技术领域Technical Field
本发明属于香精香料技术领域，涉及一种咖啡香精及其制备方法与应用。The invention belongs to the technical field of flavors and fragrances, and relates to coffee flavor and a preparation method and application thereof.
背景技术Background Art
加热卷烟，主要是通过低温加热的工作原理，加热的主要对象是烟草薄片，通过温控技术精确加热薄片，达到刚好释放出烟草中所含的芳香物质和尼古丁的温度，形成烟气。能刚好加热烟叶到足以散发出味道的程度，而不会点燃烟叶。其口味最接近传统卷烟，有望首先被吸烟消费者接受。对比分析加热卷烟与传统卷烟的特征，感官差异的根本在于两者的受热温度不同，传统卷烟属于燃吸过程，致香物质来自于烟草本身含有的致香物质的转移及卷烟燃吸过程中复杂的热裂解反应，无论是香气物质的转移还是热裂解产香，其香气物质来源主要在烟支燃烧的热解/蒸馏区，其温度大约在250～600℃，而加热卷烟采取的是加热过程，非燃烧过程，加热温度一般不超过300℃，烟支内部温度更低，因此相对于传统卷烟，加热卷烟因温度达不到传统卷烟的产香温度，故香气丰富性显著不足，因而极有必要在现有增香方式基础上，进一步通过香精配方、增香方式改良等综合手段，获得适用于加热卷烟产品的香精。Heated cigarettes mainly work on the principle of low-temperature heating. The main object of heating is tobacco flakes. The flakes are precisely heated through temperature control technology to a temperature that just releases the aromatic substances and nicotine contained in the tobacco, forming smoke. It can heat the tobacco leaves just enough to emit flavor without igniting the tobacco leaves. Its taste is closest to traditional cigarettes and is expected to be accepted by smoking consumers first. Comparative analysis of the characteristics of heated cigarettes and traditional cigarettes shows that the fundamental reason for the sensory difference lies in the different heating temperatures of the two. Traditional cigarettes are a burning and smoking process, and the aroma substances come from the transfer of aroma substances contained in the tobacco itself and the complex thermal cracking reaction during the burning and smoking process of cigarettes. Whether it is the transfer of aroma substances or the production of aroma by thermal cracking, the source of aroma substances is mainly in the pyrolysis/distillation zone of the burning cigarette, and its temperature is about 250-600°C. Heated cigarettes adopt a heating process, not a combustion process, and the heating temperature generally does not exceed 300°C. The temperature inside the cigarette is lower. Therefore, compared with traditional cigarettes, heated cigarettes cannot reach the aroma production temperature of traditional cigarettes, so the aroma richness is significantly insufficient. Therefore, it is extremely necessary to further obtain flavors suitable for heated cigarette products through comprehensive means such as flavor formulation and improvement of flavor enhancement methods on the basis of existing flavor enhancement methods.
咖啡香深受人们喜爱，目前咖啡香精的制备方法主要是通过将咖啡提取物和不同香基进行调配得到咖啡香精，很大一部分是应用在饮料和食品中，如专利CN 106260372 A公开了一种咖啡香精，其组成为咖啡提取物、苯甲醇、糠基硫醇、乙偶姻、松油烯-4-醇、丁酸等15种化合物调配组成，可获得新鲜烘焙咖啡的风味的咖啡香精；专利CN 105062673 A公开的咖啡味香精包括赖氨酸、甲硫氨酸、苯丙氨酸、酪氨酸、果糖、葡萄糖以及溶剂等，得到的咖啡香精应用于雪茄烟，形成具有咖啡香的卷烟产品。以上技术中主要是将咖啡提取物和不同的单体进行调配获得，并非从源头咖啡豆制备而得，虽可以制备得到咖啡香精，但咖啡香气丰富性不够。Coffee aroma is very popular among people. At present, the preparation method of coffee flavor is mainly to prepare coffee flavor by mixing coffee extract and different aroma bases. A large part of it is used in beverages and foods. For example, patent CN 106260372 A discloses a coffee flavor, which is composed of 15 compounds such as coffee extract, benzyl alcohol, furfurylthiol, acetoin, terpinene-4-ol, butyric acid, etc., and can obtain coffee flavor with the flavor of freshly roasted coffee; patent CN 105062673 A discloses coffee flavor including lysine, methionine, phenylalanine, tyrosine, fructose, glucose and solvent, etc. The obtained coffee flavor is applied to cigars to form cigarette products with coffee aroma. The above technology mainly obtains coffee extract by mixing with different monomers, and is not prepared from the source coffee beans. Although coffee flavor can be prepared, the richness of coffee aroma is not enough.
发明内容Summary of the invention
针对现有技术咖啡香精及其制备方法存在的缺陷，本发明的第一个目的是提供一种咖啡香精的制备方法，该方法通过对咖啡粉进行烘培预处理以及分步提取，能够获得完美融合焦甜香、烘焙香及坚果香等特有香气，且香气浓郁，协调性好，杂气少和刺激性低的咖啡香精。In view of the defects of the prior art coffee flavor and its preparation method, the first object of the present invention is to provide a method for preparing coffee flavor. The method can obtain a coffee flavor that perfectly blends unique aromas such as caramelized sweet aroma, roasted aroma and nutty aroma, and has a strong aroma, good coordination, less impurities and low irritation by pretreating coffee powder by roasting and extracting it in steps.
本发明的第二个目的是在于提供一种完美融合焦甜香、烘焙香及坚果香等特有香气，且香气浓郁，协调性好，杂气少和刺激性低的咖啡香精，可以用于加热卷烟以降低烟气刺激，改善口感，并赋予其浓郁咖啡香和焦甜香等香味。The second object of the present invention is to provide a coffee essence which perfectly blends the unique aromas such as caramel sweet aroma, roasted aroma and nutty aroma, and has a strong aroma, good coordination, less impurities and low irritation. The coffee essence can be used to heat cigarettes to reduce smoke irritation, improve the taste, and give them strong coffee aroma and caramel sweet aroma.
