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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
water
spice
cigarette
distillation
nicotiana tabacum
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610581243.8A
Other languages
Chinese (zh)
Inventor
蓝洪桥
李斌
范坚强
章雪锋
陈小明
张峰
连芬燕
谢金栋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Tobacco Fujian Industrial Co Ltd
Original Assignee
China Tobacco Fujian Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Tobacco Fujian Industrial Co Ltd filed Critical China Tobacco Fujian Industrial Co Ltd
Priority to CN201610581243.8A priority Critical patent/CN106010796A/en
Publication of CN106010796A publication Critical patent/CN106010796A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/24Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/025Recovery 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

The invention belongs to the field of cigarette flavors and particularly relates to a preparation method of a flavor, comprising the following steps: (1), subjecting tobacco to vapor distilling to obtain distillate; (2), subjecting the distillate to oil-water separation to obtain oily substance and aqueous substance; (3) subjecting the aqueous substance to reverse osmosis treatment to obtain retention; (4), extracting the retention to obtain extract liquid, removing an extracting agent from the extract liquid to obtain extract; the extracting agent is selected from one or any of petroleum ether, cyclohexane, ethyl ether and ethyl acetate. The invention also relates to the obtained flavor and application thereof. The flavor prepared herein has low nicotine level, and by adding the prepared flavor to cigarettes, it is possible to reduce throat pressure during smoking and improving smoking comfort.

