CN101570717B - Method for preparing tobacco extract and application thereof - Google Patents
Method for preparing tobacco extract and application thereof Download PDFInfo
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- CN101570717B CN101570717B CN2009100274000A CN200910027400A CN101570717B CN 101570717 B CN101570717 B CN 101570717B CN 2009100274000 A CN2009100274000 A CN 2009100274000A CN 200910027400 A CN200910027400 A CN 200910027400A CN 101570717 B CN101570717 B CN 101570717B
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Abstract
The invention relates to a method for preparing tobacco extract and application thereof. The method for preparing the tobacco extract uses tobacco as a raw material to prepare the tobacco extract through the steps of enzymolysis, ultrasonic extraction, filtration, chromatography column separation and concentration under reduced pressure; and the tobacco extract is dissolved by 80 percent ethanol and sprayed into tobacco shreds by adopting an atomizing mode. The method using enzymolysis technology and ultrasonic extraction and combining the chromatography separation has the advantages of low extraction temperature, short time, little using amount of a solvent, full extraction and high raw material utilization rate; because the extraction temperature is low, the damage to thermal-sensitive fragrant substances is reduced, fragrant components of the tobacco self is furthest kept, and simultaneously the substances influencing the taste and mouthfeel are removed; and the method is simple, the equipment is easy to operate, and no pollution is produced.
Description
Technical field
The invention belongs to the Phytochemistry technical field, specifically relate to a kind of preparation method and application thereof of tobacco extract.
Background technology
Smoking and health problem are paid close attention to by the whole world, and the burst size that reduces the cigarette smoke harmful components is the tobacco business inescapable responsibility.Along with the gradually increase of people to smoking and health problem attention rate, tobacco industry has been implemented the reducing tar and reducing harm engineering in recent years, with continuous adaptation social requirement, and along with the continuous reduction of tar content in the cigarette, fragrance component in the tobacco also reduces accordingly, need compensate low-coke tar cigarette fragrance, obviously, extracting from tobacco that fragrance material effectively compensates low-coke tar cigarette fragrance is an important channel.Tobacco extract extracting method one class that present China tobacco business generally uses is to adopt the usual vehicle extraction to obtain product, another kind of is the product that utilizes steam distillation and a small amount of supercritical carbon dioxide extracting to obtain, though the product of these method preparations can remedy cigarette perfume (or spice) preferably, but because the composition that extracts is not had Selective Separation, wherein contain the material that some are unsuitable for cigarette odor-absorbing, when increasing cigarette perfume (or spice), also cause inhaling side effects such as uncomfortable, thick poor sense of flavor and dry sensation increase, caused cigarette quality to descend.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, provide a kind of extraction temperature low, the time is short, and solvent load is few, extracts thoroughly the preparation method of the tobacco extract that raw material availability is high and application thereof.
Purpose of the present invention realizes that by following technical scheme a kind of preparation method of tobacco extract is a raw material with the tobacco, makes tobacco extract through enzymolysis, ultrasonic wave extraction, filtration, chromatographic column separation, decompression concentration step, and the detailed process step is as follows:
(1) enzymolysis: having stirring and adding in the ultrasonic wave extractor of cover water-bath heater, the deionized water that adds offal, 4～8 times of offal quality, add citric acid, adjustment system pH value is between 3.0～6.0, add cellulase, enzymolysis is 8～12 hours under 40～50 ℃ condition, stirs 10 minutes every 30 minutes when enzymolysis;
(2) ultrasonic wave extracts: after enzymolysis is finished, the deionized water that adds 4～8 times of offal quality once more extracted 30～60 minutes with ultrasonic wave under 50～60 ℃ condition, collected extract for the first time, residue partly adopts identical method to extract once more, collects extract for the second time;
(3) centrifugal filtration: above-mentioned extracted twice liquid is merged, at room temperature pass through centrifuge centrifugation 20 minutes under 1500～1800 rev/mins condition, obtain clarifying extract;
(4) chromatographic column separates: the chromatographic column that cleans up on the clarification extract after the centrifugation is adsorbed, per minute absorption 10L extract, in adsorption process, extract liquid level and can not be lower than the chromatographic column upper end, control extract face is higher than 3 centimetres of chromatographic column upper ends when absorption finishes; Be that 95% ethanol carries out wash-out with concentration then, the ethanol flow is 5L/min, when outflow liquid has color and tangible tobacco aroma is arranged, begins to collect outflow liquid;
(5) decompression concentrates: the outflow liquid that will collect is 55～65 ℃ in temperature, vacuum is concentration under the condition of 0.085～0.095Mpa, obtain density and be 0.8875～0.8986 concentrate, promptly get tobacco extract, it is a light yellow transparent liquid, and main component is damascenone, damascone, solanone, geranyl acetone, farnesyl acetone, Megastigmatrienone, neophytadiene etc.
