：前两步同实施例1，然后将提取液负压浓缩成烟草浸膏，把烟草浸膏、市售乙醇提取杨梅浸膏、丙二醇按质量份20:20:18混合均匀，即得到对照烟液。The control sample is smoke liquid. The specific preparation process is: the first two steps are the same as in Example 1, and then the extract is concentrated into tobacco extract under negative pressure. The tobacco extract, commercially available ethanol are extracted into bayberry extract, and propylene glycol is divided into 20 parts by mass: 20:18 Mix evenly to obtain the control smoke liquid.
称量电子烟烟液微胶囊，观察其质量随放置时间的变化，研究烟叶微胶囊的缓释性能。Weigh the e-cigarette liquid microcapsules, observe the changes in their quality with placement time, and study the sustained-release performance of the tobacco leaf microcapsules.
表1 烟液微胶囊随放置时间质量变化Table 1 Quality changes of tobacco liquid microcapsules with storage time
注：对照样等量的烟液（0.6400g）放置205天后完全挥发。Note: The same amount of smoke liquid (0.6400g) of the control sample will completely evaporate after being placed for 205 days.
由上述表1可以看出：本发明实施例1的烟液微胶囊放置240天后，烟液保留率为91.53%，而对照样等量的烟液放置205天后即挥发完全，可见烟液微胶囊比单独的烟液稳定性更好，保存时间更长。It can be seen from the above Table 1 that after the tobacco liquid microcapsules of Example 1 of the present invention were placed for 240 days, the tobacco liquid retention rate was 91.53%, while the same amount of tobacco liquid of the control sample evaporated completely after being placed for 205 days. It can be seen that the tobacco liquid microcapsules It has better stability and longer storage time than smoke liquid alone.
请专家评吸，感官质量评价设置项目及分值为：烟雾量10分，香气30分，协调10分，刺激性10分，杂气20分，余味20分，总分为100分，评吸结果如表2。Experts are invited to evaluate the inhalation. The sensory quality evaluation setting items and scores are: smoke volume 10 points, aroma 30 points, coordination 10 points, irritation 10 points, miscellaneous fumes 20 points, aftertaste 20 points, the total score is 100 points, evaluate the inhalation The results are shown in Table 2.
表2 感官质量评价Table 2 Sensory quality evaluation
由上述表2可以看出：本发明实施例1样品的香气、协调等感官质量得分均高于对照样，总分比对照样高5.5分。同时实施例1样品烟雾量释放更均匀稳定，还有浓郁典型的烟草香和杨梅特征香韵风格。It can be seen from the above Table 2 that the aroma, coordination and other sensory quality scores of the sample of Example 1 of the present invention are all higher than that of the control sample, and the total score is 5.5 points higher than the control sample. At the same time, the smoke amount of the sample of Example 1 is more uniform and stable, and it also has a rich and typical aroma of tobacco and bayberry.
实施例2Example 2
一种特征香型的电子烟烟液微胶囊制备方法，其具体包括以下步骤：A method for preparing characteristically fragrant electronic cigarette liquid microcapsules, which specifically includes the following steps:
1）在烟叶中加入果胶酶、蛋白酶、淀粉酶调制成的酶解溶液进行酶解反应，将酶解后的烟叶用水提取，然后负压浓缩成烟草浸膏。其中果胶酶、蛋白酶、淀粉酶添加量分别为烟叶质量的0.1%、0.3%和0.5%。酶解温度为45℃，酶解时间5h。酶解后的烟叶中加入烟叶质量6倍的水提取，提取温度为60℃，提取时间2.0h；1) Add an enzymatic solution prepared by pectinase, protease and amylase to tobacco leaves for enzymatic hydrolysis reaction, extract the enzymatically hydrolyzed tobacco leaves with water, and then concentrate them under negative pressure into tobacco extract. The addition amounts of pectinase, protease and amylase were 0.1%, 0.3% and 0.5% of the tobacco leaf mass respectively. The enzymatic hydrolysis temperature is 45°C and the enzymatic hydrolysis time is 5 hours. Add water 6 times the mass of the tobacco leaves to the enzymatically hydrolyzed tobacco leaves for extraction. The extraction temperature is 60°C and the extraction time is 2.0 hours;