Description

The preparation method of a kind of spice, prepared spice and application thereof
Technical field
The invention belongs to tobacco aromatics using field, be specifically related to the preparation method of a kind of spice, further relate to Obtained spice and purposes.
Background technology
Vegetal natural perfume be from the flower of fragrant plant, grass, leaf, branch, dry, stem, root, skin, Really, the fragrant body goods that extract in the position such as seed, resin or balsam, great majority are oily or cream Shape, minority is resin or semisolid.Form according to them and preparation method, commonly referred to quintessence oil, tincture Agent, extractum, absolute oil, face cream or oleoresin, such as Flos Rosae Rugosae quintessence oil, red date tincture, Radix Glycyrrhizae extractum, White orchid face cream and ginger oil resin.
In the preparation method of vegetal natural perfume, steam distillation is common method.Water is steamed Vapour is passed through in the container filling plant material, and volatile ingredient with steam distillation out, is produced The component of natural perfume material is the volatility grease of armaticity, commonly referred to collectively as quintessence oil.Water vapour steams In evaporating, water mainly plays three kinds of effects, i.e. water and dissipates effect, hydrolysis and thermodynamic activity, water Mechanism is simply summarized as follows, and raw material surface wet water molecule is inside the cell tissue of raw material Infiltration water displacement quintessence oil or oligodynamical quintessence oil diffuse to form being total to of quintessence oil and water in water Boiling thing quintessence oil steams condensation oil-water separation quintessence oil with water vapour simultaneously.Except in boiling water Outside the plant material that main note composition easily dissolves, hydrolyzes or decomposes, most fragrant plants Quintessence oil is prepared with steam distillation.Steam distillation has three kinds of principal modes: water distillation, Distilling above water and steam distillation, the equipment of steam distillation mainly has distillating still, condenser and profit Separator three part.There is many deficiencies in existing steam distillation technique, such as, with extraction Extract the oily timesharing in watery thing, the organic extractant of a large amount of contaminative need to be used;Multiple steaming can destroy Or decompose thermally sensitive effective ingredient etc..
Reverse osmosis is with pressure differential as motive force, isolates the membrane separation technique of solvent from solution, To reach separation, extraction, purification or the purpose of concentration, it is in opposite direction with naturally osmotic, claims For reverse osmosis.
At present, a kind of new method preparing spice of still needing, to obtain a kind of novel fragrance product.
Summary of the invention
The present inventor creatively obtains the preparation method of a kind of spice, and the method is extracted by Nicotiana tabacum L. Going out spice, the nicotine content of obtained spice is relatively low.The present inventors have additionally discovered that and this spice is added In tobacco shred, it is fabricated to Medicated cigarette, it is possible to decrease the throat pressure during cigarette smoking, improves comfort level. Further, the inventive method can effectively collect the oil phase fragrance component in the watery thing of oil-water separation gained, Economic and environment-friendly.
First aspect present invention relates to the preparation method of a kind of spice, comprises the steps,
(1) Nicotiana tabacum L. is carried out steam distillation, obtain distillation;
(2) distillation is carried out oil-water separation, obtain grease and watery thing;
(3) watery thing is carried out reverse-osmosis treated, obtain trapped substance;
(4) trapped substance is extracted, is extracted liquid, remove the extractant in extract, It is extracted thing;Described extractant is selected from petroleum ether, hexamethylene, ether and ethyl acetate Plant or multiple.
In one embodiment, described spice is extract.
In one embodiment, the pressure of reverse-osmosis treated is 0.4-5MPa, is preferably 0.5-3MPa, more preferably 0.8MPa or 1.0MPa.
In one embodiment, the weight of reverse-osmosis treated gained trapped substance is watery thing weight 0.05-0.8, preferably 0.08-0.5, more preferably 0.1 or 0.088.
In one embodiment of first aspect present invention, also include, grease and extract are mixed Close, obtain the step of mixed extract.
