CN102643718A - Gillyflower extract and preparation method and applications thereof - Google Patents
Gillyflower extract and preparation method and applications thereof Download PDFInfo
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- CN102643718A CN102643718A CN2012101237320A CN201210123732A CN102643718A CN 102643718 A CN102643718 A CN 102643718A CN 2012101237320 A CN2012101237320 A CN 2012101237320A CN 201210123732 A CN201210123732 A CN 201210123732A CN 102643718 A CN102643718 A CN 102643718A
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Abstract
The invention relates to a gillyflower extract and a preparation method and applications thereof, belonging to the technical field of cigarette processing. The preparation method comprises the following steps: drying fresh gillyflower in the shade; smashing the dried gillyflower and sieving by a sieve with 20 meshes to obtain gillyflower powder; carrying out distillation extraction by adopting a device for distilling and extracting at the same time; continuously extracting 50g of gillyflower powder and 20ml of dichloromethane for 1-5 hours at the temperature of 50 DEG C; transferring a distillation extraction liquid to a liquid separating funnel; collecting a dichloromethane layer; and utilizing the dichloromethane rotatably recovered by a rotary evaporator at constant pressure of 40 DEG C to obtain a concentrated solution which is gillyflower extract. With adoption of 0.005-0.1% of gillyflower extract used as a spice additive in flavoring of cut tobacco of cigarette, the flavor of the cigarette can be obviously improved and modified; the fresh and sweet flavor can be enhanced, the stimulation is reduced, the miscellaneous flavors can be removed and the smoke is soft and delicate.
Description
Technical field
The present invention relates to a kind of gillyflower extract, belong to technical field of cigarette processing.
Background technology
No matter be the world or domestic, reduce the important topic that tar content has become production of cigarettes, and the many fragrance matters in the tobacco are present among the tar; Be accompanied by the reduction of tar content, smoke is thin out, and fragrance weakens; Cigarette product loses original style, is difficult to accepted by the human consumer.Current, when reducing coke tar in cigarette, promote and improve flue gas concentration and fragrance, only by means of the flavoring and casing technology.Therefore, research all takes much count of tobacco industry for the cigarette flavors essence additive.
On the other hand, domestic all kinds of cigarette products, also exist as fragrance faint owe plentiful, odour characteristics not significantly, flue gas drying, pungent, sting larynx, quality defect in various degree such as sweet degree is not enough, comfort level is relatively poor, can not satisfy product intrinsic specification of quality.
VT (
Matthiola incanaL.) be life in 2 years of Cruciferae Matthiola incana or per nnial herb, claim careless sweet osmanthus, four peaches gram again, it is littoral to originate in European Mediterranean Sea, extensively cultivates at China's southern area at present.The VT seed oil content is high, is rich in linolenic acid in the seed oil, is a kind of new oilseed plant; Flower can supply to view and admire, and also can be used as medicine, and has the effect of stimulating the menstrual flow under rushing down; That the jasmine tea that gillyflower is processed has is clearing heat and detoxicating, the function of expelling phlegm for arresting cough, wet one's whistle moistening lung and removing abnormal flavor in oral cavity.Nearest research shows that the gillyflower odour component can suppress the effect of prostate cancer cell propagation.In recent years the research of VT is mainly concentrated on the research of cultivation, breeding and seed oil composition thereof.At present, do not see relevant report about the gillyflower extract as yet in the application of tobacco industry.
Summary of the invention
The purpose of this invention is to provide a kind of gillyflower extract and preparation method thereof and gillyflower extract as cigarette natural perfume Application of Additives.