本发明的第三个目的是在于提供一种咖啡香精的应用，将咖啡香精以加香的方式添加到加热卷烟烟草薄片中，可以赋予加热卷烟浓郁的咖啡和焦甜香，香气浓度高，烟香浓郁饱满，能够与烟草本香自然融合，应用效果良好。The third object of the present invention is to provide an application of coffee essence. The coffee essence is added to the tobacco slices of heated cigarettes in a flavoring manner, which can give the heated cigarettes a strong coffee and caramel sweet aroma, a high aroma concentration, a strong and full tobacco aroma, and can be naturally integrated with the original tobacco aroma, with a good application effect.
为了实现上述技术目的，本发明提供了一种咖啡香精的制备方法，包括以下步骤：In order to achieve the above technical objectives, the present invention provides a method for preparing coffee essence, comprising the following steps:
S1：将咖啡粉进行烘焙处理，得到烘焙咖啡粉；S1: roasting coffee powder to obtain roasted coffee powder;
S2：将烘焙咖啡粉采用乙醇提取，得到提取液和咖啡渣；S2: extracting roasted coffee powder with ethanol to obtain an extract and coffee grounds;
S3：将提取液进行浓缩1，所得浸膏用乙醇溶解后，依次进行冷冻、过滤和浓缩2，得到提取物1；S3: the extract is concentrated 1, the obtained extract is dissolved in ethanol, and then sequentially frozen, filtered and concentrated 2 to obtain an extract 1;
S4：将咖啡渣用水提取，所得提取液依次进行萃取、蒸干和稀释，得到提取物2；S4: extracting the coffee grounds with water, extracting, evaporating and diluting the obtained extract in sequence to obtain extract 2;
S5：将提取物1和提取物2混合，即得。S5: Mix extract 1 and extract 2 to obtain.
本发明提供的咖啡香精的制备方法关键是在于对咖啡粉进行烘焙处理，再利用不同极性的溶剂进行分步提取，并利用萃取和冷冻等分离手段进行精制除杂，最终得到同时融合了焦糖风味、烘焙风味及坚果味复合咖啡香精。烘焙过程中，使咖啡粉中丰富的化学成分发生焦糖化反应与美拉德反应，除了保持咖啡的特征香外，还产生了焦甜香、烘焙香和坚果香等致香物。再将经过烘焙后的咖啡进行分步提取，完全激发出咖啡粉中的特有香气，提升咖啡香精的香气丰富性。分步提取过程中先采用有机溶剂乙醇提取可以获得包括咖啡因、乙酸、吡啶醇、呋喃甲醇、十六酸、亚麻酸、吡啶、羟基丙酮、甲基吡啶醇、羟基丁酸、麦芽酚、5-羟甲基二氢呋喃酮等在内的致香物成分，这些化合物主要是具有焦糖和烘焙香，而采用水进一步提取获得包括咖啡因、呋喃甲醇、羟基丁酸、吡啶、甲基吡嗪、麦芽酚、二甲基吡嗪、乙氧基吡咯、乙基-甲基-吡嗪、吡咯甲醛等在内的致香物成分，这些化合物具有坚果香，而将两者复配融合形成焦糖风味、烘焙风味及坚果味复合咖啡香精。The key to the preparation method of the coffee flavor provided by the present invention is to roast the coffee powder, then use solvents of different polarities for step-by-step extraction, and use separation means such as extraction and freezing for refining and impurity removal, and finally obtain a composite coffee flavor that combines caramel flavor, roasted flavor and nutty flavor. During the roasting process, the rich chemical components in the coffee powder undergo caramelization reaction and Maillard reaction, and in addition to maintaining the characteristic aroma of coffee, aroma substances such as caramel sweet aroma, roasted aroma and nutty aroma are also produced. The roasted coffee is then extracted step by step to fully stimulate the unique aroma in the coffee powder and enhance the aroma richness of the coffee flavor. In the step-by-step extraction process, the organic solvent ethanol is first used for extraction to obtain aroma components including caffeine, acetic acid, pyridinol, furan methanol, hexadecanoic acid, linolenic acid, pyridine, hydroxyacetone, methylpyridinol, hydroxybutyric acid, maltol, 5-hydroxymethyldihydrofuranone, etc. These compounds mainly have caramel and baking aromas, and water is used for further extraction to obtain aroma components including caffeine, furan methanol, hydroxybutyric acid, pyridine, methylpyrazine, maltol, dimethylpyrazine, ethoxypyrrole, ethyl-methyl-pyrazine, pyrrolecarboxaldehyde, etc. These compounds have nutty aromas, and the two are compounded to form a caramel flavor, baking flavor and nutty flavor composite coffee flavor.
作为一个优选的方案，所述烘焙处理的条件为：温度为80～200℃，时间为20～60min。进一步优选烘焙温度为100～200℃。咖啡粉末烘焙过程中其中的化学成分会发生焦糖化反应与美拉德反应，在保持了咖啡特征香的基础上，还产生焦甜香和烘焙香。在加热烘培过程中，咖啡粉中的水分首先受热蒸发，随后发生还原糖与氨基酸的美拉德反应，随后各种多糖受热分解。生成大量的二氧化碳和风味物质，但若烘培加热温度过高会使风味物质挥发加快，并且会生成令人不愉悦和有害的酚类物质，从而达不到香气丰富的效果，并且会对加热卷烟口感产生负面效果。若烘培加热温度过低则会使咖啡粉的美拉德反应减慢，风味物质也不能有效生成。As a preferred solution, the conditions for the baking treatment are: a temperature of 80 to 200°C and a time of 20 to 60 minutes. The baking temperature is further preferably 100 to 200°C. During the baking process of coffee powder, the chemical components therein will undergo caramelization reaction and Maillard reaction, and on the basis of maintaining the characteristic aroma of coffee, a caramelized sweet aroma and a baking aroma will also be produced. During the heating and baking process, the water in the coffee powder is first evaporated by heat, and then the Maillard reaction of reducing sugar and amino acid occurs, and then various polysaccharides are decomposed by heat. A large amount of carbon dioxide and flavor substances are generated, but if the baking heating temperature is too high, the flavor substances will volatilize faster, and unpleasant and harmful phenolic substances will be generated, thereby failing to achieve the effect of rich aroma, and will have a negative effect on the taste of heated cigarettes. If the baking heating temperature is too low, the Maillard reaction of the coffee powder will be slowed down, and the flavor substances cannot be effectively generated.