In one embodiment, described spice is mixed extract.
In one embodiment, before mixing, also include grease except the step of water;Preferably, Water is removed with anhydrous sodium sulfate or anhydrous magnesium sulfate desiccant;Preferably, except the water time is 2-24 hour, It is more preferably 4 hours.
In one embodiment of first aspect present invention, including following 1) to 13) in any One or multinomial:
1) described Nicotiana tabacum L. is Nicotiana tabacum L.;Preferably, described Nicotiana tabacum L. is selected from Sanming City Youxi Nicotiana tabacum L., Tianjin bar One or more in cloth Wei Nicotiana tabacum L. and Dali auspicious cloud Nicotiana tabacum L.;
2) described steam distillation is selected from water distillation, distilling above water and direct steam distillation, For example, directly steam distillation;
3) temperature of described steam distillation is 90-120 DEG C, preferably 100 DEG C;
4) time of described steam distillation is 1-10 hour, preferably 2-8 hour, more preferably It is 2 hours, 3 hours or 6 hours;
5) steam valve aperture >=5% in wet distillation process, preferably 10-32%, more excellent Elect 10%, 15%, 20%, 25% or 30% as;6) the output speed of described distillation is 5-70kg/h, preferably 10-60kg/h, more preferably 12kg/h, 15kg/h, 30kg/h or 40kg/h;
7) described steam distillation is water at atmospheric pressure steam distillation;
8) temperature of described reverse-osmosis treated is not higher than 30 DEG C, preferably 10-30 DEG C, more preferably 10 DEG C, 25 DEG C or 30 DEG C;
9) time of described reverse-osmosis treated is 0.5-6 hour, preferably 1-4 hour, more preferably It is 1 hour, 2 hours, 3 hours or 4 hours;
10), in step (4), the addition of extractant is the 1/8-1/2 (W/W) of trapped substance, It is preferably 1/5-1/3 (W/W), more preferably 1/4 (W/W);
11), in step (4), trapped substance is repeatedly extracted, combining extraction liquid;Preferably, Extract 3-6 time, more preferably 4 times;Preferably, the weight of extraction use extractant is identical every time;
12) in step (4), by evaporative removal extractant, preferably rotary evaporation;More excellent Selection of land, evaporating temperature≤60 DEG C, evaporating pressure is 50-380mbar;It is further preferred that evaporation Temperature≤50 DEG C, evaporating pressure is 100-300mbar;It is further preferred that evaporating temperature is 30 DEG C or 35 DEG C, pressure is 210mbar or 250mbar;
13), in step (4), before removing extractant, also include extract except the step of water; Preferably, use anhydrous sodium sulfate or anhydrous magnesium sulfate desiccant except water;Preferably, except the water time For 2-24 hour, more preferably 4 hours.
Second aspect present invention relates to a kind of spice, by method described in any one of first aspect present invention Prepare.
In one embodiment of second aspect present invention, nicotine content≤1.8% in described spice (W/W), be 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)。
In one embodiment, described spice is tobacco aromatics using;Preferably, described tobacco aromatics using It is the perfume (or spice) for Nicotiana tabacum L., tobacco shred, stem, thin slice, filter tip, tipping paper, cigarette case or electronic cigarette Material.
In one embodiment, described spice is quintessence oil.
Third aspect present invention relates to a kind of cigarette compositions, and it comprises described in second aspect present invention Spice;Alternatively, carrier and adjuvant are also comprised.
In one embodiment, described cigarette compositions is for Nicotiana tabacum L., tobacco shred, stem, thin The compositions of sheet, filter tip, tipping paper, cigarette case or electronic cigarette.
Fourth aspect present invention relates to a kind of Medicated cigarette, and it comprises the spice described in second aspect present invention And/or the cigarette compositions described in third aspect present invention;Alternatively, tobacco shred is also comprised.
Fifth aspect present invention relates to the manufacture method of a kind of Medicated cigarette, including according to first party of the present invention Step that method described in any one of face prepares spice and the step that described spice is added in tobacco shred Suddenly;And/or include the step adding in tobacco shred by cigarette compositions described in third aspect present invention.