Take by weighing extract by 0.01～0.05% of cigarette shreds quality, with concentration is 80% ethanol dissolving extract, adopt the atomizing type spray to be added in the pipe tobacco, be rolled into cigarette, think that through smokeing panel test this product perfuming in cigarette is obvious: can significantly increase cigarette flavor matter and perfume quantity, make plentiful, saturating of cigarette flavor, cover assorted gas, improve the cigarette product quality.
The present invention compares with traditional extraction process, advantage is: use zymolysis technique and ultrasonic wave to extract, in conjunction with chromatography, it is low to extract temperature, time is short, solvent load is few, extracts thoroughly the raw material availability height, because it is low to extract temperature, reduced destruction, kept the aroma component of tobacco self to greatest extent, removed simultaneously inhaling flavor, the influential material of mouthfeel to the thermal sensitivity flavor matter; The inoperation of method simple device is easy, and is pollution-free.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
(1) enzymolysis: having stirring and adding in the ultrasonic wave extractor of cover water-bath heater, add offal 1000g, deionized water 5000g, add citric acid, adjustment system pH value is 4.5, add cellulase, enzymolysis is 12 hours under 43 ℃ condition, stirs 10 minutes every 30 minutes when enzymolysis;
(2) ultrasonic wave extracts: after enzymolysis is finished, add deionized water 7000g once more, extracted 60 minutes with ultrasonic wave under 50 ℃ condition, collect extract for the first time, residue partly adopts identical method to extract once more, collects extract for the second time;
(3) centrifugal filtration: above-mentioned extracted twice liquid is merged, at room temperature pass through centrifuge centrifugation 20 minutes under 1600 rev/mins condition, obtain clarifying extract;
(4) chromatographic column separates: the chromatographic column that cleans up on the clarification extract after the centrifugation is adsorbed, per minute absorption 10L extract, in adsorption process, extract liquid level and can not be lower than the chromatographic column upper end, control extract face is higher than 3 centimetres of chromatographic column upper ends when absorption finishes; Be that 95% ethanol carries out wash-out with concentration then, per minute ethanol flow is 5L/min, when outflow liquid has color and tangible tobacco aroma is arranged, begins to collect outflow liquid;
(5) decompression concentrates: the outflow liquid that will collect is 58 ℃ in temperature, vacuum is concentration under the condition of 0.090Mpa, obtain density and be 0.8880 concentrate, promptly get tobacco extract, it is a light yellow transparent liquid, and main component is damascenone, damascone, solanone, geranyl acetone, farnesyl acetone, Megastigmatrienone, neophytadiene etc.
Take by weighing extract by 0.01～0.05% of cigarette shreds quality, with concentration is 80% ethanol dissolving extract, adopt the atomizing type spray to be added in the pipe tobacco, be rolled into cigarette, think that through smokeing panel test this product perfuming in cigarette is obvious: can significantly increase cigarette flavor matter and perfume quantity, make plentiful, saturating of cigarette flavor, cover assorted gas, improve the cigarette product quality.
Embodiment 2
(1) enzymolysis: having stirring and adding in the ultrasonic wave extractor of cover water-bath heater, add offal 1000g, deionized water 7000g, add citric acid, adjustment system pH value is between 5.5, add cellulase, enzymolysis is 9 hours under 48 ℃ condition, stirs 10 minutes every 30 minutes when enzymolysis;
(2) ultrasonic wave extracts: after enzymolysis is finished, add deionized water 5000g once more, extracted 40 minutes with ultrasonic wave under 58 ℃ condition, collect extract for the first time, residue partly adopts identical method to extract once more, collects extract for the second time;
(3) centrifugal filtration: above-mentioned extracted twice liquid is merged, at room temperature pass through centrifuge centrifugation 20 minutes under 1700 rev/mins condition, obtain clarifying extract;
(4) chromatographic column separates: the chromatographic column that cleans up on the clarification extract after the centrifugation is adsorbed, per minute absorption 10L extract, in adsorption process, extract liquid level and can not be lower than the chromatographic column upper end, control extract face is higher than 3 centimetres of chromatographic column upper ends when absorption finishes; Be that 95% ethanol carries out wash-out with concentration then, the ethanol flow is 5L/min, when outflow liquid has color and tangible tobacco aroma is arranged, begins to collect outflow liquid;
(5) decompression concentrates: the outflow liquid that will collect is 63 ℃ in temperature, vacuum is concentration under the condition of 0.086Mpa, obtain density and be 0.8980 concentrate, promptly get tobacco extract, it is a light yellow transparent liquid, and main component is damascenone, damascone, solanone, geranyl acetone, farnesyl acetone, Megastigmatrienone, neophytadiene etc.