作为一个优选的方案，所述乙醇提取的条件为：固液比为：1g:5～10mL，温度为30～80℃，时间为0.5～12h。本发明采用乙醇作为溶剂是基于，乙醇无毒且安全，它可以溶解出咖啡中大部分的化学物质，得到口感更好，香气更浓郁的提取物。且乙醇的沸点是78.3℃，提取温度为30～80℃，提取时间为0.5～12h，在此条件下可以保证乙醇回流，提高乙醇提取的效率，最大化地提取咖啡中有效香气物质。As a preferred solution, the conditions for ethanol extraction are: solid-liquid ratio: 1g:5-10mL, temperature of 30-80°C, and time of 0.5-12h. The present invention uses ethanol as a solvent because ethanol is non-toxic and safe, and it can dissolve most of the chemical substances in coffee to obtain an extract with better taste and richer aroma. The boiling point of ethanol is 78.3°C, the extraction temperature is 30-80°C, and the extraction time is 0.5-12h. Under these conditions, ethanol reflux can be guaranteed, the efficiency of ethanol extraction can be improved, and the effective aroma substances in coffee can be extracted to the maximum extent.
作为一个优选的方案，所述乙醇的浓度为75～95％。不同浓度的乙醇提取所得成分是存在差异的，本发明优选采用浓度为75～95％的乙醇进行提取。As a preferred solution, the concentration of ethanol is 75-95%. Different concentrations of ethanol extracts produce different components. In the present invention, ethanol with a concentration of 75-95% is preferably used for extraction.
作为一个优选的方案，所述冷冻的条件为：温度为-4℃～-8℃，时间为2～12h。在利用乙醇提取咖啡的过程中，不可避免的会将咖啡表面的蜡质提取到提取液中，而蜡质在乙醇中的溶解度较低，会影响所得提取物的产品质量，造成使用过程中有悬浮物、溶解性差等问题。另外这类含有蜡质的提取物使用时，会对卷烟的口感和香气造成不利影响，因而，需要快速、有效去除蜡质，提高天然香料的产品质量。目前，主要是通过乙醇回溶、低温冷冻的方式可以有效脱除植物蜡质，即提取物溶解后置于-4℃～-8℃低温沉降，从而使得植物蜡质与其它不溶物析出，然后过滤或离心去除，在此条件下放置足够长的时间，蜡质和大分子物质析出的比较充分，得到的咖啡提取物的品质较好。As a preferred solution, the freezing conditions are: temperature of -4°C to -8°C, time of 2 to 12h. In the process of extracting coffee with ethanol, it is inevitable to extract the wax on the surface of the coffee into the extract, and the solubility of the wax in ethanol is low, which will affect the product quality of the obtained extract, resulting in suspended matter and poor solubility during use. In addition, when this type of extract containing wax is used, it will have an adverse effect on the taste and aroma of cigarettes. Therefore, it is necessary to quickly and effectively remove the wax and improve the product quality of natural flavors. At present, the plant wax can be effectively removed mainly by ethanol re-dissolution and low-temperature freezing, that is, the extract is dissolved and placed at -4°C to -8°C for low-temperature precipitation, so that the plant wax and other insoluble substances are precipitated, and then filtered or centrifuged for removal. Under this condition, it is placed for a long enough time, and the wax and macromolecular substances are precipitated more fully, and the quality of the obtained coffee extract is better.
作为一个优选的方案，所述浓缩2至固含量为20％～30％。As a preferred solution, the concentration 2 is performed to a solid content of 20% to 30%.
作为一个优选的方案，所述水提取的条件为：固液比为1g:5～10mL，温度为室温，时间为20～40min。As a preferred solution, the conditions for water extraction are: solid-liquid ratio of 1 g: 5-10 mL, temperature of room temperature, and time of 20-40 min.
作为一个优选的方案，所述水提取采用超声辅助提取。As a preferred solution, the water extraction adopts ultrasound-assisted extraction.
作为一个优选的方案，所述萃取采用的有机相为乙酸乙酯和/或二氯甲烷，萃取有机相和水相体积比3～5:5～8。乙醇提取过的咖啡渣还有较多的香气组分，利用水对咖啡渣进行超声提取，可以将咖啡中的有效香气组分最大程度获得，但同时水提取物中还含有较多的糖类、蛋白质和纤维素等物质，这些大分子物质对卷烟抽吸会造成负面效果，因此需要用有机溶剂对水提取物进行萃取分离，其中乙酸乙酯和二氯甲烷可以将咖啡水提取物中的香气进行有效萃取，尤其是二氯甲烷可以将水提取物中大部分的挥发性香气物萃取完全，得到香气品质较高的咖啡提取物。As a preferred solution, the organic phase used in the extraction is ethyl acetate and/or dichloromethane, and the volume ratio of the extraction organic phase to the aqueous phase is 3-5:5-8. The coffee grounds extracted with ethanol still have more aroma components. Ultrasonic extraction of coffee grounds with water can obtain the effective aroma components in coffee to the greatest extent, but at the same time, the water extract also contains more sugars, proteins, cellulose and other substances. These macromolecular substances will have a negative effect on cigarette smoking. Therefore, it is necessary to extract and separate the water extract with an organic solvent, among which ethyl acetate and dichloromethane can effectively extract the aroma in the coffee water extract, especially dichloromethane can completely extract most of the volatile aroma substances in the water extract to obtain a coffee extract with higher aroma quality.