Sixth aspect present invention relates to spice described in second aspect present invention and/or third party of the present invention Cigarette compositions described in face is making tobacco product or during reducing drawing tobacco goods Throat pressure, the purposes improved in comfort level;Preferably, described tobacco product is Medicated cigarette.
The present invention quotes in full following document:
GB2635-92 flue-cured tobacco
GBT18771.2-2002 Nicotiana tabacum L. term part 2: Nicotiana tabacum L. processing, tobacco product.
In the present invention, if no special instructions, grease refers to what distillation obtained after oil-water separation Containing a small amount of or the oil reservoir of micro-moisture, the oil content in oil reservoir is less than 100%.
In the present invention, if no special instructions, watery thing refers to what distillation obtained after oil-water separation The water layer divided containing a small amount of or micro oil, the water content in water layer is less than 100%.
In the present invention, if no special instructions, Nicotiana tabacum L. refers to that Solanaceae is annual or perennial herb, addicted to Good class crop.This genus there are about more than 60 and plants, and is wild species mostly.Main cultispecies has Flos Carthami cigarette Grass and Folium Nicotianae rusticae.Both originates in South America, is all spontaneous amphidiploid.Flos Carthami cigarette Grass, also known as Nicotiana tabacum, is worldwide commodity production cigarette kind.Again because of modulator approach and plant source, District, cultivation step is different and forms polytype: flue-cured tobacco, burley tobaccos, Maryland, cigar, Fumigation, Turkish tobaccos, Dark sun-cured, Sun cured tobacco etc..Each type has again a lot of cultivar.Yellow Henbane is cultivated more with the former Soviet Union and India, and there is a small amount of cultivation on the ground such as Xinjiang, China, Gansu.This Henbane (N.alata Link and Otta) and powder blue smoke grass (N.glauca Graham) in genus are planted Plant for viewing and admiring.
In the present invention, if no special instructions, nicotine is also known as nicotine, and molecular formula is C10H14N2, It is a kind of plant alkaloid of containing of Nicotiana plant, is one of Nicotiana tabacum L. important component, property severe toxicity, little dose Amount can make central nervous excitation, breathes and strengthens, and blood pressure raises, and occurs depressed and neural time heavy dose of System is benumbed.
In the present invention, if no special instructions, water distillation refers to put in water raw material distill.
In the present invention, if no special instructions, distilling above water refers to be placed on raw material the sieve above the water surface Distill on plate.
In the present invention, if no special instructions, direct steam distillation refers to that the bottom distilling container sets Having air inlet, air inlet be passed through allogenic water steam, raw material is placed on the sieve plate above air inlet Distill.
The beneficial effect that the present invention obtains:
1, in spice prepared by the inventive method, nicotine content is low.
2, spice prepared by the inventive method adds to and makes Medicated cigarette in tobacco shred, can effectively reduce volume Pressure to throat during cigarette suction, improves the comfort level of suction.
3, the inventive method, can effectively collect the oil phase spice in the watery thing of oil-water separation gained and become Point, economic and environment-friendly.
Accompanying drawing explanation
In order to make present disclosure be more likely to be clearly understood, concrete below according to the present invention Embodiment also combines accompanying drawing, and the present invention is further detailed explanation, wherein
Fig. 1 is the flow chart of spice preparation method of the present invention.
Detailed description of the invention
Unless otherwise noted, following embodiment all uses following material and reagent:
Sanming City Youxi Nicotiana tabacum L., purchased from China Tobacco Corporation, tobacco leaf degree C3F/2010T;
Zimbabwe's Nicotiana tabacum L., purchased from China Tobacco Corporation, tobacco leaf degree CJOT/2010;
Dali auspicious cloud Nicotiana tabacum L., purchased from China Tobacco Corporation, tobacco leaf degree C3F/2010T;
Steam, can be provided with collection Thermal Power Co., Ltd by Xiamen state;
Ethyl acetate (A.R.), Chemical Reagent Co., Ltd., Sinopharm Group;
Ether (A.R.), Chemical Reagent Co., Ltd., Sinopharm Group;
