CN106010796A - Flavor preparation method, flavor prepared by preparation method and application of flavor - Google Patents
Flavor preparation method, flavor prepared by preparation method and application of flavor Download PDFInfo
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- CN106010796A CN106010796A CN201610581243.8A CN201610581243A CN106010796A CN 106010796 A CN106010796 A CN 106010796A CN 201610581243 A CN201610581243 A CN 201610581243A CN 106010796 A CN106010796 A CN 106010796A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000796 flavoring agent Substances 0.000 title abstract description 11
- 235000019634 flavors Nutrition 0.000 title abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 85
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 84
- 241000208125 Nicotiana Species 0.000 claims abstract description 80
- 239000000284 extract Substances 0.000 claims abstract description 35
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 32
- 235000013599 spices Nutrition 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 24
- 238000001256 steam distillation Methods 0.000 claims abstract description 24
- 230000000391 smoking effect Effects 0.000 claims abstract description 18
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 17
- 239000012465 retentate Substances 0.000 claims abstract description 12
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 10
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960002715 nicotine Drugs 0.000 claims abstract description 10
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000003208 petroleum Substances 0.000 claims abstract description 3
- 239000000341 volatile oil Substances 0.000 claims description 42
- 239000003921 oil Substances 0.000 claims description 26
- 238000004821 distillation Methods 0.000 claims description 25
- 238000001704 evaporation Methods 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 239000003205 fragrance Substances 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 9
- 239000002274 desiccant Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 235000019505 tobacco product Nutrition 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- 239000003571 electronic cigarette Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 239000002304 perfume Substances 0.000 abstract 1
- 244000061176 Nicotiana tabacum Species 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 241000894007 species Species 0.000 description 3
- 235000007173 Abies balsamea Nutrition 0.000 description 2
- 244000020518 Carthamus tinctorius Species 0.000 description 2
- 235000003255 Carthamus tinctorius Nutrition 0.000 description 2
- 244000018716 Impatiens biflora Species 0.000 description 2
- 244000184734 Pyrus japonica Species 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 239000004857 Balsam Substances 0.000 description 1
- 206010013911 Dysgeusia Diseases 0.000 description 1
- 244000062730 Melissa officinalis Species 0.000 description 1
- 235000010654 Melissa officinalis Nutrition 0.000 description 1
- 244000061322 Nicotiana alata Species 0.000 description 1
- 244000006449 Nicotiana forgetiana Species 0.000 description 1
- 241000208128 Nicotiana glauca Species 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 241000208292 Solanaceae Species 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000013532 brandy Nutrition 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019506 cigar Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229940069445 licorice extract Drugs 0.000 description 1
- 239000000865 liniment Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 239000008601 oleoresin Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229940098465 tincture Drugs 0.000 description 1
- -1 tinctures Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000001432 zingiber officinale rosc. oleoresin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Cosmetics (AREA)
Abstract
本发明属于烟用香料领域,具体涉及一种香料的制备方法,包括如下步骤,(1)将烟草进行水蒸汽蒸馏,得到馏出物;(2)将馏出物进行油水分离,得到油状物和水状物;(3)将水状物进行反渗透处理,得到截留物;(4)将截留物进行萃取,得到萃取液,去除萃取液中的萃取剂,得到萃取物;所述萃取剂选自石油醚、环己烷、乙醚和乙酸乙酯中的一种或多种。本发明还涉及所制得的香料及其用途。本发明方法所制备的香料中尼古丁含量低,将所制备的香料添加到卷烟中,可降低抽吸时对喉部的压力,提高抽吸时的舒适度。The invention belongs to the field of spices for tobacco, and specifically relates to a preparation method of spices, comprising the following steps: (1) subjecting tobacco to steam distillation to obtain a distillate; (2) separating the distillate from oil and water to obtain an oil and water; (3) carry out reverse osmosis treatment to the water to obtain the retentate; (4) extract the retentate to obtain the extract, remove the extractant in the extract to obtain the extract; the extractant One or more selected from petroleum ether, cyclohexane, diethyl ether and ethyl acetate. The present invention also relates to the prepared perfume and its use. The nicotine content in the flavor prepared by the method of the invention is low, and adding the prepared flavor to the cigarette can reduce the pressure on the throat during smoking and improve the comfort during smoking.
Description
技术领域technical field
本发明属于烟用香料领域,具体涉及一种香料的制备方法,还涉及所制得的香料及用途。The invention belongs to the field of spices for tobacco, and in particular relates to a preparation method of spices, and also relates to the prepared spices and their uses.
背景技术Background technique
植物性天然香料是从芳香植物的花、草、叶、枝、干、茎、根、皮、果、籽、树脂或香膏等部位中提取出的含香物制品,大多数为油状或膏状,少数呈树脂或半固态。根据它们的形态和制法,通常称为精油、酊剂、浸膏、净油、香脂或油树脂,例如玫瑰精油、枣子酊、甘草浸膏、白兰香脂和姜油树脂。Plant-based natural fragrances are fragrance-containing products extracted from the flowers, grasses, leaves, branches, trunks, stems, roots, skins, fruits, seeds, resins or balms of aromatic plants, most of which are oily or ointment Shape, few are resinous or semi-solid. Depending on their form and method of preparation, they are commonly called essential oils, tinctures, extracts, absolutes, balsams, or oleoresins, such as rose essential oil, date tincture, licorice extract, brandy balsam, and ginger oleoresin.