作为一个优选的方案，所述稀释至固含量为20％～30％。As a preferred solution, the dilution is performed to a solid content of 20% to 30%.
作为一个优选的方案，所述提取物1和提取物2混合的体积比为1:1～3。提取物1和提取物2包含完全不同风味的致香成分，按优选的比例范围内复合，能够达到最佳的卷烟应用效果。As a preferred solution, the volume ratio of the extract 1 and the extract 2 is 1:1 to 3. The extract 1 and the extract 2 contain aroma components with completely different flavors, and the combination within the preferred ratio range can achieve the best cigarette application effect.
本发明还提供了一种咖啡香精，能够降低烟气刺激，改善口感，具有浓郁的咖啡香和焦甜香的咖啡香精。The present invention also provides a coffee essence which can reduce smoke stimulation, improve taste and has a strong coffee aroma and a burnt sweet aroma.
本发明还提供了一种咖啡香精的应用，其应用于加热卷烟的制备，可以赋予加热卷烟浓郁的咖啡和焦甜香，香气浓度高，烟香浓郁饱满。The present invention also provides an application of coffee essence, which is applied to the preparation of heated cigarettes and can give the heated cigarettes a strong coffee and caramel sweet aroma, a high aroma concentration, and a strong and full tobacco aroma.
作为一个优选的方案，将所述咖啡香精采用丙二醇稀释1～2倍后添加至烟草薄片上。As a preferred solution, the coffee essence is diluted 1 to 2 times with propylene glycol and then added to the tobacco sheet.
与现有技术相比，本发明的技术方案带来的有益技术效果：Compared with the prior art, the technical solution of the present invention has the following beneficial technical effects:
1.本发明技术方案将咖啡粉末经过烘焙处理，咖啡会发生焦糖化反应与美拉德反应，产生大量风味物质，在保持咖啡特征香的基础上还产生焦甜香和烘焙香，再进一步对烘焙咖啡粉进行分步提取，不但能够最大化地获得烘焙咖啡中的致香物组分，而且可以将不同特征香味的致香物成分分类提取，再按适当比例完美复配融合，最终获得完美融合焦甜香、烘焙香及坚果香等特有香气，且香气浓郁，协调性好，杂气少和刺激性低的咖啡香精。1. The technical solution of the present invention is to subject coffee powder to roasting treatment, so that the coffee will undergo caramelization reaction and Maillard reaction, produce a large amount of flavor substances, and produce caramelized sweet aroma and roasted aroma on the basis of maintaining the characteristic aroma of coffee, and then further extract the roasted coffee powder in steps, which can not only maximize the acquisition of aroma components in roasted coffee, but also classify and extract aroma components of different characteristic aromas, and then perfectly compound and fuse them in appropriate proportions, and finally obtain a coffee flavor that perfectly blends unique aromas such as caramelized sweet aroma, roasted aroma and nutty aroma, and has a strong aroma, good coordination, less impurities and low irritation.
2.本发明技术方案将咖啡香精添加在加热卷烟的烟草薄片中，赋予了加热卷烟浓郁的咖啡香，且香气丰富，能够与烟草本香自然融合，应用效果良好。2. The technical solution of the present invention adds coffee flavor to the tobacco flakes of the heated cigarette, giving the heated cigarette a strong coffee aroma, and the aroma is rich, which can be naturally integrated with the original aroma of tobacco, and the application effect is good.
3.本发明技术方案提供的咖啡香精提取方法简单，成本低，有利于实现规模化生产。3. The coffee essence extraction method provided by the technical solution of the present invention is simple, low-cost, and is conducive to large-scale production.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
为了更清楚地说明本发明的技术方案，下面对实施例或对比例中所需要使用的附图作简单介绍。下述附图仅包含本发明阐述过程中涉及的一些实施例和对比例，对于本领域普通技术人员而言，在不付出创造性劳动的前提下，可以根据这些附图获得其他附图。In order to more clearly illustrate the technical solution of the present invention, the following briefly introduces the drawings required for use in the embodiments or comparative examples. The following drawings only include some embodiments and comparative examples involved in the process of explaining the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
图1是本发明实施例1～2和对比实施例1制备所得咖啡香精香气组分含量对比图。从结果可知，100℃咖啡粉末中含有的香气物质最多，并且含量最高。主要有羟基丙酮、吡啶、乙酰基吡嗪、乙酰甲基吡嗪、甲基吡啶醇、甲基吡嗪、甲酸糠醛、羟甲基糠醛、呋喃甲醇乙酸酯、吡咯甲醛、乙氧基吡咯、麦芽酚、5-甲基吡咯甲醛、二氢苯丙呋喃、吲哚、氨基喹啉、乙酸、糠醛、呋喃甲醇、乙氧基呋喃、5-甲基糠醛、羟基吡啶以及咖啡因等物质。Fig. 1 is a comparison chart of the aroma component contents of coffee essences prepared in Examples 1 to 2 of the present invention and Comparative Example 1. It can be seen from the results that the 100°C coffee powder contains the most aroma substances and the highest content. The main substances are hydroxyacetone, pyridine, acetylpyrazine, acetylmethylpyrazine, methylpyridinol, methylpyrazine, formic acid furfural, hydroxymethylfurfural, furan methanol acetate, pyrrole carboxaldehyde, ethoxypyrrole, maltol, 5-methylpyrrole carboxaldehyde, dihydrobenzofuran, indole, aminoquinoline, acetic acid, furfural, furan methanol, ethoxyfuran, 5-methylfurfural, hydroxypyridine and caffeine.