Anhydrous sodium sulfate (A.R.), Chemical Reagent Co., Ltd., Sinopharm Group;
Reverse osmosis membrane is GE HWS RO 8040HR (salt rejection rate NaCl 99.5%).
Embodiment 1 prepares quintessence oil A
With reference to the flow process of Fig. 1, weigh 30kg Sanming City Youxi Nicotiana tabacum L., insert the extraction pot of distillating still In hanging basket, opening steam heating valve, valve opening is 20%, vapo(u)rizing temperature (steam temperature) Being 100 DEG C, water vapour is entered in distillating still by bottom, be fully contacted with Nicotiana tabacum L. material, disperse and Gasification, the steam (vapor) outlet derivation from distillating still top of the water of formation and the mixed vapour of volatile essential oil, Condensed device condenses, and obtains distillation, and the output speed of distillation is 40kg/h, and distillation time is 2 hours.
Distillation enters oil water separator and separates, and collects and obtains grease (the direct quintessence oil of Nicotiana tabacum L. A) 20g and watery thing 80kg.
Using first-stage reverse osmosis film, regulation membrane stack pressure is 0.8MPa, and cooling water temperature is 25 DEG C, Watery thing 80kg is concentrated into 8kg, is concentrated solution.Concentrated solution is added in extraction kettle, add Enter the extraction of ethyl acetate 2kg, be repeated 4 times, combining extraction liquid, add a certain amount of anhydrous Na2SO4 It is dried 4 hours, is filtered to remove desiccant.Using Rotary Evaporators, arranging thickening temperature is 35 DEG C, Vacuum is 210mbar, obtains oil 3g in extract, i.e. water after steaming ethyl acetate.
By oil 3g mix homogeneously in direct for Nicotiana tabacum L. quintessence oil 20g and water, prepare the quintessence oil A of 23g.
Quintessence oil A is added in tobacco shred, according to routine side according to the ratio of 0.01% (W/W) Legal system is made Medicated cigarette 1#.
Embodiment 2 prepares quintessence oil B
With reference to the flow process of Fig. 1, weigh 30kg Zimbabwe Nicotiana tabacum L., insert the extraction pot of distillating still In hanging basket, opening steam heating valve, valve opening is 15%, vapo(u)rizing temperature (steam temperature) Being 100 DEG C, water vapour is entered in distillating still by bottom, be fully contacted with Nicotiana tabacum L. material, disperse and Gasification, the steam (vapor) outlet derivation from distillating still top of the water of formation and the mixed vapour of volatile essential oil, Condensed device condenses, and obtains distillation, and the flow of distillation was at 30kg/ hour, and distillation time is 3.0 hour.Distillation enters oil water separator and separates, and collects grease (the direct quintessence oil of Nicotiana tabacum L.) 22g and watery thing 90kg.
Using first-stage reverse osmosis film, regulation membrane stack pressure is 1.0MPa, and cooling water temperature is 25 DEG C, Watery thing 90kg is concentrated into 8kg, is concentrated solution.Concentrated solution is added in extraction kettle, add Enter ether 2kg extraction, be repeated 4 times, combining extraction liquid, add a certain amount of anhydrous Na2SO4Dry Dry 4 hours, it is filtered to remove desiccant.Using Rotary Evaporators, arranging thickening temperature is 30 DEG C, Vacuum is 250mbar, obtains oil 4g in extract, i.e. water after being steamed by ether.
By oil 4g mix homogeneously in direct for Nicotiana tabacum L. quintessence oil 22g and water, prepare 26g quintessence oil B.
Quintessence oil B is added in tobacco shred, conventionally according to 0.01% (W/W) ratio It is fabricated to Medicated cigarette 2#.
Embodiment 3 prepares quintessence oil C
With reference to the flow process of Fig. 1, weigh 100kg Dali auspicious cloud Nicotiana tabacum L., insert carrying of distillating still Taking in tank hanging basket, open steam heating valve, valve opening is 10%, vapo(u)rizing temperature (water vapour Temperature) it is 100 DEG C, water vapour is entered in distillating still by bottom, be fully contacted with Nicotiana tabacum L. material, Dispersion and gasification, the water of formation and the mixed vapour of the volatile essential oil steam from alembic top go out Mouth is derived, and condensed device condenses, and obtains distillation, and the flow of distillation, at 12kg/ hour, steams The time of evaporating is 6.0 hours.Distillation enters oil water separator and separates, and (Nicotiana tabacum L. is straight to collect grease Connect quintessence oil) 80g and watery thing 72kg.