植物性天然香料的制备方法中,水蒸汽蒸馏法是常用方法。将水蒸汽通入盛有植物原料的容器中,挥发性成分随水蒸汽蒸馏出来,所制取天然香料的组分为芳香性的挥发性油状物,一般统称为精油。水蒸汽蒸馏中,水主要发挥三种作用,即水散作用、水解作用和热力作用,水的作用过程简单归纳如下,原料表面润湿—水分子向原料的细胞组织内部渗透—水置换精油或微量溶解—精油向水中扩散—形成精油与水的共沸物—精油与水蒸汽同时蒸出—冷凝—油水分离—精油。除了在沸水中主香成分容易溶解、水解或分解的植物原料外,绝大多数芳香植物均可用水蒸汽蒸馏法制备精油。水蒸汽蒸馏法有三种主要形式:水中蒸馏、水上蒸馏和水汽蒸馏,水蒸汽蒸馏的设备主要有蒸馏釜、冷凝器和油水分离器三部分。现有的水蒸汽蒸馏工艺存在诸多不足,比如,以萃取法提取水状物中的油分时,需使用大量污染性的有机萃取剂;复蒸会破坏或分解对温度敏感的有效成分等。Among the preparation methods of plant-based natural spices, steam distillation is a common method. The water vapor is passed into the container containing the plant raw materials, and the volatile components are distilled out with the water vapor. The components of the prepared natural fragrance are aromatic volatile oils, which are generally referred to as essential oils. In steam distillation, water mainly plays three functions, namely, water dispersion, hydrolysis and thermal effect. The process of water action is simply summarized as follows: Wetting the surface of the raw material—water molecules penetrate into the cell tissue of the raw material—water replaces the essential oil or Trace dissolution—diffusion of essential oil into water—formation of azeotrope of essential oil and water—simultaneous distillation of essential oil and water vapor—condensation—separation of oil and water—essential oil. Except for the plant raw materials whose main aroma components are easily dissolved, hydrolyzed or decomposed in boiling water, most aromatic plants can be used to prepare essential oils by steam distillation. There are three main forms of steam distillation: water distillation, water distillation and water vapor distillation. The equipment for steam distillation mainly includes three parts: distillation still, condenser and oil-water separator. There are many deficiencies in the existing steam distillation process. For example, when extracting the oil in the water by extraction, a large amount of polluting organic extractant needs to be used; re-evaporation will destroy or decompose the effective components that are sensitive to temperature.
反渗透是以压力差为推动力,从溶液中分离出溶剂的膜分离技术,以达到分离、提取、纯化或浓缩的目的,它和自然渗透的方向相反,称为反渗透。Reverse osmosis is a membrane separation technology that uses pressure difference as the driving force to separate the solvent from the solution to achieve the purpose of separation, extraction, purification or concentration. It is opposite to the direction of natural osmosis and is called reverse osmosis.
目前,尚需一种新的制备香料的方法,以得到一种新型的香料产品。At present, a new method for preparing spices is still needed to obtain a novel spice product.
发明内容Contents of the invention
本发明人创造性地获得了一种香料的制备方法,该方法由烟草提取出香料,所制得香料的尼古丁含量较低。本发明人还发现将该香料添加到烟丝中制作成卷烟,可降低卷烟抽吸过程中的喉部压力,提高舒适度。并且,本发明方法能有效收集油水分离所得水状物中的油相香料成分,经济环保。The present inventors have creatively obtained a preparation method of spices, which extracts spices from tobacco, and the nicotine content of the prepared spices is relatively low. The inventors also found that adding the flavor into shredded tobacco to make cigarettes can reduce throat pressure during cigarette smoking and improve comfort. Moreover, the method of the present invention can effectively collect the oil-phase fragrance components in the water obtained from the oil-water separation, and is economical and environment-friendly.
本发明第一方面涉及一种香料的制备方法,包括如下步骤,The first aspect of the present invention relates to a preparation method of spices, comprising the following steps,
(1)将烟草进行水蒸汽蒸馏,得到馏出物;(1) Steam distilling the tobacco to obtain a distillate;
(2)将馏出物进行油水分离,得到油状物和水状物;(2) the distillate is subjected to oil-water separation to obtain oil and water;
(3)将水状物进行反渗透处理,得到截留物;(3) carrying out reverse osmosis treatment to the aqueous substance to obtain the retentate;
(4)将截留物进行萃取,得到萃取液,去除萃取液中的萃取剂,得到萃取物;所述萃取剂选自石油醚、环己烷、乙醚和乙酸乙酯中的一种或多种。(4) Extract the retentate to obtain an extract, remove the extractant in the extract to obtain an extract; the extractant is selected from one or more of petroleum ether, cyclohexane, ether and ethyl acetate .
在一个实施方案中,所述香料为萃取物。In one embodiment, the fragrance is an extract.