其中乙酰基吡嗪、乙酰甲基吡嗪、甲基吡啶醇都是在咖啡加热过程中产生的香气物质。羟甲基糠醛、甲酸糠醛、麦芽酚、二氢苯丙呋喃、糠醛、呋喃甲醇、乙氧基呋喃、5-甲基糠醛等具有烘焙香的香气物质在100℃咖啡提取物中含量最高，表明100～200℃的加热对产生特征香气组分有重要作用，是该工艺过程中最重要的前处理手段。Among them, acetylpyrazine, acetylmethylpyrazine and methylpyridinol are all aroma substances produced during the heating process of coffee. Hydroxymethylfurfural, formic acid furfural, maltol, dihydrobenzofuran, furfural, furfural methanol, ethoxyfuran, 5-methylfurfural and other aroma substances with baking aroma have the highest content in 100℃ coffee extract, indicating that heating at 100-200℃ plays an important role in producing characteristic aroma components and is the most important pretreatment method in this process.
具体实施方式DETAILED DESCRIPTION
以下实施例仅就本发明的优选实施方案进行具体描述，并非对本发明的实施范围进行限定，对于技术领域的普通技术人员，在不脱离本发明的前提下，所作出的改进应当视为本发明的保护范围内。The following examples are only specific descriptions of the preferred embodiments of the present invention, and are not intended to limit the scope of implementation of the present invention. For ordinary technicians in the technical field, any improvements made without departing from the present invention should be deemed to be within the scope of protection of the present invention.
实施例1Example 1
本实施例咖啡香精的制备方法由以下步骤组成：The preparation method of coffee essence in this embodiment consists of the following steps:
S1、称取100g咖啡粉在100℃下加热40min，取50g加热后冷却的咖啡粉加入500mL95％的乙醇在60℃下回流提取3h，过滤，得到提取液和咖啡渣；S1. Weigh 100 g of coffee powder and heat it at 100° C. for 40 min. Take 50 g of the heated and cooled coffee powder and add 500 mL of 95% ethanol to reflux extract at 60° C. for 3 h. Filter to obtain an extract and coffee grounds.
S2、将提取液第一次浓缩至干，加入40mL乙醇溶解浸膏，在-4℃下放置2h冷冻析出沉淀，过滤，第二次滤液浓缩至10mL，固含量为20％，得提取物1；S2, the extract was concentrated to dryness for the first time, 40 mL of ethanol was added to dissolve the extract, and the extract was placed at -4 ° C for 2 h to freeze and precipitate, and filtered. The filtrate was concentrated to 10 mL for the second time, and the solid content was 20%, and the extract 1 was obtained;
S3、将步骤S1所得咖啡渣用500mL水混合超声提取30min，过滤，将滤液用300mL的二氯甲烷萃取，二氯甲烷相在30℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, the coffee grounds obtained in step S1 were mixed with 500 mL of water and subjected to ultrasonic extraction for 30 min, filtered, and the filtrate was extracted with 300 mL of dichloromethane. The dichloromethane phase was concentrated under reduced pressure and evaporated to dryness at 30° C., and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取2mL提取物1和2mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 2 mL of extract 1 and 2 mL of extract 2 respectively, mix them, and dilute them 1 time with propylene glycol to obtain coffee essence.
实施例2Example 2
本实施例咖啡香精的制备方法由以下步骤组成：The preparation method of coffee essence in this embodiment consists of the following steps:
S1、称取200g咖啡粉在200℃下加热40min，取50g加热后冷却的咖啡粉加入500mL95％的乙醇在60℃下回流提取3h，过滤，得到提取液和咖啡渣；S1. Weigh 200 g of coffee powder and heat it at 200° C. for 40 min. Take 50 g of the heated and cooled coffee powder and add 500 mL of 95% ethanol to reflux extract at 60° C. for 3 h. Filter to obtain an extract and coffee grounds.
S2、将提取液浓缩至干，加入50mL乙醇溶解浸膏，在-4℃下放置2h冷冻析出沉淀，过滤，第二次浓缩至10mL，固含量为25％，得提取物1；S2, concentrate the extract to dryness, add 50 mL of ethanol to dissolve the extract, freeze it at -4 ° C for 2 h to precipitate the precipitate, filter it, and concentrate it to 10 mL for the second time, with a solid content of 25%, to obtain extract 1;
S3、将步骤S1所得咖啡渣用800mL水混合后超声提取30min，过滤，将滤液用500mL的乙酸乙酯萃取，乙酸乙酯相在40℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, the coffee grounds obtained in step S1 were mixed with 800 mL of water and subjected to ultrasonic extraction for 30 min, filtered, and the filtrate was extracted with 500 mL of ethyl acetate. The ethyl acetate phase was concentrated under reduced pressure and evaporated to dryness at 40° C., and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取2mL提取物1和4mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 2 mL of extract 1 and 4 mL of extract 2, mix them, and dilute them by 1 time with propylene glycol to obtain coffee essence.
实施例3Example 3
本实施例咖啡香精的制备方法由以下步骤组成：The preparation method of coffee essence in this embodiment consists of the following steps:
S1、称取100g咖啡粉在120℃下加热50min，取50g加热后冷却的咖啡粉加入500mL95％的乙醇在70℃下回流提取3h，过滤，得到提取液和咖啡渣；S1. Weigh 100 g of coffee powder and heat it at 120° C. for 50 min. Take 50 g of the heated and cooled coffee powder and add 500 mL of 95% ethanol to reflux extract at 70° C. for 3 h. Filter to obtain an extract and coffee grounds.