2）将提取液离心和膜分离，其中膜分离采用碳化硅管式膜，孔径为0.5μm；2) Centrifuge the extract and separate it with a membrane. The membrane separation uses a silicon carbide tubular membrane with a pore size of 0.5 μm;
3）将提取液负压浓缩成烟草浸膏，把将烟草浸膏、市售乙醇提取杨梅浸膏与还原糖、氨基酸、溶剂混合均匀，调节反应体系的pH值为8，补水至体系中水分含量为12%，搅拌均匀，控制体系反应温度为95℃，反应时间为2h，冷却后离心除杂，即得到美拉德反应物。其中溶剂为丙二醇、甘油两种。还原糖为质量1:2的阿拉伯糖、葡萄糖。氨基酸为质量比2:1:1:2的脯氨酸、苏氨酸、丝氨酸、苯丙氨酸。烟草浸膏的质量份为20时，杨梅浸膏的质量份为20，还原糖的质量份为15，氨基酸的质量份为1.0、溶剂的质量份为20。调节反应体系的pH值采用的化合物是Na0H；3) Concentrate the extract into tobacco extract under negative pressure, mix the tobacco extract, commercially available ethanol-extracted bayberry extract with reducing sugar, amino acids, and solvents, adjust the pH value of the reaction system to 8, and add water to the system. The content is 12%, stir evenly, control the reaction temperature of the system to 95°C, and the reaction time to 2 hours. After cooling, centrifuge to remove impurities, and the Maillard reactant is obtained. The solvents are propylene glycol and glycerin. Reducing sugars are arabinose and glucose with a mass of 1:2. The amino acids are proline, threonine, serine, and phenylalanine in a mass ratio of 2:1:1:2. When the mass parts of tobacco extract are 20, the mass parts of bayberry extract are 20, the mass parts of reducing sugar are 15, the mass parts of amino acids are 1.0, and the mass parts of solvent are 20. The compound used to adjust the pH value of the reaction system is NaOH;
4）将环糊精缓慢加入水中，加热到60℃搅拌溶解（环糊精溶液浓度约2%）后，缓慢加入美拉德反应物（环糊精溶液与美拉德反应物的质量比为1：8），对混合物进行高速分散，得到乳液微胶囊，喷雾干燥得到所需电子烟烟液微胶囊。4) Slowly add cyclodextrin to water, heat to 60°C, stir and dissolve (the concentration of the cyclodextrin solution is about 2%), then slowly add the Maillard reactant (the mass ratio of the cyclodextrin solution to the Maillard reactant is 1:8), the mixture is dispersed at high speed to obtain emulsion microcapsules, and spray-dried to obtain the required e-cigarette liquid microcapsules.
实施例3Example 3
一种特征香型的电子烟烟液微胶囊制备方法，其具体包括以下步骤：A method for preparing characteristically fragrant electronic cigarette liquid microcapsules, which specifically includes the following steps:
1）在烟叶中加入果胶酶、蛋白酶、淀粉酶调制成的酶解溶液进行酶解反应，将酶解后的烟叶用水提取，然后负压浓缩成烟草浸膏。其中果胶酶、蛋白酶、淀粉酶添加量分别为烟叶质量的0.4%、0.4%和0.3%。酶解温度为50℃，酶解时间8h。酶解后的烟叶中加入烟叶质量8倍的水提取，提取温度为70℃，提取时间2.5h；1) Add an enzymatic solution prepared by pectinase, protease and amylase to tobacco leaves for enzymatic hydrolysis reaction, extract the enzymatically hydrolyzed tobacco leaves with water, and then concentrate them under negative pressure into tobacco extract. The added amounts of pectinase, protease and amylase were 0.4%, 0.4% and 0.3% of the tobacco leaf mass respectively. The enzymatic hydrolysis temperature was 50°C and the enzymatic hydrolysis time was 8 hours. After enzymatic hydrolysis, add water 8 times the mass of the tobacco leaves for extraction. The extraction temperature is 70°C and the extraction time is 2.5 hours;
2）将提取液离心和膜分离，其中膜分离采用碳化硅管式膜，孔径为0.5μm；2) Centrifuge the extract and separate it with a membrane. The membrane separation uses a silicon carbide tubular membrane with a pore size of 0.5 μm;