Take by weighing extract by 0.01～0.05% of cigarette shreds quality, with concentration is 80% ethanol dissolving extract, adopt the atomizing type spray to be added in the pipe tobacco, be rolled into cigarette, think that through smokeing panel test this product perfuming in cigarette is obvious: can significantly increase cigarette flavor matter and perfume quantity, make plentiful, saturating of cigarette flavor, cover assorted gas, improve the cigarette product quality.
Claims (4)
1. the preparation method of a tobacco extract is a raw material with the tobacco, makes tobacco extract through enzymolysis, ultrasonic wave extraction, filtration, chromatographic column separation, decompression concentration step, and the detailed process step is as follows:
(1) enzymolysis: having stirring and adding in the ultrasonic wave extractor of cover water-bath heater, the water that adds offal, 4～8 times of offal quality, add citric acid, adjust system pH between 3.0～6.0, add cellulase, enzymolysis is 8～12 hours under 40～50 ℃ condition, stirs 10 minutes every 30 minutes when enzymolysis;
(2) ultrasonic wave extracts: after enzymolysis is finished, the water that adds 4～8 times of offal quality once more extracted 30～60 minutes with ultrasonic wave under 50～60 ℃ condition, collected extract for the first time, residue partly adopts identical method to extract once more, collects extract for the second time;
(3) filter: extracted twice liquid merging that will be above-mentioned, at room temperature pass through centrifuge centrifugation 20 minutes under 1500～1800 rev/mins condition, obtain clarifying extract;
(4) chromatographic column separates: the chromatographic column that cleans up on the clarification extract after the centrifugation is adsorbed, per minute absorption 10L extract, in adsorption process, extract liquid level and can not be lower than the chromatographic column upper end, control extract face is higher than 3 centimetres of chromatographic column upper ends when absorption finishes; Be that 95% ethanol carries out wash-out with concentration then, the flow of per minute ethanol is 5 liters, when outflow liquid has color and tangible tobacco aroma is arranged, begins to collect outflow liquid;
(5) decompression concentrates: the outflow liquid that will collect is 55～65 ℃ in temperature, and vacuum is concentration under the condition of 0.085～0.095Mpa, obtains density and be 0.8875～0.8986 concentrate, promptly gets tobacco extract.
2. the preparation method of tobacco extract as claimed in claim 1, its feature also is: the hydromining deionized water that adds in described step (1), (2).
3. the application of tobacco extract as claimed in claim 1 is characterized in that: described extract employing concentration is 80% ethanol dissolving extract, adopts the atomizing type spray to be added in the pipe tobacco.