S2、将提取液浓缩至干，加入40mL乙醇溶解浸膏，在-4℃下放置2h冷冻析出沉淀，过滤，滤液浓缩至10mL，固含量为20％，得提取物1；S2, concentrate the extract to dryness, add 40 mL of ethanol to dissolve the extract, freeze it at -4 ° C for 2 h to precipitate the precipitate, filter it, and concentrate the filtrate to 10 mL with a solid content of 20%, to obtain extract 1;
S3、将步骤S1所得咖啡渣用500mL水混合后超声提取30min，过滤，将滤液用300mL的二氯甲烷萃取，二氯甲烷相在30℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, the coffee grounds obtained in step S1 were mixed with 500 mL of water and subjected to ultrasonic extraction for 30 min, filtered, and the filtrate was extracted with 300 mL of dichloromethane. The dichloromethane phase was concentrated under reduced pressure at 30° C. and evaporated to dryness, and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取2mL提取物1和4mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 2 mL of extract 1 and 4 mL of extract 2, mix them, and dilute them by 1 time with propylene glycol to obtain coffee essence.
实施例4Example 4
本实施例咖啡香精的制备方法由以下步骤组成：The preparation method of coffee essence in this embodiment consists of the following steps:
S1、称取100g咖啡粉在180℃下加热60min，取50g加热后冷却的咖啡粉加入500mL95％的乙醇在60℃下回流提取2h，过滤，得到提取液和咖啡渣；S1. Weigh 100 g of coffee powder and heat it at 180° C. for 60 min. Take 50 g of the heated and cooled coffee powder and add 500 mL of 95% ethanol to reflux extract at 60° C. for 2 h. Filter to obtain an extract and coffee grounds.
S2、将提取液浓缩至干，加入80mL乙醇溶解浸膏，在-4℃下放置2h冷冻析出沉淀，过滤，滤液浓缩至10mL，固含量为20％，得提取物1；S2, the extract was concentrated to dryness, 80 mL of ethanol was added to dissolve the extract, and the extract was placed at -4°C for 2 h to freeze and precipitate, and the filtrate was concentrated to 10 mL with a solid content of 20%, thereby obtaining extract 1;
S3、将步骤S1所得咖啡渣用500mL水混合后超声提取30min，过滤，将滤液用300mL的二氯甲烷萃取，二氯甲烷相在30℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, the coffee grounds obtained in step S1 were mixed with 500 mL of water and subjected to ultrasonic extraction for 30 min, filtered, and the filtrate was extracted with 300 mL of dichloromethane. The dichloromethane phase was concentrated under reduced pressure at 30° C. and evaporated to dryness, and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取1mL提取物1和1mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 1 mL of extract 1 and 1 mL of extract 2, mix them, and dilute them by 1 time with propylene glycol to obtain coffee essence.
对比实施例1Comparative Example 1
本对比实施例咖啡香精的制备过程中对咖啡粉不进行加热烘培处理，其制备方法由以下步骤组成：In the preparation process of the coffee essence of this comparative example, the coffee powder is not subjected to heating and baking treatment, and the preparation method thereof comprises the following steps:
S1、取80g咖啡粉加入800mL75％的乙醇在60℃下回流提取3h，过滤，得到提取液和咖啡渣；S1. Take 80g of coffee powder, add 800mL of 75% ethanol, reflux and extract at 60°C for 3h, filter and obtain an extract and coffee grounds;
S2、将提取液第一次浓缩至干，加入60mL乙醇溶解浸膏，在-4℃下放置2h冷冻析出沉淀，过滤，第二次滤液浓缩至10mL，固含量为20％，得提取物1；S2, the extract was concentrated to dryness for the first time, 60 mL of ethanol was added to dissolve the extract, and the extract was placed at -4 ° C for 2 h to freeze and precipitate, and filtered. The filtrate was concentrated to 10 mL for the second time, and the solid content was 20%, and the extract 1 was obtained;
S3、将步骤S1所得咖啡渣用800mL水混合后进行水超声提取30min，过滤，将滤液用500mL的二氯甲烷萃取，二氯甲烷相在40℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, mixing the coffee grounds obtained in step S1 with 800 mL of water, and then performing water ultrasonic extraction for 30 min, filtering, and extracting the filtrate with 500 mL of dichloromethane, the dichloromethane phase was concentrated under reduced pressure at 40° C. and evaporated to dryness, and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取5mL提取物1和8mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 5 mL of extract 1 and 8 mL of extract 2, mix them respectively, and dilute them 1 time with propylene glycol to obtain coffee essence.
对比实施例2Comparative Example 2
本对比实施例咖啡香精的制备过程中对咖啡粉不进行加热烘培处理，其制备方法由以下步骤组成：In the preparation process of the coffee essence of this comparative example, the coffee powder is not subjected to heating and baking treatment, and the preparation method thereof comprises the following steps:
S1、取80g咖啡粉加入800mL75％的乙醇在60℃下回流提取3h，过滤，得到提取液和咖啡渣；S1. Take 80g of coffee powder, add 800mL of 75% ethanol, reflux and extract at 60°C for 3h, filter and obtain an extract and coffee grounds;
S2、将提取液浓缩至10mL，固含量为20％，得提取物1；S2, concentrating the extract to 10 mL with a solid content of 20%, to obtain extract 1;
S3、将步骤S1所得咖啡渣用800mL水混合后进行水超声提取30min，过滤，将滤液用500mL的二氯甲烷萃取，二氯甲烷相在40℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, mixing the coffee grounds obtained in step S1 with 800 mL of water, and then performing water ultrasonic extraction for 30 min, filtering, and extracting the filtrate with 500 mL of dichloromethane, the dichloromethane phase was concentrated under reduced pressure at 40° C. and evaporated to dryness, and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取5mL提取物1和8mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 5 mL of extract 1 and 8 mL of extract 2, mix them respectively, and dilute them 1 time with propylene glycol to obtain coffee essence.