The purpose of foregoing invention is to realize through following technical scheme:
1, a kind of gillyflower extract is characterized in that this gillyflower extract can use following method to extract
Obtain:
(1) fresh gillyflower is dried in the shade, pulverized 20 mesh sieves again and get the gillyflower powder;
(2) adopting simultaneously, distilling and extracting device carries out the while distillation extraction to the described gillyflower powder of step (1); Take by weighing the described gillyflower powder of step (1) 50g, place a round-bottomed flask of distilling and extracting device simultaneously, add 500 ~ 1500ml zero(ppm) water; Electric mantle with may command voltage heats; Control voltage is 200 V, and temperature is 100-110 ℃, keeps the water boiling to produce steam; Take by weighing 20 ml methylene dichloride and place another round-bottomed flask of distilling and extracting device simultaneously, with the water bath with thermostatic control heating, temperature stops heating 50 ℃ of continuous extractions 1 ~ 5 hour, uses 10 ml dichloromethane rinse distilling and extracting device simultaneously then;
(3) extraction liquid that will adorn in the round-bottomed flask of methylene dichloride is transferred in the separating funnel, shakes up the back standing demix, collects dichloromethane layer; Use Rotary Evaporators to steam the methylene dichloride that reclaims, till dripless is dripped to the Rotary Evaporators prolong, again liquid concentrator in the receiving flask is cooled to normal temperature, promptly get described gillyflower extract in 40 ℃ of condition underspins of normal pressure.
2, a kind of gillyflower preparation method of extract may further comprise the steps:
(1) fresh gillyflower is dried in the shade, pulverized 20 mesh sieves again and get the gillyflower powder;
(2) adopting simultaneously, distilling and extracting device carries out the while distillation extraction to the described gillyflower powder of step (1); Take by weighing the described gillyflower powder of step (1) 50g, place a round-bottomed flask of distilling and extracting device simultaneously, add 500 ~ 1500ml zero(ppm) water; Electric mantle with may command voltage heats; Control voltage is 200 V, and temperature is 100-110 ℃, keeps the water boiling to produce steam; Take by weighing 20 ml methylene dichloride and place another round-bottomed flask of distilling and extracting device simultaneously,,, stop heating, use 10 ml dichloromethane rinse distilling and extracting device simultaneously then 50 ℃ of continuous extractions 1 ~ 5 hour with the water bath with thermostatic control heating;
(3) extraction liquid that will adorn in the round-bottomed flask of methylene dichloride is transferred in the separating funnel, shakes up the back standing demix, collects dichloromethane layer; Use Rotary Evaporators to steam the methylene dichloride that reclaims, till dripless is dripped to the Rotary Evaporators prolong, again liquid concentrator in the receiving flask is cooled to normal temperature, promptly get described gillyflower extract in 40 ℃ of condition underspins of normal pressure.
3, technique scheme 1 described a kind of gillyflower extract is as cigarette natural perfume Application of Additives.
4, described gillyflower extract is as in the cigarette natural perfume Application of Additives, and the perfuming consumption that can also be this gillyflower extract is 0.005% ~ 0.1% of a cigarette shreds weight.
The applicant has carried out gc-flight time mass spectrum coupling (GC-TOF-MS) to the aroma component in the gillyflower extract and has analyzed:
Its GC conditions: chromatographic column is PE-35MS (30 m * 0.32 mm, 0.25 μ m); Injector temperature is 250 ℃; Carrier gas is high-purity helium, and flow velocity is 1ml/min; Splitting ratio is 20:1; Temperature programming: 50 ℃ of initial temperatures, keep 5 min, the speed with 10 ℃/min rises to 200 ℃ then, keeps 10 min, is warmed up to 250 ℃ with 10 ℃/min again and keeps 5 min; Sample size 2 μ l.
Its mass spectrum condition: the ionization mode is EI+; Electron energy is 70 eV; Ion source temperature is 220 ℃; Interface temperature is 220 ℃; Sweep limit is 40 ~ 400 amu (atomic mass units).Through MassLynx V4.1 chem workstation DPS, in NIST2008 and WILYL standard spectrum storehouse, retrieve, carry out spectrum elucidation in conjunction with pertinent literature, confirm its odor component.Quantitative analysis is tried to achieve the relative percentage composition of each odor component respectively through area normalization method.Analytical results sees table 1-table 5 for details:
Shown by table 1-table 5 analytical results: the massfraction that the chemical ingredients that aroma component identifies in the described gillyflower extract accounts for this gillyflower extract is 89.62%.Chemical ingredients to identifying is carried out classification analysis, finds wherein mainly to comprise terpenes (50.82% massfraction), alcohols (31.18% massfraction), ketone (2.90% massfraction), aldehydes (2.89% massfraction) and ester class (0.72% massfraction) compound.Wherein, the main volatile composition has: 2-beta-pinene (13.28% massfraction), isocurcumenol (10.90% massfraction), 3-carene (10.16% massfraction), the other alkene (4.53% massfraction) of beta waves, spathulenol (3.39% massfraction), β-cadinene (3.29% massfraction) etc.Described massfraction all is meant the massfraction that accounts for this gillyflower extract, and this gillyflower extract has its unique fragrance, and to contain a large amount of terpenes relevant with alcohols material with it.Show the inventive method proportioning and technology cleverly, made gillyflower extract contains more aroma component, helps the application of gillyflower extract as spice additive.