4. the application of tobacco extract as claimed in claim 3, its feature also is: described extract consumption is 0.01～0.05% of a pipe tobacco weight.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100274000A CN101570717B (en) | 2009-06-01 | 2009-06-01 | Method for preparing tobacco extract and application thereof |
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| CN2009100274000A CN101570717B (en) | 2009-06-01 | 2009-06-01 | Method for preparing tobacco extract and application thereof |
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| CN101570717A CN101570717A (en) | 2009-11-04 |
| CN101570717B true CN101570717B (en) | 2011-10-05 |
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| CN101838587B (en) * | 2010-05-27 | 2012-07-04 | 无锡华海香料有限公司 | Method for extracting natural Chinese herbal medicinal flavor component and application of extractive thereof |
| CN102078701B (en) * | 2010-12-20 | 2012-11-14 | 东莞广州中医药大学中医药数理工程研究院 | Energy-saving synergetic method and device in extracting production process of traditional Chinese medicine |
| US9254001B2 (en) | 2011-04-27 | 2016-02-09 | R.J. Reynolds Tobacco Company | Tobacco-derived components and materials |
| CN102326863A (en) * | 2011-07-02 | 2012-01-25 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of cigarette paper filter material containing nicotiana tabacum extract |
| CN102488318A (en) * | 2011-11-18 | 2012-06-13 | 安徽中烟工业有限责任公司 | Preparation method for aired tobacco extracts and essential oil |
| CN102816640B (en) * | 2012-09-05 | 2013-08-07 | 无锡华海香料有限公司 | Preparation method of jujube extract and application thereof |
| CN103126062B (en) * | 2013-03-04 | 2015-07-29 | 湖北中烟工业有限责任公司 | One grows tobacco composition extracting method |
| CN103361176B (en) * | 2013-07-31 | 2014-12-10 | 广州市澳键丰泽生物科技有限公司 | Aroma compound |
| CN103361177B (en) * | 2013-07-31 | 2015-07-08 | 广州市澳键丰泽生物科技有限公司 | Method for extraction of aroma compounds from aroma materials |
| CN104138028B (en) * | 2014-07-15 | 2016-02-24 | 上海烟草集团有限责任公司 | A kind of extracting method of tobacco flavor composition and application thereof |
| CN104480182B (en) * | 2014-12-03 | 2017-11-10 | 湖北中烟工业有限责任公司 | The preparation method of cigarette burley tobaccos flavouring humectant |
| CN105062681A (en) * | 2015-08-17 | 2015-11-18 | 湖北中烟工业有限责任公司 | Preparation method for beta vulgaris spice for cigarettes |
| CN105132176A (en) * | 2015-09-28 | 2015-12-09 | 中国烟草总公司郑州烟草研究院 | Preparation method of Mao cigarette extract and application of Mao cigarette extract to cigarette filter stick |
| CN105639718B (en) * | 2016-02-29 | 2017-06-30 | 湖北中烟工业有限责任公司 | A kind of preparation method and application of the tobacco extract of easy low-temperature atomizing |
| CN106085603A (en) * | 2016-07-21 | 2016-11-09 | 武汉黄鹤楼香精香料有限公司 | A kind of cigarette paper colourless tobacco extract and preparation method thereof |
| CN109007957B (en) * | 2018-06-21 | 2021-10-29 | 重庆中烟工业有限责任公司 | Tobacco extract, preparation method thereof and tobacco product |
| CN110663993B (en) * | 2019-10-10 | 2022-04-22 | 福建中烟工业有限责任公司 | Tobacco extract and preparation method thereof |
| CN111480894A (en) * | 2020-03-25 | 2020-08-04 | 内蒙古昆明卷烟有限责任公司 | Cigarette cartridge containing biological enzyme and tobacco product |
| CN112089087B (en) * | 2020-10-28 | 2022-02-01 | 云南中宝龙天然香料有限公司 | Multistage extraction method of essential oil type tobacco extract |
| CN112425814B (en) * | 2020-11-20 | 2022-02-22 | 河北中烟工业有限责任公司 | Preparation method of high-fragrance tobacco extract |
| CN112471586B (en) * | 2020-11-20 | 2022-03-11 | 河北中烟工业有限责任公司 | Method for simultaneously preparing tobacco essential oil and tobacco juice |
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Address after: 214112 Jiangsu city of Wuxi province new Qumei Wu Cun Mei Yuk Road No. 7, room 117 Patentee after: Wuxi Huahai flavor Co., Ltd. Address before: 214112 Jiangsu Province, Wuxi City District Mei Tin Town Hung Road No. 37, No. 3 Patentee before: Wuxi Huahai Flavors Ltd. |
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Application publication date: 20091104 Assignee: Yingtan Huabao flavors Co. Assignor: Wuxi Huahai flavor Co., Ltd. Contract record no.: 2018320000137 Denomination of invention: Method for preparing tobacco extract and application thereof Granted publication date: 20111005 License type: Exclusive License Record date: 20180801 |
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Effective date of registration: 20210918 Address after: 335000 Ying Nan avenue, Longgang area, Yingtan economic and Technological Development Zone, Jiangxi Patentee after: YINGTAN HUABAO ESSENCE Co.,Ltd. Address before: 214112 room 7, No. 117, Meiyu Road, Meicun, Xinwu District, Wuxi City, Jiangsu Province Patentee before: Wuxi Huahai flavor Co.,Ltd. |
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