对比实施例3Comparative Example 3
本对比实施例咖啡香精的制备过程中对咖啡粉在300℃加热烘培40min，其制备方法由以下步骤组成：In the preparation process of the coffee essence of this comparative example, the coffee powder is heated and roasted at 300° C. for 40 minutes. The preparation method thereof consists of the following steps:
S1、取80g咖啡粉加入800mL75％的乙醇在60℃下回流提取3h，过滤，得到提取液和咖啡渣；S1. Take 80g of coffee powder, add 800mL of 75% ethanol, reflux and extract at 60°C for 3h, filter and obtain an extract and coffee grounds;
S2、将提取液浓缩至干，加入60mL乙醇溶解浸膏，在-4℃下放置2h冷冻析出沉淀，过滤，滤液浓缩至10mL，固含量为20％，得提取物1；S2, concentrate the extract to dryness, add 60 mL of ethanol to dissolve the extract, place it at -4 ° C for 2 hours to freeze and precipitate, filter, and concentrate the filtrate to 10 mL with a solid content of 20%, to obtain extract 1;
S3、将步骤S1所得咖啡渣用800mL水混合后进行水超声提取30min，过滤，将滤液用500mL的二氯甲烷萃取，二氯甲烷相在40℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, mixing the coffee grounds obtained in step S1 with 800 mL of water, and then performing water ultrasonic extraction for 30 min, filtering, and extracting the filtrate with 500 mL of dichloromethane, the dichloromethane phase was concentrated under reduced pressure at 40° C. and evaporated to dryness, and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取5mL提取物1和8mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 5 mL of extract 1 and 8 mL of extract 2, mix them respectively, and dilute them 1 time with propylene glycol to obtain coffee essence.
对比实施例4Comparative Example 4
本对比实施例咖啡香精的制备过程中对咖啡粉在50℃加热烘培60min，其制备方法由以下步骤组成：In the preparation process of the coffee essence of this comparative example, the coffee powder is heated and roasted at 50° C. for 60 minutes. The preparation method thereof consists of the following steps:
S1、取80g咖啡粉加入800mL75％的乙醇在60℃下回流提取3h，过滤，得到提取液和咖啡渣；S1. Take 80g of coffee powder, add 800mL of 75% ethanol, reflux and extract at 60°C for 3h, filter and obtain an extract and coffee grounds;
S2、将提取液浓缩至干，加入60mL乙醇溶解浸膏，在-4℃下放置2h冷冻析出沉淀，过滤，滤液浓缩至10mL，固含量为20％，得提取物1；S2, concentrate the extract to dryness, add 60 mL of ethanol to dissolve the extract, place it at -4 ° C for 2 hours to freeze and precipitate, filter, and concentrate the filtrate to 10 mL with a solid content of 20%, to obtain extract 1;
S3、将步骤S1所得咖啡渣用800mL水混合后进行水超声提取30min，过滤，将滤液用500mL的二氯甲烷萃取，二氯甲烷相在40℃下减压浓缩蒸干后用10mL95％乙醇稀释至固含量为20％，得提取物2；S3, mixing the coffee grounds obtained in step S1 with 800 mL of water, and then performing water ultrasonic extraction for 30 min, filtering, and extracting the filtrate with 500 mL of dichloromethane, the dichloromethane phase was concentrated under reduced pressure at 40° C. and evaporated to dryness, and then diluted with 10 mL of 95% ethanol to a solid content of 20%, to obtain extract 2;
S4、分别取5mL提取物1和8mL提取物2混合，用丙二醇稀释1倍，即得咖啡香精。S4. Take 5 mL of extract 1 and 8 mL of extract 2, mix them respectively, and dilute them 1 time with propylene glycol to obtain coffee essence.
对比实施例5Comparative Example 5
本对比例与实施例1的区别仅在于提取物1和提取物2的体积比为1:4，其余条件一致。The difference between this comparative example and Example 1 is that the volume ratio of extract 1 to extract 2 is 1:4, and the other conditions are the same.
对比实施例6Comparative Example 6
本对比例与实施例1的区别仅在于提取物1和提取物2的体积比为2:1，其余条件一致。The difference between this comparative example and Example 1 is that the volume ratio of extract 1 to extract 2 is 2:1, and the other conditions are the same.
将实施例1～2和对比实施例1所得咖啡香精进行香气组分测定，利用SPME-GC-MS进行分析，结果如图1。如图所示，本发明制备的咖啡香精含有的香气成分和含量都明显高于对比实施例1，说明通过将咖啡豆预加热的步骤可以充分激发咖啡的香气。The coffee essences obtained in Examples 1 to 2 and Comparative Example 1 were subjected to aroma component determination and analyzed by SPME-GC-MS, and the results are shown in Figure 1. As shown in the figure, the aroma components and contents contained in the coffee essence prepared by the present invention are significantly higher than those in Comparative Example 1, indicating that the aroma of coffee can be fully stimulated by preheating the coffee beans.
应用实施例Application Examples
将实施例1～4和对比实施例1～6得到的咖啡香精以加香的方式添加到加热卷烟配方薄片上，添加量为0.2％，赋予加热卷烟有一定的咖啡香。进行感官评价，参照GB5604.4—2005《卷烟第4部分：感官技术要求》，组织人员进行评吸，评吸人数为8人。分别依照香气、谐调、杂气、刺激性、余味5项指标对咖啡加热前后提取物在加热卷烟中的感官质量进行评价，评吸结果见表1。The coffee essence obtained in Examples 1 to 4 and Comparative Examples 1 to 6 was added to the heated cigarette formula sheet in an aroma-adding manner, with an addition amount of 0.2%, giving the heated cigarette a certain coffee aroma. Sensory evaluation was conducted, and personnel were organized to conduct smoking evaluation with reference to GB5604.4-2005 "Cigarette Part 4: Sensory Technical Requirements", with 8 people conducting the evaluation. The sensory quality of the coffee extract in the heated cigarette before and after heating was evaluated according to the five indicators of aroma, harmony, miscellaneous gas, irritation, and aftertaste, and the evaluation results are shown in Table 1.