Odor component through the present invention is extracted effective aroma component from gillyflower is analyzed; And through the cigarette that adds the gillyflower extract being carried out sensory evaluating smoking's experiment; The result shows that the gillyflower extract that the present invention prepares can effectively improve and modify cigarette odor-absorbing as the cigarette flavors additive, and is remarkable in aspect effects such as soft flue gas, minimizing stimulations.
Embodiment:
The used equipment of the present invention is conventional commercially available equipment, and major equipment is a while distillation extraction appearance, available from Shanghai Yin Ze plant and instrument ltd, and the working method of distilling and extracting device when the use working method of this while distillation extraction appearance belongs to routine.Rotary Evaporators (model: R-210; The place of production: Switzerland).Reagent: methylene dichloride is an extraction agent, analytical pure, commercially available prod.
Embodiment 1:
Preparation gillyflower extract: (1) with fresh gillyflower dry in the shade to the water cut of gillyflower be 15% massfraction, pulverized 20 mesh sieves again and got the gillyflower powder; Described drying in the shade is that conventional article are placed on ventilated and the place that loses the sun goes slow.
(2) adopting simultaneously, the distillation extraction appearance carries out the while distillation extraction to the described gillyflower powder of step (1); Take by weighing the described gillyflower powder of step (1) 50g; Place a round-bottomed flask of distillation extraction appearance simultaneously, add 500ml zero(ppm) water, heat with the electric mantle of may command voltage; Control voltage is 200 V, and temperature is 100-110 ℃ and keeps the water boiling to produce steam; Take by weighing 20 ml methylene dichloride and place another round-bottomed flask of distilling and extracting device simultaneously,,, stop heating, use 10 ml dichloromethane rinse distillation extraction appearance simultaneously then 50 ℃ of continuous extractions 1 hour with the water bath with thermostatic control heating;
(3) extraction liquid that will adorn in the round-bottomed flask of methylene dichloride is transferred in the separating funnel, shakes up the back standing demix, collects lower floor's dichloromethane layer; Use Rotary Evaporators to steam the methylene dichloride that reclaims, till dripless is dripped to the Rotary Evaporators serpentine condenser, again liquid concentrator in the receiving flask is cooled to normal temperature, promptly get described gillyflower extract in 40 ℃ of condition underspins of normal pressure.
The application of gillyflower extract: getting above-mentioned gillyflower extract, to use massfraction be that 95% ethanol is made into the solution of concentration as 20mg/ ml; Use micro sprayer; Be sprayed at evenly respectively by the common process program by 0.005% or 0.05% or 0.1% perfuming amount (the perfuming amount is the weight percent of pipe tobacco) respectively that (the perfuming amount of 3 parts of pipe tobaccos is respectively 0.005% in the pipe tobacco of 3 parts of identical cigarette compositions of 100g; 0.05%, 0.1%), is mixed evenly, in the airtight climatic chamber that is stored in 22 ℃ ± 2 ℃ of temperature and relative humidity 60% ± 5%; Process the identical sample cigarette of auxiliary material specification behind 48 h and prop up, number as follows:
Carry out sensory evaluation according to GB5606.4-2005 " technical requirements of cigarette sense organ ", and to its sample cigarette Zhi Jinhang qualitative description targetedly.Zhi Jinhang smokes panel test to the sample cigarette, result such as following table 7:
Smell fragrant aspect; Sample 1#, 2#-, 3# compare with contrast 0#: send light fresh and sweet perfume (or spice), fruital and the banksia rose thoroughly, fragrance is soft, and with the fragrant harmony of tobacco; Along with the increase fragrance of VT extract addition has increase slightly on intensity, whole smell fragrant odor type also can slight change.