在一个实施方案中,反渗透处理的压力为0.4-5MPa,优选为0.5-3MPa,更优选为0.8MPa或1.0MPa。In one embodiment, the pressure of the reverse osmosis treatment is 0.4-5 MPa, preferably 0.5-3 MPa, more preferably 0.8 MPa or 1.0 MPa.
在一个实施方案中,反渗透处理所得截留物的重量为水状物重量的0.05-0.8,优选为0.08-0.5,更优选为0.1或0.088。In one embodiment, the weight of the retentate obtained from the reverse osmosis treatment is 0.05-0.8, preferably 0.08-0.5, more preferably 0.1 or 0.088 of the weight of the water.
本发明第一方面的一个实施方式中,还包括,将油状物和萃取物混合,得到混合提取物的步骤。In one embodiment of the first aspect of the present invention, it also includes the step of mixing the oily substance and the extract to obtain a mixed extract.
在一个实施方案中,所述香料为混合提取物。In one embodiment, the flavor is a mixed extract.
在一个实施方案中,混合前,还包括对油状物除水的步骤;优选地,用无水硫酸钠或无水硫酸镁干燥剂除水;优选地,除水时间为2-24小时,更加优选为4小时。In one embodiment, before mixing, it also includes the step of removing water from the oil; preferably, using anhydrous sodium sulfate or anhydrous magnesium sulfate desiccant to remove water; preferably, the water removal time is 2-24 hours, more preferably Preferably 4 hours.
本发明第一方面的一个实施方式中,包括如下1)至13)中的任意一项或者多项:In an embodiment of the first aspect of the present invention, any one or more of the following 1) to 13) is included:
1)所述烟草为烟叶;优选地,所述烟草选自三明尤溪烟叶、津巴布韦烟叶和云南大理祥云烟叶中的一种或多种;1) The tobacco is tobacco leaves; preferably, the tobacco is selected from one or more of Sanming Youxi tobacco leaves, Zimbabwe tobacco leaves and Yunnan Dali Xiangyun tobacco leaves;
2)所述水蒸汽蒸馏选自水中蒸馏、水上蒸馏和直接水蒸汽蒸馏,例如为直接水蒸汽蒸馏;2) the steam distillation is selected from distillation in water, distillation on water and direct steam distillation, such as direct steam distillation;
3)所述水蒸汽蒸馏的温度为90-120℃,优选为100℃;3) The temperature of the steam distillation is 90-120°C, preferably 100°C;
4)所述水蒸汽蒸馏的时间为1-10小时,优选为2-8小时,更优选为2小时、3小时或6小时;4) The steam distillation time is 1-10 hours, preferably 2-8 hours, more preferably 2 hours, 3 hours or 6 hours;
5)水蒸汽蒸馏过程中的蒸汽阀门开度≥5%,优选为10-32%,更优选为10%、15%、20%、25%或30%;6)所述馏出物的产出速率为5-70kg/h,优选为10-60kg/h,更优选为12kg/h、15kg/h、30kg/h或40kg/h;5) The opening of the steam valve in the steam distillation process is ≥5%, preferably 10-32%, more preferably 10%, 15%, 20%, 25% or 30%; 6) the product of the distillate The output rate is 5-70kg/h, preferably 10-60kg/h, more preferably 12kg/h, 15kg/h, 30kg/h or 40kg/h;
7)所述水蒸汽蒸馏为常压水蒸汽蒸馏;7) the steam distillation is atmospheric pressure steam distillation;
8)所述反渗透处理的温度不高于30℃,优选为10-30℃,更优选为10℃、25℃或30℃;8) The temperature of the reverse osmosis treatment is not higher than 30°C, preferably 10-30°C, more preferably 10°C, 25°C or 30°C;
9)所述反渗透处理的时间为0.5-6小时,优选为1-4小时,更优选为1小时、2小时、3小时或4小时;9) The reverse osmosis treatment time is 0.5-6 hours, preferably 1-4 hours, more preferably 1 hour, 2 hours, 3 hours or 4 hours;
10)步骤(4)中,萃取剂的添加量为截留物的1/8-1/2(W/W),优选为1/5-1/3(W/W),更优选为1/4(W/W);10) In step (4), the amount of extractant added is 1/8-1/2 (W/W) of the retentate, preferably 1/5-1/3 (W/W), more preferably 1/ 4(W/W);
11)步骤(4)中,对截留物进行多次萃取,合并萃取液;优选地,萃取3-6次,更优选为4次;优选地,每次萃取使用萃取剂的重量相同;11) In step (4), extract the retentate multiple times, and combine the extracts; preferably, extract 3-6 times, more preferably 4 times; preferably, use the same weight of extractant for each extraction;
12)步骤(4)中,通过蒸发去除萃取剂,优选为旋转蒸发;更优选地,蒸发温度≤60℃,蒸发压力为50-380mbar;进一步优选地,蒸发温度≤50℃,蒸发压力为100-300mbar;更进一步优选地,蒸发温度为30℃或35℃,压力为210mbar或250mbar;12) In step (4), the extraction agent is removed by evaporation, preferably rotary evaporation; more preferably, the evaporation temperature is ≤60°C, and the evaporation pressure is 50-380mbar; further preferably, the evaporation temperature is ≤50°C, and the evaporation pressure is 100 -300mbar; more preferably, the evaporation temperature is 30°C or 35°C, and the pressure is 210mbar or 250mbar;
13)步骤(4)中,去除萃取剂前,还包括对萃取液除水的步骤;优选地,采用无水硫酸钠或无水硫酸镁干燥剂除水;优选地,除水时间为2-24小时,更优选为4小时。13) In step (4), before removing the extractant, it also includes the step of removing water from the extract; preferably, using anhydrous sodium sulfate or anhydrous magnesium sulfate desiccant to remove water; preferably, the water removal time is 2- 24 hours, more preferably 4 hours.