3）将提取液负压浓缩成烟草浸膏，把将烟草浸膏、市售乙醇提取杨梅浸膏与还原糖、氨基酸、溶剂混合均匀，调节反应体系的pH值为10，补水至体系中水分含量为12%，搅拌均匀，控制体系反应温度为120℃，反应时间为3h，冷却后离心除杂，即得到本发明的美拉德反应物。其中溶剂为甘油，还原糖为葡萄糖。氨基酸为质量比2:1:1:1的脯氨酸、亮氨酸、色氨酸、丝氨酸的混合物。烟草浸膏的质量份为20时，杨梅浸膏的质量份为25，还原糖的质量份为10，氨基酸的质量份为2.0、溶剂的质量份为18。调节反应体系的pH值采用的化合物是K0H；3) Concentrate the extract into tobacco extract under negative pressure, mix the tobacco extract, commercially available ethanol-extracted bayberry extract with reducing sugar, amino acids, and solvents, adjust the pH value of the reaction system to 10, and add water to the system. The content is 12%, stir evenly, control the reaction temperature of the system to 120°C, and the reaction time to 3 hours. After cooling, centrifuge to remove impurities to obtain the Maillard reactant of the present invention. The solvent is glycerol and the reducing sugar is glucose. The amino acid is a mixture of proline, leucine, tryptophan, and serine in a mass ratio of 2:1:1:1. When the mass parts of tobacco extract are 20, the mass parts of bayberry extract are 25, the mass parts of reducing sugar are 10, the mass parts of amino acids are 2.0, and the mass parts of solvent are 18. The compound used to adjust the pH value of the reaction system is KOH;
4）将聚乙烯醇缓慢加入水中，加热到90℃搅拌溶解（聚乙烯醇溶液浓度约4%）后，缓慢加入美拉德反应物（聚乙烯醇溶液与美拉德反应物的质量比为1：6），对混合物进行高速分散，得到乳液微胶囊，喷雾干燥，即得到所需电子烟烟液微胶囊。4) Slowly add polyvinyl alcohol to water, heat to 90°C, stir and dissolve (polyvinyl alcohol solution concentration is about 4%), then slowly add Maillard reactant (the mass ratio of polyvinyl alcohol solution to Maillard reactant is 1:6), the mixture is dispersed at high speed to obtain emulsion microcapsules, and spray-dried to obtain the required e-cigarette liquid microcapsules.
对实施例2、3的烟液微胶囊进行了相关的感官质量评价，其评析结果与实施例1相当。Relevant sensory quality evaluation was conducted on the smoke liquid microcapsules of Examples 2 and 3, and the evaluation results were equivalent to those of Example 1.
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何属于本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求的保护范围为准。The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed in the present invention. All are covered by the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
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| CN101204249A (en)* | 2007-12-11 | 2008-06-25 | 广东中烟工业公司 | A kind of preparation method of tobacco extract |
| CN105200857A (en)* | 2015-08-20 | 2015-12-30 | 嘉兴景程生物科技有限公司 | Fresh-scent cigarette paper and preparation method thereof |
| CN106433982A (en)* | 2016-09-21 | 2017-02-22 | 宝可科技（上海）有限公司 | Method for preparing fresh and sweet flavor essence from tobacco leaf stem threads |
| CN111013505A (en)* | 2019-12-25 | 2020-04-17 | 郑州轻工业大学 | A kind of slow-release flavor microcapsule for cigarette and preparation method thereof |
| CN114271467A (en)* | 2021-12-30 | 2022-04-05 | 广州百花香料股份有限公司 | A kind of preparation method of pandan leaf extract and prepared pandan leaf extract |
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| CN101204249A (en)* | 2007-12-11 | 2008-06-25 | 广东中烟工业公司 | A kind of preparation method of tobacco extract |
| CN105200857A (en)* | 2015-08-20 | 2015-12-30 | 嘉兴景程生物科技有限公司 | Fresh-scent cigarette paper and preparation method thereof |
| CN106433982A (en)* | 2016-09-21 | 2017-02-22 | 宝可科技（上海）有限公司 | Method for preparing fresh and sweet flavor essence from tobacco leaf stem threads |
| CN111013505A (en)* | 2019-12-25 | 2020-04-17 | 郑州轻工业大学 | A kind of slow-release flavor microcapsule for cigarette and preparation method thereof |
| CN114271467A (en)* | 2021-12-30 | 2022-04-05 | 广州百花香料股份有限公司 | A kind of preparation method of pandan leaf extract and prepared pandan leaf extract |
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