Sensory evaluating smoking result shows: sample 1#, 2#-, 3# compare with contrast 0#; Fresh and sweet note in the flue gas increases, and has light gillyflower characteristic note, and perfume quantity and flue gas concentration have lifting; Pungency decreases, and the sensation of Hui Tian is arranged on pleasant impression.Yet, along with the increase of addition, this group of Buddhists going together on a pilgrimage of tobacco there is inhibition slightly, also can bring residual on the pleasant impression slightly.Therefore, interpolation gillyflower extract can obviously improve and modify cigarette flavor, increases fresh and sweet note, makes the fragrant plentiful exquisiteness of cigarette, reduces stimulation, removes the gas of mixing, and makes the flue gas exquisiteness soft.
Embodiment 2:
Preparation gillyflower extract: remove step (1) with fresh gillyflower dry in the shade to the water cut of gillyflower be 17% massfraction; Step (2) fills and adds 1000ml zero(ppm) water in the round-bottomed flask of gillyflower powder; The round-bottomed flask that fills methylene dichloride is outside 50 ℃ of continuous extractions 3 hours; All the other steps are identical with embodiment 1, no longer repeat.
The application of gillyflower extract: identical with embodiment 1, effect is with embodiment 1.
Embodiment 3,
Preparation gillyflower extract: remove step (1) with fresh gillyflower dry in the shade to the water cut of gillyflower be 20% massfraction; Step (2) fills and adds 1500ml zero(ppm) water in the round-bottomed flask of gillyflower powder; The round-bottomed flask that fills methylene dichloride is outside 50 ℃ of continuous extractions 5 hours; All the other steps are identical with embodiment 1, no longer repeat.
The application of gillyflower extract: identical with embodiment 1, effect is with embodiment 1.
Claims (4)
1. gillyflower extract is characterized in that this gillyflower extract can use following method to extract and obtain:
(1) fresh gillyflower is dried in the shade, pulverized 20 mesh sieves again and get the gillyflower powder;
(2) adopting simultaneously, distilling and extracting device carries out the while distillation extraction to the described gillyflower powder of step (1); Take by weighing the described gillyflower powder of step (1) 50g; Place a round-bottomed flask of distilling and extracting device simultaneously, add 500 ~ 1500ml zero(ppm) water, heat with the electric mantle of may command voltage; Control voltage is 200 V, and temperature is 100-110 ℃ and keeps the water boiling to produce steam; Take by weighing 20 ml methylene dichloride and place another round-bottomed flask of distilling and extracting device simultaneously,,, stop heating, use 10 ml dichloromethane rinse distilling and extracting device simultaneously then 50 ℃ of continuous extractions 1 ~ 5 hour with the water bath with thermostatic control heating;
(3) extraction liquid that will adorn in the round-bottomed flask of methylene dichloride is transferred in the separating funnel, shakes up the back standing demix, collects dichloromethane layer; Use Rotary Evaporators to steam the dichloromethane layer of collecting, till dripless is dripped to the Rotary Evaporators prolong, again liquid concentrator in the receiving flask is cooled to normal temperature, promptly get described gillyflower extract in 40 ℃ of condition underspins of normal pressure.