本发明第二方面涉及一种香料,由本发明第一方面任一项所述方法制备得到。The second aspect of the present invention relates to a spice prepared by any one of the methods described in the first aspect of the present invention.
本发明第二方面的一个实施方式中,所述香料中的尼古丁含量≤1.8%(W/W),优选为≤1.7%(W/W)、≤1.6%(W/W)、≤1.5%(W/W)、≤1.4%(W/W)、≤1.3%(W/W)或≤1.2%(W/W),更优选为1.01%(W/W)、1.03%(W/W)、1.13%(W/W)、1.31%(W/W)、1.32%(W/W)、1.36%(W/W)、1.41%(W/W)、1.48%(W/W)或1.52%(W/W)。In an embodiment of the second aspect of the present invention, the nicotine content in the spices is ≤1.8% (W/W), preferably ≤1.7% (W/W), ≤1.6% (W/W), ≤1.5% (W/W), ≤1.4% (W/W), ≤1.3% (W/W) or ≤1.2% (W/W), more preferably 1.01% (W/W), 1.03% (W/W ), 1.13% (W/W), 1.31% (W/W), 1.32% (W/W), 1.36% (W/W), 1.41% (W/W), 1.48% (W/W) or 1.52% (W/W).
在一个实施方案中,所述香料为烟用香料;优选地,所述烟用香料是用于烟叶、烟丝、梗丝、薄片、滤嘴、接装纸、烟盒或电子烟的香料。In one embodiment, the flavor is a flavor for tobacco; preferably, the flavor for tobacco is a flavor for tobacco leaves, shredded tobacco, shredded stems, sheets, filters, tipping papers, cigarette cases or electronic cigarettes.
在一个实施方案中,所述香料为精油。In one embodiment, the fragrance is an essential oil.
本发明第三方面涉及一种烟用组合物,其包含本发明第二方面所述的香料;可选地,还包含载体和辅料。The third aspect of the present invention relates to a smoking composition, which includes the fragrance described in the second aspect of the present invention; optionally, also includes a carrier and auxiliary materials.
在一个实施方案中,所述烟用组合物是用于烟叶、烟丝、梗丝、薄片、滤嘴、接装纸、烟盒或电子烟的组合物。In one embodiment, the smoking composition is a composition for tobacco leaves, shredded tobacco, cut stems, sheets, filters, tipping papers, cigarette cases or electronic cigarettes.
本发明第四方面涉及一种卷烟,其包含本发明第二方面所述的香料和/或本发明第三方面所述的烟用组合物;可选地,还包含烟丝。The fourth aspect of the present invention relates to a cigarette, which comprises the spice according to the second aspect of the present invention and/or the smoking composition described in the third aspect of the present invention; optionally, shredded tobacco.
本发明第五方面涉及一种卷烟的制作方法,包括按照本发明第一方面任一项所述方法制备香料的步骤以及将所述香料添加到烟丝中的步骤;和/或包括将本发明第三方面所述烟用组合物添加到烟丝中的步骤。The fifth aspect of the present invention relates to a method for making cigarettes, including the steps of preparing spices according to any one of the methods described in the first aspect of the present invention and the step of adding the spices to shredded tobacco; The step of adding the smoking composition described in the third aspect to shredded tobacco.
本发明第六方面涉及本发明第二方面所述香料和/或本发明第三方面所述烟用组合物在制作烟草制品或者在降低抽吸烟草制品过程中的喉部压力、提高舒适度中的用途;优选地,所述烟草制品为卷烟。The sixth aspect of the present invention relates to the spices described in the second aspect of the present invention and/or the smoking composition described in the third aspect of the present invention in making tobacco products or reducing throat pressure and improving comfort in the process of smoking tobacco products purposes; preferably, the tobacco product is a cigarette.
本发明全文引用下述文献:The present invention cites the following documents in full:
GB2635-92烤烟GB2635-92 flue-cured tobacco
GBT18771.2-2002烟草术语第2部分:烟草加工、烟草制品。GBT18771.2-2002 Tobacco Terminology Part 2: Tobacco Processing, Tobacco Products.
本发明中,如无特别说明,油状物是指馏出物经油水分离后得到的含少量或微量水分的油层,油层中的油含量小于100%。In the present invention, unless otherwise specified, the oily substance refers to the oil layer containing a small amount or a small amount of water obtained after the distillate is separated from oil and water, and the oil content in the oil layer is less than 100%.