Using first-stage reverse osmosis film, regulation membrane stack pressure is 1.0MPa, and cooling water temperature is 25 DEG C, Watery thing 72kg is concentrated into 8kg, is concentrated solution.Concentrated solution is added in extraction kettle, add Enter ether 2kg extraction, be repeated 4 times, merge ether extraction liquid, add a certain amount of anhydrous Na2SO4 It is dried 4 hours, is filtered to remove desiccant.Using Rotary Evaporators, arranging thickening temperature is 30 DEG C, Vacuum is 250mbar, obtains oil 19g in extract, i.e. water after being steamed by ether.
By 19 mix homogeneously oily in direct for Nicotiana tabacum L. quintessence oil 80g and water, prepare the quintessence oil C of 99g.
Quintessence oil C is added in tobacco shred, according to routine side according to the ratio of 0.01% (W/W) Legal system is made Medicated cigarette 3#.
Comparative example 1
Weigh 30kg Sanming City Youxi Nicotiana tabacum L., insert in the extraction pot hanging basket of distillating still, open steam Heating valve, valve opening is 20%, and vapo(u)rizing temperature (steam temperature) is 100 DEG C, and water steams Vapour is entered in distillating still by bottom, is fully contacted with Nicotiana tabacum L. material, disperses and gasifies, the water of formation Deriving with the mixed vapour of the volatile essential oil steam (vapor) outlet from distillating still top, condensed device condenses, Obtaining distillation, the flow of distillation was at 40kg/ hour, and distillation time is 2.0 hours.Distillation Entrance oil water separator separates, and collects grease (the direct quintessence oil of Nicotiana tabacum L.) 19.8g and watery thing 80kg.
Watery thing 80kg is added in extraction kettle, adds the extraction of ethyl acetate 20kg, be repeated 4 times, Combining extraction liquid, adds a certain amount of anhydrous Na2SO4It is dried 4 hours, is filtered to remove desiccant. Using Rotary Evaporators, arranging thickening temperature is 35 DEG C, and vacuum is 210mbar, steams acetic acid Oil 2.6g in extract, i.e. water is obtained after ethyl ester.
By oil 2.6g mix homogeneously in direct for Nicotiana tabacum L. quintessence oil 19.8g and water, prepare 22.4g's Quintessence oil E.
Quintessence oil E is added in tobacco shred, according to routine side according to the ratio of 0.01% (W/W) Legal system is made Medicated cigarette I.
Comparative example 2
Nicotiana tabacum L. direct quintessence oil A embodiment 1 prepared is according to the ratio of 0.01% (W/W) Example is added in tobacco shred, is conventionally fabricated to Medicated cigarette II.
Experimental example 1
Use Agilent gas chromatograph-mass spectrometer 7890A-5975C to measure embodiment 1-3 and comparative example obtains To the direct quintessence oil of Nicotiana tabacum L., the nicotine content in oil and quintessence oil (A-C and E), result in water It is shown in Table 1.
Table 1 nicotine content (W/W)
The direct quintessence oil of Nicotiana tabacum L. Oil in water Quintessence oil
Embodiment 1 1.41% 1.01% 1.32%
Embodiment 2 1.52% 1.13% 1.48%
Embodiment 3 1.36% 1.03% 1.31%
Comparative example 1 1.43% 1.46% 1.45%
As shown in Table 1, compared with comparative example 1 method, in water prepared by the inventive method oil and Nicotine content in quintessence oil is lower.
Experimental example 2
According to standard GB/T 5606.4-2005, Medicated cigarette 1#~3# and Medicated cigarette I~II are carried out sense organ Quality is smoked panel test, and the results are shown in Table 2.
Table 2 aesthetic quality smoke panel test
As shown in Table 2, compared with comparative example 1 technique, spice prepared by the inventive method adds In Medicated cigarette, strength dispersion when making suction, throat pressure sense improves, and comfortableness improves.
And, compared with quintessence oil A direct with the Nicotiana tabacum L. that oil-water separation obtains, prepared by the inventive method Spice add in Medicated cigarette, during suction strength dispersion, comfortableness and throat pressure sense are further Improving, pleasant impression does not has astringent sense.
Obviously, above-described embodiment is only for clearly demonstrating example, and not to reality Execute the restriction of mode.For those of ordinary skill in the field, at the base of described above Can also make other changes in different forms on plinth.Here without also cannot be to all Embodiment give exhaustive.And the obvious change thus extended out or variation are still located Among the protection domain of the invention.