2. gillyflower preparation method of extract may further comprise the steps:
(1) fresh gillyflower is dried in the shade, pulverized 20 mesh sieves again and get the gillyflower powder;
(2) adopting simultaneously, distilling and extracting device carries out the while distillation extraction to the described gillyflower powder of step (1); Take by weighing the described gillyflower powder of step (1) 50g, place a round-bottomed flask of distilling and extracting device simultaneously, add 500 ~ 1500ml zero(ppm) water; Electric mantle with may command voltage heats; Control voltage is 200 V, and temperature is 100-110 ℃, keeps the water boiling to produce steam; Take by weighing 20 ml methylene dichloride and place another round-bottomed flask of distilling and extracting device simultaneously,,, stop heating, use 10 ml dichloromethane rinse distilling and extracting device simultaneously then 50 ℃ of continuous extractions 1 ~ 5 hour with the water bath with thermostatic control heating;
(3) extraction liquid that will adorn in the round-bottomed flask of methylene dichloride is transferred in the separating funnel, shakes up the back standing demix, collects dichloromethane layer; Use Rotary Evaporators to steam the dichloromethane layer of collecting, till dripless is dripped to the Rotary Evaporators prolong, again liquid concentrator in the receiving flask is cooled to normal temperature, promptly get described gillyflower extract in 40 ℃ of condition underspins of normal pressure.
3. the described gillyflower extract of claim 1 is as cigarette natural perfume Application of Additives.
4. gillyflower extract according to claim 3 is characterized in that as cigarette natural perfume Application of Additives: the consumption of this gillyflower extract is 0.005%～0.1% of a cigarette shreds weight.
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Cited By (7)
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| CN103074159A (en) * | 2013-01-25 | 2013-05-01 | 安徽中烟工业有限责任公司 | Preparation method of indocalamus leaf volatile oil and application of volatile oil in cigarette |
| CN104814904A (en) * | 2015-05-18 | 2015-08-05 | 樊文花 | Phalaenopsis brightening mask and preparation method thereof |
| CN105154235A (en) * | 2015-07-15 | 2015-12-16 | 河南中烟工业有限责任公司 | Cigarette Chinese photinia perfume, and preparation method and application thereof |
| KR20160097767A (en) * | 2015-02-10 | 2016-08-18 | 주식회사 엘지생활건강 | Perfume composition |
| CN106957723A (en) * | 2016-10-13 | 2017-07-18 | 武汉黄鹤楼香精香料有限公司 | A kind of cigarette preparation method of gillyflower extract |
| WO2017183744A1 (en) * | 2016-04-20 | 2017-10-26 | 주식회사 엘지생활건강 | Aroma composition |
| CN107582599A (en) * | 2017-10-20 | 2018-01-16 | 程志鹏 | The method of antimicrobial component and the application of antimicrobial component are extracted in a kind of leaf from violet |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074159A (en) * | 2013-01-25 | 2013-05-01 | 安徽中烟工业有限责任公司 | Preparation method of indocalamus leaf volatile oil and application of volatile oil in cigarette |
| KR20160097767A (en) * | 2015-02-10 | 2016-08-18 | 주식회사 엘지생활건강 | Perfume composition |
| KR102114893B1 (en) | 2015-02-10 | 2020-05-25 | 주식회사 엘지생활건강 | Perfume composition |
| CN104814904A (en) * | 2015-05-18 | 2015-08-05 | 樊文花 | Phalaenopsis brightening mask and preparation method thereof |
| CN105154235A (en) * | 2015-07-15 | 2015-12-16 | 河南中烟工业有限责任公司 | Cigarette Chinese photinia perfume, and preparation method and application thereof |
| CN105154235B (en) * | 2015-07-15 | 2019-03-08 | 河南中烟工业有限责任公司 | A kind of cigarette Chinese photinia fragrance, preparation method and applications |
| WO2017183744A1 (en) * | 2016-04-20 | 2017-10-26 | 주식회사 엘지생활건강 | Aroma composition |
| CN109069386A (en) * | 2016-04-20 | 2018-12-21 | 株式会社 Lg 生活健康 | Spice composition |
| CN109069386B (en) * | 2016-04-20 | 2022-02-25 | 株式会社 Lg 生活健康 | Perfume composition |
| CN106957723A (en) * | 2016-10-13 | 2017-07-18 | 武汉黄鹤楼香精香料有限公司 | A kind of cigarette preparation method of gillyflower extract |
| CN107582599A (en) * | 2017-10-20 | 2018-01-16 | 程志鹏 | The method of antimicrobial component and the application of antimicrobial component are extracted in a kind of leaf from violet |
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Application publication date: 20120822 |