本发明中,如无特别说明,水状物是指馏出物经油水分离后得到的含少量或微量油分的水层,水层中的水含量小于100%。In the present invention, unless otherwise specified, the watery substance refers to the water layer containing a small or trace amount of oil obtained after the distillate is separated from oil and water, and the water content in the water layer is less than 100%.
本发明中,如无特别说明,烟草是指茄科一年生或多年生草本,嗜好类作物。本属约有60多个种,大多是野生种。主要栽培种有红花烟草和黄花烟草。二者均原产南美洲,都是自然产生的双二倍体。红花烟草又称普通烟草,是世界性商品生产用烟种。又因调制方法及种源、地区、栽培措施不同而形成多种类型:烤烟、白肋烟、马里兰烟、雪茄烟、熏烟、香料烟、晒红烟、晒黄烟等。每一类型中又有很多栽培品种。黄花烟草以前苏联和印度栽培较多,中国新疆、甘肃等地有少量栽培。本属中的花烟草(N.alata Link and Otta)和粉蓝烟草(N.glauca Graham)栽种供观赏。In the present invention, unless otherwise specified, tobacco refers to the annual or perennial herb of the family Solanaceae, a hobby crop. There are more than 60 species in this genus, most of which are wild species. The main cultivated species are Nicotiana safflower and Nicotiana japonica. Both are native to South America and are naturally occurring amphidiploids. Safflower tobacco, also known as ordinary tobacco, is a kind of tobacco used in the production of commodities worldwide. Due to different preparation methods, sources, regions, and cultivation measures, various types are formed: flue-cured tobacco, burley tobacco, Maryland tobacco, cigar tobacco, smoked tobacco, oriental tobacco, sun-cured red tobacco, sun-cured yellow tobacco, etc. Within each type there are many cultivars. Nicotiana japonica was cultivated more in the Soviet Union and India in the past, and it was cultivated in a small amount in Xinjiang, Gansu and other places in China. Nicotiana tabacum (N. alata Link and Otta) and Nicotiana tabacum (N. glauca Graham) in this genus are grown for ornamental purposes.
本发明中,如无特别说明,尼古丁又称烟碱,分子式为C10H14N2,是烟草属植物含有的一种植物碱,是烟草重要成分之一,性剧毒,小剂量能使中枢神经兴奋,呼吸增强,血压升高,大剂量时发生抑郁和神经系统麻痹。In the present invention, unless otherwise specified, nicotine is also called nicotine, and its molecular formula is C 10 H 14 N 2 . It is a plant alkaloid contained in Nicotiana plants and one of the important components of tobacco. The central nervous system is excited, breathing is enhanced, blood pressure is increased, and depression and nervous system paralysis occur in large doses.
本发明中,如无特别说明,水中蒸馏是指将原料放入水中进行蒸馏。In the present invention, unless otherwise specified, distillation in water refers to putting raw materials into water for distillation.
本发明中,如无特别说明,水上蒸馏是指将原料放在水面上方的筛板上进行蒸馏。In the present invention, unless otherwise specified, distillation over water means that the raw material is placed on a sieve plate above the water surface for distillation.
本发明中,如无特别说明,直接水蒸汽蒸馏是指蒸馏容器的下部设有进气孔,由进气孔通入外源水蒸汽,原料放置在进气孔上方的筛板上进行蒸馏。In the present invention, unless otherwise specified, direct steam distillation means that the lower part of the distillation vessel is provided with an air inlet through which external source water vapor is introduced, and the raw material is placed on a sieve plate above the air inlet for distillation.
本发明取得的有益效果:The beneficial effect that the present invention obtains:
1、本发明方法制备的香料中尼古丁含量低。1. The nicotine content in the spices prepared by the method of the present invention is low.
2、本发明方法制备的香料添加到烟丝中制成卷烟,可有效降低卷烟抽吸时对喉部的压力,提高抽吸的舒适度。2. The spices prepared by the method of the present invention are added to shredded tobacco to make cigarettes, which can effectively reduce the pressure on the throat when cigarettes are smoked, and improve the comfort of smoking.
3、本发明方法,可有效收集油水分离所得水状物中的油相香料成分,经济环保。3. The method of the present invention can effectively collect the oil-phase fragrance components in the water obtained from oil-water separation, and is economical and environmentally friendly.
附图说明Description of drawings
为了使本发明的内容更容易被清楚的理解,下面根据本发明的具体实施例并结合附图,对本发明作进一步详细的说明,其中In order to make the content of the present invention more easily understood, the present invention will be described in further detail below according to specific embodiments of the present invention in conjunction with the accompanying drawings, wherein
图1为本发明香料制备方法的流程图。Fig. 1 is the flowchart of the preparation method of spices of the present invention.