表1实施例1～4和对比实施例1～6得到的咖啡香精评吸结果Table 1 The results of coffee flavor evaluation obtained in Examples 1 to 4 and Comparative Examples 1 to 6
从表中可以看出，10款提取物综合评价由高到低为实施例1＞实施例3＞对比实施例5＞对比实施例6＞实施例4＞实施例2＞对比实施例4＞对比实施例1＞对比实施例2＞对比实施例3，表明加热后咖啡提取物在香气和整体质量上有一定的提升，能够增加丰富烟香，提高香气质量，同时通过乙醇可以有效溶解出咖啡中大部分的化学物质，得到口感更好，香气更浓郁的提取物。其中100℃加热咖啡提取物在上述指标中表现更为明显，能够降低烟气刺激，改善口感，赋予加热卷烟浓郁的咖啡香和焦甜香、香气浓度高，烟香浓郁饱满。另外将提取物进行冷冻进行精制分离，可以有效去除提取物中的蜡质和大分子物质，有效提升提取物的香气品质，提升加热卷烟感官质量。As can be seen from the table, the comprehensive evaluation of the 10 extracts is from high to low as follows: Example 1 > Example 3 > Comparative Example 5 > Comparative Example 6 > Example 4 > Example 2 > Comparative Example 4 > Comparative Example 1 > Comparative Example 2 > Comparative Example 3, indicating that the coffee extract has a certain improvement in aroma and overall quality after heating, can increase the richness of the tobacco aroma, improve the aroma quality, and at the same time, most of the chemical substances in the coffee can be effectively dissolved by ethanol to obtain an extract with better taste and richer aroma. Among them, the coffee extract heated at 100°C performs more significantly in the above indicators, can reduce smoke irritation, improve taste, and give the heated cigarettes a rich coffee aroma and caramel sweet aroma, high aroma concentration, and rich and full tobacco aroma. In addition, freezing the extract for refined separation can effectively remove wax and macromolecular substances in the extract, effectively improve the aroma quality of the extract, and improve the sensory quality of heated cigarettes.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310437141.9ACN118834727A (en) | 2023-04-23 | 2023-04-23 | Coffee essence and preparation method and application thereof |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310437141.9ACN118834727A (en) | 2023-04-23 | 2023-04-23 | Coffee essence and preparation method and application thereof |
| Publication Number | Publication Date |
|---|---|
| CN118834727Atrue CN118834727A (en) | 2024-10-25 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310437141.9APendingCN118834727A (en) | 2023-04-23 | 2023-04-23 | Coffee essence and preparation method and application thereof |
| Country | Link |
|---|---|
| CN (1) | CN118834727A (en) |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119592371A (en)* | 2024-12-03 | 2025-03-11 | 茂名华美实业有限公司 | Essence containing coffee and cocoa composite extract and preparation method thereof |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN119592371A (en)* | 2024-12-03 | 2025-03-11 | 茂名华美实业有限公司 | Essence containing coffee and cocoa composite extract and preparation method thereof |
| Publication | Publication Date | Title |
|---|---|---|
| CN108464528B (en) | Tobacco-flavored electronic cigarette tobacco tar and preparation method thereof | |
| CN101497845B (en) | Method for producing cigarette flavor by maillard reaction with red date extract as raw material | |
| CN105105321B (en) | A kind of electronic cigarette tobacco extract and electronic cigarette liquid without sweet sense | |
| CN105011355B (en) | A kind of essential oil of tobaccos and extracting method thereof and application | |
| CN104403794A (en) | Preparation method and application of Pu'er tea extract to cigarettes | |
| CN105533793B (en) | A kind of preparation method of Dark sun-cured tobacco extract | |
| CN111528518B (en) | Low-nicotine tobacco extract, preparation method thereof and special tobacco tar for cigarette without burning under heating | |
| CN115399498B (en) | Tobacco extract, preparation method thereof and tobacco product | |
| CN102907760A (en) | Method for regulating chemical components of tobacco material | |
| CN109938396B (en) | Preparation method of tobacco endogenous Maillard reaction spice and application of tobacco endogenous Maillard reaction spice in novel tobacco products | |
| CN109090702A (en) | The preparation method and applications of Luo Han Guo Paste In Foods maillard reaction product | |
| CN108504454A (en) | A kind of modified form cigarette preparation method of liquor tailing fragrance and its application in cigarette | |
| CN118834727A (en) | Coffee essence and preparation method and application thereof | |
| CN107502449A (en) | A kind of preparation method and application of rhamnoides extract Maillard reaction type tobacco aromaticss | |
| CN110846133A (en) | A kind of caramel flavor for cigarette under negative pressure condition and preparation method thereof | |
| CN109251793B (en) | Essence for improving oral comfort of cigarette subjected to heating and non-combustion as well as preparation method and application of essence | |
| CN115505458B (en) | Tobacco essence with strong fragrance style | |
| CN105062675A (en) | Preparation method of beta vulgaris Maillard reactant for tobacco | |
| CN105686068B (en) | An e-liquid in the style of Burley tobacco | |
| CN114525173A (en) | A kind of licorice compound spice and preparation method and application thereof | |
| CN108179061A (en) | A kind of longan essence, preparation method and the application in cigarette | |
| CN113826942B (en) | Preparation method of sun-cured tobacco extract with sweet characteristic and processing method of sun-cured tobacco | |
| CN115005486B (en) | Method for thermochemically and hierarchically extracting nicotine and flavor substances in tobacco | |
| CN116286186A (en) | A jujube scorched-sweet spice that reduces harmful components burned and absorbed, and its preparation method and application | |
| CN109700068B (en) | Method for preparing sun-cured tobacco absolute oil by oil bleaching method and application thereof |
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |