CN103497834A - Method for preparing dandelion absolute oil and application of dandelion absolute oil in cigarettes - Google Patents
Method for preparing dandelion absolute oil and application of dandelion absolute oil in cigarettes Download PDFInfo
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- CN103497834A CN103497834A CN201310496718.XA CN201310496718A CN103497834A CN 103497834 A CN103497834 A CN 103497834A CN 201310496718 A CN201310496718 A CN 201310496718A CN 103497834 A CN103497834 A CN 103497834A
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Abstract
The invention discloses a method for preparing dandelion absolute oil and an application of the dandelion absolute oil in cigarettes. The method for preparing the dandelion absolute oil comprises the following steps of dandelion raw material obtaining, drying and smashing, solution extracting, extract liquid concentration, cold storage and standing, dewaxing through centrifuge, liquor concentration, freezing and standing and separation, wherein the process of liquor concentration is conducted until no alcohol smell exists, and the absolute oil is obtained after separation. The dandelion absolute oil is applied to cigarette production as spice for the cigarettes. When the cigarettes are burnt and smoked, the smoke concentration is improved, flavor is rich, foreign flavor and stimulation are reduced, and the content of parts of harmful ingredients in cigarette smoke can be reduced. The method for preparing the dandelion absolute oil is characterized in that a refined preparation technology for dandelion extract is provided, through an appropriate separation purification technology, the dandelion extract undergoes refined processing, and therefore the product quality and the effects are improved obviously. The method has the reference value for refined processing of natural spice. The method for preparing the dandelion absolute oil and the application of the dandelion absolute oil in cigarettes have the advantages that production raw materials are abundant and easy to obtain, the production technology is simple and easy to operate, the product quality is stable and easy to control, the production cost is not high, and therefore practical production significance and value are achieved.
Description
Technical field
The present invention relates to plant milk extract precision work and application thereof, specifically taraxacum absolute oil and the application in tobacco thereof.The application of this technology does not change the existing complete processing of cigarette, can improve cigarette smoking quality, reduces the hazardness of cigarette.
Background technology
Along with the tar content of domestic cigarette product constantly reduces, the problems such as the decline of cigarette flavor amount, style and features reduction, comfortableness variation have been caused to some extent.For improving the overall quality of cigarette product, development effectiveness significantly, the novel fragrance of stay in grade or the processing that become more meticulous is a main solution route to traditional spices.This wherein, natural perfume becomes the emphasis of recent researches exploitation because of advantages such as its note is abundant, fragrance is true to nature, safety and environmental protections.
China has abundant vegetal natural perfume resource, but relatively backward owing to extracting complete processing, and Flavour resources only has part to be exploited, and a lot of vegetal natural perfumes can only be accomplished preliminary extraction, and product quality is more coarse.This not only causes the high-quality natural perfume of Chinese market in short supply, and has wasted to a certain extent the precious resources of China.Therefore, carry out the working research that becomes more meticulous of natural perfume, the industry closely bound up to food, daily use chemicals, tobacco etc. and essence and flavoring agent has realistic meaning.
Taraxacum is the composite family per nnial herb, and its aboundresources, widely distributed is a kind of medicine food dual purpose plant.In Chinese traditional medicine often with taraxacum (
toraxacum mongolicumhand. Mazz.), alkali ground taraxacum (
toraxacum borealisinensekitam.) or belong to the dry all herbal medicines of several plants together, be used for the treatment of the diseases such as the infectious diseases such as upper respiratory tract infection, parotitis, acute tonsillitis, mazoitis and Digestive tract.Modern pharmacological research shows that taraxacum has broad-spectrum antibacterial action, also has anti-inflammatory, the effect such as anti-oxidant, antitumor.The leaf of taraxacum and spend in contain abundant phenolic acid, be good free-radical scavengers; Contain multiple terpenoid and aldehyde, ketone compounds in taraxacum volatile oil, to improving cigarette smoking quality, certain effect is arranged.Main effective constituent being applied in cigarette products in the selective extraction taraxacum, can play the effect of falling evil, flavouring.
There is the researchist to add in pipe tobacco and roll into cigarette to reduce cigarette harm [Huang Huangui by the chopping of taraxacum herb or by its alcohol extract before, Deng. taraxacum health cigarette (P) the .2004 November 26 of cigarette capable of reducing harm, application number 200410052449.9].But add mode not easy to operate in concrete production technique the direct chopping of taraxacum herb, the root of taraxacum is difficult for cutting into silk, the bobbles that on seed, white pappus is formed is difficult for processing, the taraxacum blade is narrow, traditional tobacco leaf filament cutter is not exclusively applicable, and the taraxacum plant directly add the suction quality that may affect cigarette product.In addition, often foreign matter content is higher, quality stability is bad for the plant milk extract that relatively simple extensive extraction processing mode makes.Therefore, be necessary to Herba Taraxaci extract extracted, the further investigation of purifying process, exploitation is applicable to the product that becomes more meticulous that cigarette adds, and guarantees that stable preparation process, product quality are reliable.
Summary of the invention
Purpose of the present invention just is being based on existing Research foundation; adopt suitable extraction and separation and purification means; develop the cigaret additive become more meticulous---the taraxacum absolute oil; and accomplish scale production; put in some way in cigarette again; thereby improve suction quality and the sense organ comfort level of cigarette, reduce the content of part objectionable constituent in cigarette smoke.
The objective of the invention is to be achieved through the following technical solutions: a kind of preparation method of taraxacum absolute oil is to take taraxacum by following processing step, to make as raw material: taraxacum raw material → drying and crushing → solvent extraction → vat liquor concentrate → refrigerate standing → dewaxing by centrifuge → clear liquid be concentrated into without alcohol flavor → freezing standing → separate to obtain absolute oil.
Described taraxacum raw material is taraxacum, alkali ground taraxacum or dry herb or the over-ground part that belongs to several plants together, fully crushed after being dried to 20～40 orders.
In solvent extraction step, solvent for use is 60～95 %(V/V) edible ethanol, the mass ratio of solvent and raw material is controlled between 3:1～8:1.Adopt lixiviate under room temperature, each 5～7 days, lixiviate 3 times during extraction; Or adopt 60～75 ℃ of heating to extract, each 2～3 hours, extract 2 times; Or adopt ultrasonic wave, microwave-assisted extraction mode to be extracted.
In aforesaid method, after extracting solution is evaporated to paste containing amount and is about 5～15 %, quiet putting in 20～10 ℃ of environment of – until the plant wax is fully separated out, centrifugal or filtering and removing plant wax; Clear liquid further is concentrated into without the alcohol flavor, and now solution presents not miscible two-phase, and upper oil phase is thick opaque fluid extract, and lower floor's water is clarification Vandyke brown liquid; By this mixed solution, again in 20～10 ℃ of environment of Jing Zhi Yu –, after upper strata oily matter solidifies, the isolated for disposal lower aqueous solution obtains the taraxacum absolute oil.
For blackish green thickness oily liquid, there is blue or green perfume (or spice) and hay fragrance under the taraxacum absolute oil room temperature that adopts aforesaid method to prepare.The product acid number is 36.8～38.0, and sample is through 1:1(95% ethanol) detection refractive index n after dilution
d 20be about 1.35～1.45, relative density (25 ℃) is 0.88～0.90 g/cm
3.
By taraxacum absolute oil of the present invention after finite concentration ethanol or ethanol and mixed with propylene glycol solvent cut, perfuming link spray in production of cigarettes is added on cigarette shreds, while burning and sucking cigarette, can increase flue gas concentration, enrich note, increase sweet sense, wet one's whistle in addition, sharp phlegm and fall evil effect.Concrete usage ratio is: taraxacum absolute oil consumption is 0.001 of pipe tobacco weight～0.05 ‰, can be used alone or be deployed into essence with other spices to use.
After tested: the cigarette according to made of the present invention is compared with blank reference cigarette, and in cigarette mainstream flue gas, the content of grain phase free radical obviously reduces, and the reduction amplitude, between 20～30 %, and obviously alleviates the reaction of caused by smoking respiratory tract.
Characteristics of the present invention are to remove in traditional taraxacum crude extract by the processing that becomes more meticulous the impurity such as plant wax, tannin that the cigarette smoking mouthfeel had to side effect, active constituent-enriched, products obtained therefrom quality and effect have obvious lifting than taraxacum crude extract, can significantly improve the suction quality of cigarette, can reduce the content of the objectionable constituent such as free radical in cigarette smoke simultaneously, reduce the stimulation of smoking cigarette to the human body throat, without any side effects.And raw materials for production are rich and easy to get, production technique is simple to operation, and product with stable quality is easily controlled, and production cost is not high, therefore has more the meaning and value of actual production.
The accompanying drawing explanation
Fig. 1 taraxacum vat liquor (on), absolute oil (in) with the lower floor's water that separates absolute oil (under) the HPLC-DAD color atlas.
Fig. 2 taraxacum vat liquor (on), absolute oil (in) with the lower floor's water that separates absolute oil (under) the HPLC-ELSD color atlas.
Embodiment
Below in conjunction with example, the present invention is described further, but does not limit the present invention.
extract example 1
Get taraxacum over-ground part 0.8 kg of drying and crushing, with 70 ℃ of 95 % ethanol heating, extract twice, solid-liquid ratio is respectively 1:4 and 1:3, is total to obtain vat liquor 4.2 kg.Vat liquor is evaporated to 617 g, vacuum tightness Wei – 0.09 MPa, and bath temperature is no more than 50 ℃.Concentrated solution is refrigerated to standing 2 hours, with micron order filter membrane vacuum filtration, then clean filter residue with a small amount of ethanol, be total to obtain 699 g filtrates.Filtrate after dewaxing further is evaporated to without the alcohol flavor, now concentrated solution presents not miscible two-phase, be placed on sufficient standing in liquid distributing device, lower floor's water is clarification Vandyke brown liquid, upper oil phase is thick opaque fluid extract, but because upper and lower two phase liquid color is all very dark, naked eyes are difficult for observing phase boundary, and now directly separatory is had any problem.Then above-mentioned two phase liquid is put under 20 ℃ of environment of – after standing 2 hours, upper oil phase is solidified as solid-state, and it is liquid that lower floor's water is still, and now directly carrying out solid-liquid separation can be by the profit two-phase separately.Obtain taraxacum absolute oil 32 g.
extract example 2
Be purchased from dry herb 25 kg of taraxacum of Chinese Medicinal Materials Markets, be crushed to 20 order left and right; Adopt the steam heating pot for solvent extraction lixiviate at twice of volume 200 L, add respectively 5 times of raw material weights, the 80 % ethanol of 4 times, Heating temperature is stablized to timing after 60 ℃, each lixiviate 2 h; Be total to obtain vat liquor 196 kg.With concentrated vat liquor to 15 kg of external circulation evaporator, vacuum tightness Wei – 0.08 MPa, 40～45 ℃ of temperature.Concentrated solution is placed in to freezer (0～6 ℃) standing over night, uses at once the tripod pendulum type batch centrifugal dewaxing by centrifuge after taking-up, obtain dewaxed filtrate 12.8 kg.Filtrate adopts the Rotary Evaporators concentrating under reduced pressure of volume 20 L, Zhen Kong Du – 0.09 MPa, and temperature, not higher than 65 ℃, obtains approximately 4 kg of concentrated solution.Jiang freezing in 20 ℃ of freezers of its Zhi Yu –, after upper strata oily matter fully solidifies, the isolated for disposal lower aqueous solution, obtain approximately 1 kg of taraxacum absolute oil.
detection example
The sample that the example 2 of take makes is example, and when getting taraxacum vat liquor, taraxacum absolute oil and separating absolute oil, the aqueous solution of lower floor carries out respectively the high performance liquid chromatography detection, and chromatographic condition is as follows:
Chromatographic column: Waters XTerra C18 post (250 mm * 2.1 mm, 5 μ m); Adopt gradient elution: initial moving phase is acetonitrile: water=20:80 (V/V), and in 70 min, constant gradient is changed to acetonitrile: water=80:20 replaces with 100 % acetonitrile wash-outs afterwards; Flow velocity 1.0 mL/min; Column temperature is 30 ℃; Sample size: 5 μ L; Detector: the DAD ELSD that connects, DAD detects wavelength (λ): 420 nm; ELSD, atomizing gas (N
2) flow velocity: 0.62 mL/min, the spraying gun temperature: 45 ℃, evaporator temperature: 50 ℃.
Gained HPLC-DAD color atlas, HPLC-ELSD color atlas are as shown in Figure 1 and Figure 2.
From Fig. 1 and Fig. 2, can find out: through precision work such as dewaxing, oily water separations, process in the taraxacum absolute oil obtained and removed the water soluble component that most of polarity is larger (in color atlas, front 20 min go out the material at peak), enrichment the composition of the medium and small polarity of part, make product quality purer.
application example
The application test of taraxacum absolute oil of the present invention (take embodiment 2 product be example):
Take 0.010 g taraxacum absolute oil, add 95 % alcohol dilution to 1.000 g, mix.Adopt the perfuming cigarette injector to add 2 μ L taraxacum absolute oil diluents (the perfuming amount is 0.02 ‰) in every blank cigarette, put into constant temperature (22 ± 1 ℃) constant humidity (relative humidity 60 ± 2 %) more than case inner equilibrium 48 h.Separately get the blank cigarette of part, with the perfuming cigarette injector wherein every add 2 μ L 95 % ethanol, and under similarity condition more than balance 48 h, cigarette in contrast.After lower layer of water phased soln when adopting same method by isolated plant wax in production process and separating absolute oil dilutes, in every blank cigarette, inject 2 μ L.Smelt fragrant estimate and the cigarette organoleptic effect is smoked panel test by possessing 9 people more than provincial judging panel's qualification.
Analyses Methods for Sensory Evaluation Results shows: the taraxacum absolute oil has blue or green perfume (or spice) and hay perfume (or spice), adds in cigarette and makes flue gas sweet, full, the enrichment flue gas, enriches note, and throat's pungency reduces; The perfume of smelling of plant wax also has obvious wax gas except the green grass or young crops perfume (or spice) with taraxacum, and when cigarette burns and sucks, there is bitterness sense in oral cavity, and the residence time of bitter taste is very long, and oral cavity has residual; Lower floor's water while separating absolute oil, it smells fragrant blue or green gas will be weaker than absolute oil, and when cigarette burns and sucks, slightly thick, the flue gas of flue gas sinks, and that oral cavity has is residual, lingual surface prickling sensation is slightly strong.
Method according to GB/T 19609-2004, utilize automatic smoking machine to burn and suck cigarette, the glass fiber filter Fume collector is collected total particulate matter, collect the total particulate matter of 5 cigarette of the same race on each filter disc, carry out determining free radicals with electron spin resonance spectrometer (ESR), using the index of ESR strength of signal as the free radical amount.The granule phase substance ESR strength of signal that burns and sucks that contrasts cigarette of take is benchmark, and the sample cigarette is flue gas grain phase free radical scavenging activity than the minimizing value of contrast cigarette granule phase substance ESR strength of signal with the ratio that contrasts cigarette granule phase substance ESR strength of signal.After tested, in the cigarette mainstream flue gas of interpolation taraxacum absolute oil, a grain phase free radical scavenging activity reaches 28 %.
From above-mentioned evaluation result, can find out: Herba Taraxaci extract by suitable separation and purification means precision work, product quality obviously improves, in cigarette, the organoleptic effect effect also significantly promotes, and can remove cigarette mainstream flue gas middle part gradation phase free radical, there is " flavouring " effect of " harm reduction " simultaneously.
Claims (8)
1. the preparation method of a taraxacum absolute oil is characterized in that: be to take taraxacum by following processing step, to make as raw material: taraxacum raw material → drying and crushing → solvent extraction → vat liquor concentrate → refrigerate standing → dewaxing by centrifuge → clear liquid be concentrated into without alcohol flavor → freezing standing → separate to obtain absolute oil.
2. the preparation method of taraxacum absolute oil according to claim 1, it is characterized in that: described taraxacum raw material is taraxacum, alkali ground taraxacum or dry herb or the over-ground part that belongs to several plants together, fully crushed after being dried to 20～40 orders.
3. the preparation method of taraxacum absolute oil according to claim 1, it is characterized in that: in solvent extraction step, solvent for use is 60～95 %(V/V) edible ethanol, the mass ratio of solvent and raw material is controlled between 3:1～8:1.
4. according to the preparation method of the described taraxacum absolute oil of claim 1 or 3, it is characterized in that: adopt lixiviate under room temperature, each 5～7 days, lixiviate 3 times during extraction; Or adopt 60～75 ℃ of heating to extract, each 2～3 hours, extract 2 times; Or adopt ultrasonic wave, microwave-assisted extraction mode to be extracted.
5. the preparation method of taraxacum absolute oil according to claim 1, it is characterized in that: at the vat liquor enrichment step, it is 5～15 % that vat liquor is evaporated to paste containing amount.
6. the application of taraxacum absolute oil in cigarette prepared according to the described method of claim 1, it is characterized in that: by the taraxacum absolute oil after ethanol or ethanol and mixed with propylene glycol solvent cut, perfuming link spray in production of cigarettes is added on cigarette shreds, while burning and sucking cigarette, can increase flue gas concentration, enrich note, increase sweet sense, wet one's whistle in addition, sharp phlegm and fall evil effect.
7. the application of taraxacum absolute oil according to claim 6 in cigarette is characterized in that: taraxacum absolute oil consumption is 0.001 of pipe tobacco weight～0.05 ‰.
8. the application of taraxacum absolute oil according to claim 6 in cigarette is characterized in that: the taraxacum absolute oil can be used alone or is deployed into essence with other spices and uses.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103960771A (en) * | 2014-05-16 | 2014-08-06 | 吴泉忠 | Environmentally-friendly cigarette additive |
| CN104939291A (en) * | 2015-05-08 | 2015-09-30 | 湖北中烟工业有限责任公司 | Method for enhancing inherent aroma of tobaccos by aid of natural plants |
| CN109700068A (en) * | 2019-03-05 | 2019-05-03 | 云南中烟新材料科技有限公司 | A kind of floating oil method prepares the method and its application of sun-cured tobacco absolute oil |
| CN116268539A (en) * | 2023-04-24 | 2023-06-23 | 江苏浩丰生物科技有限公司 | Ampelopsis japonica extract, preparation method thereof and application thereof in tobacco industry |
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| CN109700068A (en) * | 2019-03-05 | 2019-05-03 | 云南中烟新材料科技有限公司 | A kind of floating oil method prepares the method and its application of sun-cured tobacco absolute oil |
| CN109700068B (en) * | 2019-03-05 | 2021-11-26 | 云南中烟新材料科技有限公司 | Method for preparing sun-cured tobacco absolute oil by oil bleaching method and application thereof |
| CN116268539A (en) * | 2023-04-24 | 2023-06-23 | 江苏浩丰生物科技有限公司 | Ampelopsis japonica extract, preparation method thereof and application thereof in tobacco industry |
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