具体实施方式detailed description
如无另外说明,以下各实施例均采用如下材料和试剂:Unless otherwise stated, each of the following examples adopts the following materials and reagents:
三明尤溪烟叶,购自中国烟草总公司,烟叶等级C3F/2010T;Sanming Youxi Tobacco Leaf, purchased from China National Tobacco Corporation, tobacco grade C3F/2010T;
津巴布韦烟叶,购自中国烟草总公司,烟叶等级CJOT/2010;Tobacco leaves from Zimbabwe, purchased from China National Tobacco Corporation, grade CJOT/2010;
云南大理祥云烟叶,购自中国烟草总公司,烟叶等级C3F/2010T;Yunnan Dali Xiangyun Tobacco Leaf, purchased from China National Tobacco Corporation, tobacco leaf grade C3F/2010T;
蒸汽,由厦门国能同集热电有限公司提供;Steam, provided by Xiamen Guoneng Tongji Thermal Power Co., Ltd.;
乙酸乙酯(A.R.),国药集团化学试剂有限公司;Ethyl acetate (A.R.), Sinopharm Chemical Reagent Co., Ltd.;
乙醚(A.R.),国药集团化学试剂有限公司;Diethyl ether (A.R.), Sinopharm Chemical Reagent Co., Ltd.;
无水硫酸钠(A.R.),国药集团化学试剂有限公司;Anhydrous sodium sulfate (A.R.), Sinopharm Chemical Reagent Co., Ltd.;
反渗透膜为GE HWS RO 8040HR(脱盐率NaCl 99.5%)。The reverse osmosis membrane is GE HWS RO 8040HR (salt removal rate NaCl 99.5%).
实施例1制备精油AEmbodiment 1 prepares essential oil A
参照图1的流程,称取30kg三明尤溪烟叶,置入蒸馏釜的提取罐吊篮中,开启蒸汽加热阀门,阀门开度为20%,蒸馏温度(水蒸汽温度)为100℃,水蒸汽由下部进入蒸馏釜内,与烟叶物料充分接触、分散和气化,形成的水和挥发性精油的混合蒸汽从蒸馏釜上部的蒸汽出口导出,经冷凝器冷凝,得到馏出物,馏出物的产出速率为40kg/h,蒸馏时间为2小时。With reference to the flow chart in Figure 1, weigh 30kg of Sanming Youxi tobacco leaves, put them into the extraction tank hanging basket of the distillation kettle, open the steam heating valve, the valve opening is 20%, the distillation temperature (water vapor temperature) is 100°C, and the water vapor Enter the still from the lower part, fully contact with the tobacco leaf material, disperse and gasify, the formed mixed steam of water and volatile essential oil is led out from the steam outlet of the upper part of the still, condensed by the condenser, and distillate is obtained. The output rate was 40 kg/h and the distillation time was 2 hours.
馏出物进入油水分离器进行分离,收集得到油状物(烟叶直接精油A)20g和水状物80kg。The distillate enters the oil-water separator for separation, collects and obtains 20 g of oil (direct essential oil A of tobacco leaves) and 80 kg of water.
采用一级反渗透膜,调节膜堆压力为0.8MPa,冷却水温度为25℃,将水状物80kg浓缩至8kg,即为浓缩液。将浓缩液加入萃取釜中,加入乙酸乙酯2kg萃取,重复4次,合并萃取液,加入一定量无水Na2SO4干燥4小时,过滤除去干燥剂。采用旋转蒸发仪,设置浓缩温度为35℃,真空度为210mbar,蒸出乙酸乙酯后得萃取物,即水中油3g。Using a first-stage reverse osmosis membrane, adjust the pressure of the membrane stack to 0.8MPa, and the temperature of the cooling water to 25°C, and concentrate 80kg of water to 8kg, which is the concentrate. Put the concentrated solution into the extraction kettle, add 2kg of ethyl acetate to extract, repeat 4 times, combine the extracts, add a certain amount of anhydrous Na 2 SO 4 to dry for 4 hours, and filter to remove the desiccant. Using a rotary evaporator, set the concentration temperature to 35°C and the vacuum degree to 210mbar, and evaporate the ethyl acetate to obtain the extract, namely 3g of oil in water.
将烟叶直接精油20g和水中油3g混合均匀,制备得到23g的精油A。20 g of direct tobacco leaf essential oil and 3 g of oil in water were evenly mixed to prepare 23 g of essential oil A.
将精油A按照0.01%(W/W)的比例添加到烟丝中,按照常规方法制作成卷烟1#。The essential oil A was added to shredded tobacco at a ratio of 0.01% (W/W), and cigarette 1# was made according to a conventional method.
实施例2制备精油BEmbodiment 2 prepares essential oil B
参照图1的流程,称取30kg津巴布韦烟叶,置入蒸馏釜的提取罐吊篮中,开启蒸汽加热阀门,阀门开度为15%,蒸馏温度(水蒸汽温度)为100℃,水蒸汽由下部进入蒸馏釜中,与烟叶物料充分接触、分散和气化,形成的水和挥发性精油的混合蒸汽从蒸馏釜上部的蒸汽出口导出,经冷凝器冷凝,得到馏出物,馏出物的流量在30kg/小时,蒸馏时间为3.0小时。馏出物进入油水分离器分离,收集油状物(烟叶直接精油)22g和水状物90kg。With reference to the flow chart in Figure 1, weigh 30kg of Zimbabwean tobacco leaves, put them into the extraction tank hanging basket of the still, open the steam heating valve, the valve opening is 15%, the distillation temperature (steam temperature) is 100°C, and the water vapor is discharged from the lower part Enter the still, fully contact with the tobacco leaf material, disperse and gasify, the formed mixed steam of water and volatile essential oil is led out from the steam outlet on the upper part of the still, condensed by the condenser, and the distillate is obtained. The flow rate of the distillate is at 30kg/hour, the distillation time is 3.0 hours. The distillate enters the oil-water separator for separation, and collects 22 g of oil (direct essential oil of tobacco leaves) and 90 kg of water.