Claims (10)

1. a preparation method for spice, comprises the steps,
(1) Nicotiana tabacum L. is carried out steam distillation, obtain distillation;
(2) distillation is carried out oil-water separation, obtain grease and watery thing;
(3) watery thing is carried out reverse-osmosis treated, obtain trapped substance;
(4) trapped substance is extracted, is extracted liquid, remove the extractant in extract, It is extracted thing;
One or more in petroleum ether, hexamethylene, ether and ethyl acetate of described extractant.
Preparation method the most according to claim 1, wherein, the membrane stack pressure of reverse-osmosis treated Power is 0.4-5MPa, preferably 0.5-3MPa, more preferably 0.8MPa or 1.0MPa.
Preparation method the most according to claim 1, wherein, reverse-osmosis treated gained retains The weight of thing is the 0.05-0.8 of watery thing weight, preferably 0.08-0.5, more preferably 0.1 or 0.088.
Preparation method the most according to claim 1, it also includes, by grease and extraction Thing mixes, and obtains the step of mixed extract;
Preferably, before mixing, also include grease except the step of water;
It is highly preferred that remove water with anhydrous sodium sulfate or anhydrous magnesium sulfate desiccant;
It is highly preferred that except the water time is 2-24 hour, more preferably 4 hours.
Preparation method the most according to any one of claim 1 to 4, it is characterised in that as Lower 1) to 13) in any one or multinomial:
1) described Nicotiana tabacum L. is Nicotiana tabacum L.;Preferably, described Nicotiana tabacum L. is selected from Sanming City Youxi Nicotiana tabacum L., Tianjin bar One or more in cloth Wei Nicotiana tabacum L. and Dali auspicious cloud Nicotiana tabacum L.;
2) described steam distillation is selected from water distillation, distilling above water and direct steam distillation, For example, directly steam distillation;
3) temperature of described steam distillation is 90-120 DEG C, preferably 100 DEG C;
4) time of described steam distillation is 1-10 hour, preferably 2-8 hour, more preferably It is 2 hours, 3 hours or 6 hours;
5) steam valve aperture >=5% in wet distillation process, preferably 10-32%, more excellent Elect 10%, 15%, 20%, 25% or 30% as;
6) the output speed of described distillation is 5-70kg/h, preferably 10-60kg/h, more preferably For 12kg/h, 15kg/h, 30kg/h or 40kg/h;
7) described steam distillation is water at atmospheric pressure steam distillation;
8) temperature of described reverse-osmosis treated is not higher than 30 DEG C, preferably 10-30 DEG C, more preferably 10 DEG C, 25 DEG C or 30 DEG C;
9) time of described reverse-osmosis treated is 0.5-6 hour, preferably 1-4 hour, more preferably It is 1 hour, 2 hours, 3 hours or 4 hours;
10) addition of extractant is the 1/8-1/2 (W/W) of trapped substance, preferably 1/5-1/3 (W/W), more preferably 1/4 (W/W);
11) trapped substance is repeatedly extracted, combining extraction liquid;Preferably, extract 3-6 time, More preferably 4 times;Preferably, the weight of extraction use extractant is identical every time;
12) in step (4), by evaporative removal extractant, preferably rotary evaporation;More excellent Selection of land, evaporating temperature≤60 DEG C, evaporating pressure is 50-380mbar;It is further preferred that evaporation Temperature≤50 DEG C, evaporating pressure is 100-300mbar;It is further preferred that evaporating temperature is 30 DEG C or 35 DEG C, evaporating pressure is 210mbar or 250mbar;
13), in step (4), before removing extractant, also include extract except the step of water; Preferably, use anhydrous sodium sulfate or anhydrous magnesium sulfate desiccant except water;Preferably, except the water time For 2-24 hour, more preferably 4 hours.
6. a spice, is prepared by method according to any one of claim 1 to 5;
Preferably, nicotine content≤1.8% (W/W) in described spice, more 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);
Preferably, described spice is tobacco aromatics using;It is highly preferred that described tobacco aromatics using is for cigarette The spice of leaf, tobacco shred, stem, thin slice, filter tip, tipping paper, cigarette case or electronic cigarette;
Preferably, described spice is quintessence oil.
7. a cigarette compositions, it comprises the spice described in claim 6;
Alternatively, carrier and adjuvant are also comprised;
Preferably, described cigarette compositions be for Nicotiana tabacum L., tobacco shred, stem, thin slice, filter tip, The compositions of tipping paper, cigarette case or electronic cigarette.
8. a Medicated cigarette, it comprises the spice described in claim 6 and/or claim 7 institute The cigarette compositions stated;Alternatively, tobacco shred is also comprised.
9. a manufacture method for Medicated cigarette, including according to according to any one of claim 1 to 5 Step that method prepares spice and the step that described spice is added in tobacco shred;And/or include by Described in claim 7, cigarette compositions adds the step in tobacco shred to.
10. cigarette compositions described in spice described in claim 6 and/or claim 7 is making Tobacco product or reducing the throat pressure during drawing tobacco goods, improving in comfort level Purposes;Preferably, described tobacco product is Medicated cigarette.
CN201610581243.8A 2016-07-22 2016-07-22 Flavor preparation method, flavor prepared by preparation method and application of flavor Pending CN106010796A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610581243.8A CN106010796A (en) 2016-07-22 2016-07-22 Flavor preparation method, flavor prepared by preparation method and application of flavor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610581243.8A CN106010796A (en) 2016-07-22 2016-07-22 Flavor preparation method, flavor prepared by preparation method and application of flavor

Publications (1)

Publication Number Publication Date
CN106010796A true CN106010796A (en) 2016-10-12

Family

ID=57117178

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610581243.8A Pending CN106010796A (en) 2016-07-22 2016-07-22 Flavor preparation method, flavor prepared by preparation method and application of flavor

Country Status (1)

Country Link
CN (1) CN106010796A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108219958A (en) * 2018-03-06 2018-06-29 四川三联新材料有限公司 A kind of quick-fried pearl fragrance and preparation method thereof, quick-fried pearl and the application of quick-fried pearl
CN110305734A (en) * 2019-07-03 2019-10-08 亳州职业技术学院 A kind of extraction process of root of Dahurain angelica leaf volatile oil
CN114931234A (en) * 2022-05-19 2022-08-23 河北中烟工业有限责任公司 Tobacco source aroma substance, extraction method thereof and cigarette

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986760A (en) * 2006-12-22 2007-06-27 中国烟草总公司郑州烟草研究院 Water vapor extracted and refined sophora flower oil and its application in perfuming cigarette
CN102524934A (en) * 2012-01-12 2012-07-04 中国林业科学研究院林产化学工业研究所 Reconstructed tobacco coating liquid component-component group chemical kitchen combination, coupling preparation, and coupling preparation process
CN102559388A (en) * 2012-02-27 2012-07-11 浙江中烟工业有限责任公司 Essential oil of tobaccos as well as preparation method and application thereof to cigarettes
CN102907760A (en) * 2012-09-03 2013-02-06 上海聚华科技股份有限公司 Method for regulating chemical components of tobacco material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986760A (en) * 2006-12-22 2007-06-27 中国烟草总公司郑州烟草研究院 Water vapor extracted and refined sophora flower oil and its application in perfuming cigarette
CN102524934A (en) * 2012-01-12 2012-07-04 中国林业科学研究院林产化学工业研究所 Reconstructed tobacco coating liquid component-component group chemical kitchen combination, coupling preparation, and coupling preparation process
CN102559388A (en) * 2012-02-27 2012-07-11 浙江中烟工业有限责任公司 Essential oil of tobaccos as well as preparation method and application thereof to cigarettes
CN102907760A (en) * 2012-09-03 2013-02-06 上海聚华科技股份有限公司 Method for regulating chemical components of tobacco material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
单银花等: "玫瑰精油提取与纯化工艺研究进展", 《应用科技》 *
高宏建等: "水蒸汽蒸馏法提取烟草精油的研究", 《食品工业科技》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108219958A (en) * 2018-03-06 2018-06-29 四川三联新材料有限公司 A kind of quick-fried pearl fragrance and preparation method thereof, quick-fried pearl and the application of quick-fried pearl
CN110305734A (en) * 2019-07-03 2019-10-08 亳州职业技术学院 A kind of extraction process of root of Dahurain angelica leaf volatile oil
CN114931234A (en) * 2022-05-19 2022-08-23 河北中烟工业有限责任公司 Tobacco source aroma substance, extraction method thereof and cigarette

Similar Documents

Publication Publication Date Title
CN103525558B (en) Tea flower essence with fruity flavor characteristic and application thereof to cigarettes
CN105969524A (en) Composition and application of composition in cigarettes
CN103478885B (en) A kind of reconstituted tobacoo containing tea flower extract and preparation method thereof
CN105950298A (en) Preparation methods of tea hydrolat and tea essential oil
CN1875796A (en) Natural flavoring material with perfuming and health caring functions and application thereof
CN103478894A (en) Camellia extract composition with spicy fragrance and application of same to cigarettes
CN104544549A (en) Electronic cigarette smoke solution prepared through green tea leaf extract
CN103484248A (en) Tea flower essence with fresh and sweet characteristics, and application of essence in cigarettes
CN104544552A (en) Electronic cigarette smoke solution prepared through oolong leaf extract
CN106490674A (en) A kind of electronics tobacco tar of fresh breath and preparation method thereof
CN104544543A (en) Electronic cigarette smoke solution prepared through black tea leaf extract
CN103497837A (en) Tea flower essential oil, preparation method and application of essential oil to cigarette
CN106010796A (en) Flavor preparation method, flavor prepared by preparation method and application of flavor
CN105996116B (en) Contain the extra-strong tea just composition of object extract processed and its application
CN101194751A (en) Plants additive agent for tobacco and method for producing the same
CN106350225A (en) Preparation method and application of solid tree moss extract for cigarettes
CN107637858A (en) A kind of plant for improving water extraction and alcohol precipitation method extraction causes perfumery and extracting method and application
CN104544544A (en) Electronic cigarette smoke solution prepared through white tea leaf extract
CN110358630A (en) A kind of clear spicy tobacco aromaticss, preparation method and the application in cigarette
CN106148011A (en) The preparation method of a kind of cigarette radix valerianae extract and the application in Medicated cigarette thereof
CN106167739A (en) A kind of containing doing the microcapsule of extract of Folium Camelliae sinensis, Preparation Method And The Use
CN104544548A (en) Electronic cigarette smoke solution prepared through yellow tea leaf extract
CN103074159A (en) Preparation method of indocalamus leaf volatile oil and application of volatile oil in cigarette
CN102551195A (en) Extract of common coltsfoot flower extracted with petroleum ether and preparation method and application thereof
CN103653238A (en) Preparation method for carica papaya leaf extract and application for same in cigarettes

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20161012

RJ01 Rejection of invention patent application after publication