采用一级反渗透膜,调节膜堆压力为1.0MPa,冷却水温度为25℃,将水状物90kg浓缩至8kg,即为浓缩液。将浓缩液加入萃取釜中,加入乙醚2kg萃取,重复4次,合并萃取液,加入一定量无水Na2SO4干燥4小时,过滤除去干燥剂。采用旋转蒸发仪,设置浓缩温度为30℃,真空度为250mbar,将乙醚蒸出后得萃取物,即水中油4g。Using a first-stage reverse osmosis membrane, adjust the pressure of the membrane stack to 1.0MPa, and the temperature of the cooling water to 25°C, and concentrate 90kg of water to 8kg, which is the concentrate. Put the concentrated solution into the extraction kettle, add 2kg of diethyl ether to extract, repeat 4 times, combine the extracts, add a certain amount of anhydrous Na 2 SO 4 to dry for 4 hours, and filter to remove the desiccant. Using a rotary evaporator, set the concentration temperature to 30°C and the vacuum degree to 250mbar, distill off the diethyl ether to obtain the extract, namely 4g of oil in water.
将烟叶直接精油22g和水中油4g混合均匀,制备得到26g精油B。22g of direct tobacco leaf essential oil and 4g of oil in water were evenly mixed to prepare 26g of essential oil B.
将精油B按照0.01%(W/W)比例添加到烟丝中,按照常规方法制作成卷烟2#。The essential oil B was added to shredded tobacco at a ratio of 0.01% (W/W), and cigarette 2# was made according to a conventional method.
实施例3制备精油CEmbodiment 3 prepares essential oil C
参照图1的流程,称取100kg云南大理祥云烟叶,置入蒸馏釜的提取罐吊篮中,开启蒸汽加热阀门,阀门开度为10%,蒸馏温度(水蒸汽温度)为100℃,水蒸汽由下部进入蒸馏釜中,与烟叶物料充分接触、分散和气化,形成的水和挥发性精油的混合蒸汽从蒸馏罐上部的蒸汽出口导出,经冷凝器冷凝,得到馏出物,馏出物的流量在12kg/小时,蒸馏时间为6.0小时。馏出物进入油水分离器分离,收集油状物(烟叶直接精油)80g和水状物72kg。With reference to the flow chart in Figure 1, weigh 100 kg Yunnan Dali Xiangyun tobacco leaves, put them into the extraction tank hanging basket of the distillation kettle, open the steam heating valve, the valve opening is 10%, the distillation temperature (water vapor temperature) is 100 °C, and the water vapor Enter the still from the lower part, fully contact with the tobacco leaf material, disperse and gasify, the formed mixed steam of water and volatile essential oil is led out from the steam outlet of the upper part of the still, condensed by the condenser, and the distillate is obtained. The flow rate is 12 kg/hour, and the distillation time is 6.0 hours. The distillate enters the oil-water separator for separation, and 80 g of oily matter (direct essential oil of tobacco leaves) and 72 kg of watery matter are collected.
采用一级反渗透膜,调节膜堆压力为1.0MPa,冷却水温度为25℃,将水状物72kg浓缩至8kg,即为浓缩液。将浓缩液加入萃取釜中,加入乙醚2kg萃取,重复4次,合并乙醚萃取液,加入一定量无水Na2SO4干燥4小时,过滤除去干燥剂。采用旋转蒸发仪,设置浓缩温度为30℃,真空度为250mbar,将乙醚蒸出后得萃取物,即水中油19g。Using a first-stage reverse osmosis membrane, adjust the pressure of the membrane stack to 1.0MPa, and the temperature of the cooling water to 25°C, and concentrate 72kg of the water to 8kg, which is the concentrate. Add the concentrated solution into the extraction kettle, add 2 kg of diethyl ether to extract, repeat 4 times, combine the diethyl ether extracts, add a certain amount of anhydrous Na 2 SO 4 to dry for 4 hours, and filter to remove the desiccant. Using a rotary evaporator, set the concentration temperature to 30°C and the vacuum degree to 250mbar, distill off the diethyl ether to obtain the extract, that is, 19g of oil in water.
将烟叶直接精油80g和水中油19混合均匀,制备得到99g的精油C。80 g of tobacco leaf essential oil and oil in water 19 were evenly mixed to prepare 99 g of essential oil C.
将精油C按照0.01%(W/W)的比例添加到烟丝中,按照常规方法制作成卷烟3#。The essential oil C was added to shredded tobacco at a ratio of 0.01% (W/W), and cigarette 3# was made according to a conventional method.
对比例1Comparative example 1
称取30kg三明尤溪烟叶,置入蒸馏釜的提取罐吊篮中,开启蒸汽加热阀门,阀门开度为20%,蒸馏温度(水蒸汽温度)为100℃,水蒸汽由下部进入蒸馏釜内,与烟叶物料充分接触、分散和气化,形成的水和挥发性精油的混合蒸汽从蒸馏釜上部的蒸汽出口导出,经冷凝器冷凝,得到馏出物,馏出物的流量在40kg/小时,蒸馏时间为2.0小时。馏出物进入油水分离器分离,收集油状物(烟叶直接精油)19.8g和水状物80kg。Weigh 30kg of Sanming Youxi tobacco leaves, put them into the extraction tank hanging basket of the still, open the steam heating valve, the valve opening is 20%, the distillation temperature (steam temperature) is 100°C, and the water vapor enters the still from the lower part , fully contact with the tobacco leaf material, disperse and gasify, the formed mixed steam of water and volatile essential oil is exported from the steam outlet on the upper part of the still, and condensed by a condenser to obtain a distillate, the flow rate of the distillate is 40kg/hour, The distillation time was 2.0 hours. The distillate enters the oil-water separator for separation, and 19.8 g of oily matter (direct essential oil of tobacco leaves) and 80 kg of watery matter are collected.
将水状物80kg加入萃取釜中,加入乙酸乙酯20kg萃取,重复4次,合并萃取液,加入一定量无水Na2SO4干燥4小时,过滤除去干燥剂。采用旋转蒸发仪,设置浓缩温度为35℃,真空度为210mbar,蒸出乙酸乙酯后得萃取物,即水中油2.6g。Add 80kg of the aqueous substance into the extraction kettle, add 20kg of ethyl acetate to extract, repeat 4 times, combine the extracts, add a certain amount of anhydrous Na 2 SO 4 to dry for 4 hours, and filter to remove the desiccant. Using a rotary evaporator, set the concentration temperature to 35°C and the vacuum degree to 210mbar, and evaporate the ethyl acetate to obtain the extract, namely 2.6g of oil in water.
将烟叶直接精油19.8g和水中油2.6g混合均匀,制备得到22.4g的精油E。19.8 g of direct tobacco leaf essential oil and 2.6 g of oil in water were evenly mixed to prepare 22.4 g of essential oil E.
将精油E按照0.01%(W/W)的比例添加到烟丝中,按照常规方法制作成卷烟Ⅰ。The essential oil E was added to shredded tobacco at a ratio of 0.01% (W/W), and cigarette I was made according to a conventional method.
对比例2Comparative example 2
将实施例1制备得到的烟叶直接精油A按照0.01%(W/W)的比例添加到烟丝中,按照常规方法制作成卷烟Ⅱ。The tobacco leaf direct essential oil A prepared in Example 1 was added to shredded tobacco at a ratio of 0.01% (W/W), and cigarette II was made according to a conventional method.
实验例1Experimental example 1
采用安捷伦气质联用仪7890A-5975C测定实施例1-3和对比例得到的烟叶直接精油、水中油和精油(A-C及E)中的尼古丁含量,结果见表1。The nicotine content in the tobacco leaf direct essential oil, oil in water and essential oil (A-C and E) obtained in Examples 1-3 and Comparative Examples was measured by Agilent GC-MS 7890A-5975C, and the results are shown in Table 1.
表1尼古丁含量(W/W)Table 1 Nicotine content (W/W)
由表1可知,与对比例1方法相比,本发明方法制备的水中油和精油中的尼古丁含量更低。As can be seen from Table 1, compared with the method of Comparative Example 1, the nicotine content in the oil in water and essential oil prepared by the method of the present invention is lower.
实验例2Experimental example 2
依据国家标准GB5606.4-2005对卷烟1#~3#和卷烟Ⅰ~Ⅱ进行感官质量评吸,结果见表2。According to the national standard GB5606.4-2005, the sensory quality of cigarettes 1# to 3# and cigarettes I to II was smoked, and the results are shown in Table 2.
表2感官质量评吸Table 2 sensory quality evaluation
由表2可知,与对比例1工艺相比,本发明方法制备的香料添加到卷烟中,使抽吸时劲头分散,喉部压力感改善,舒适性提高。It can be seen from Table 2 that, compared with the process of Comparative Example 1, the spice prepared by the method of the present invention is added to the cigarette, which can disperse the force when smoking, improve the pressure feeling in the throat, and improve the comfort.
而且,与油水分离得到的烟叶直接精油A相比,本发明方法制备的香料添加到卷烟中,抽吸时劲头分散,舒适性和喉部压力感进一步改善,余味没有涩感。Moreover, compared with the direct essential oil A of tobacco leaves obtained by oil-water separation, the fragrance prepared by the method of the present invention is added to cigarettes, the strength is dispersed during smoking, the comfort and throat pressure are further improved, and the aftertaste has no astringent feeling.
显然,上述实施例仅仅是为清楚地说明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。Apparently, the above-mentioned embodiments are only examples for clear description, rather than limiting the implementation. For those of ordinary skill in the art, on the basis of the above description, other changes or changes in different forms can also be made. It is not necessary and impossible to exhaustively list all the implementation manners here. And the obvious changes or changes derived therefrom are still within the scope of protection of the present invention.
Claims (10)
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