CN105559145A - E-cigarette flavor and preparation method thereof - Google Patents
E-cigarette flavor and preparation method thereof Download PDFInfo
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- CN105559145A CN105559145A CN201510974399.8A CN201510974399A CN105559145A CN 105559145 A CN105559145 A CN 105559145A CN 201510974399 A CN201510974399 A CN 201510974399A CN 105559145 A CN105559145 A CN 105559145A
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Abstract
The invention discloses an e-cigarette flavor and a preparation method thereof. The e-cigarette flavor is a natural e-cigarette flavor prepared with a biological fermentation method in combination with a dry distillation flavor preparation technology. The preparation method comprises the steps as follows: different fruits and vegetables are mixed in proportion and fermented with yeast, and an enzyme extract solution is prepared. Meanwhile, fermentation residues are treated with the dry distillation technology and fractions with the strong curing aroma are obtained. Fresh fruits produce abundant secondary metabolites and a large number of aromatic substances with the fruit flavor after microbial fermentation. Fermented residues of fruits contain rich aroma-producing precursors such as fructose, protein and the like. A series of small-molecular aroma substances are produced during heating and dry distillation. The e-cigarette liquid flavor having the natural fruit aroma and the curing aroma can be obtained after these aroma components are mixed in a proper proportion.
Description
Technical field:
The present invention relates to a kind of electronic cigarette liquid additive formulations and addictive preparation method, belong to chemical industry preparing technical field.
Background technology:
Fruit ferment is a kind of is raw material with fruit, having abundant nutrition material and being rich in the fermented product of fruital smell through multiple probiotics fermention.Fruit can experience the chemical change of series of complex during the fermentation, consequently creates a large amount of fragrance matters after fermentation, and this fermented product has abundant fruital fragrance.Because fruit ferment is acknowledged as " natural ", and contain and enrich fruital.It is very have application prospect that this fermentoid is used as aromatising prods.
Electronic cigarette is always extensively concerned as the novel tobacco goods risen in recent years.Because it has heating non-burning characteristic, solving traditional tobacco is in the past the problem of a large amount of toxic and harmfuls produced in burning.Because of but a kind of comparatively healthy tobacco substitute products.Current electronic cigarette spices substantially still forms so that synthetic perfume is composite, and the application of natural perfume material is still less.In order to address this problem, the existing report making electronic cigarette spices of multiple natural plant extracts in recent years.Existing fruit extract makes the report of electronic cigarette spices at present.
CN102719313A discloses a kind of preparation method of fermented type fruit tobacco flavor.It is that cider and bananas juice are mixed rear formation composite fruit juice by weight 1: 0.5-2; Then add sugar and acid to composite fruit juice, regulate its pol and acidity, make the sugar in composite fruit juice be 11 ° ~ 12 °, acidity is 3.5 ~ 4.0; In deployed composite fruit juice in mass ratio 1000-100: 1 add active saccharomyces cerevisiae, mix and carry out alcoholic fermentation; After fermentation ends, cross and filter saccharomyces cerevisiae, in apparatus for acetic acid fermentation tank, carry out acetic fermentation, ferment complete fruit juice after filtering, be stored in airtight container.
CN104388191A discloses a kind of fruits tobacco aromatics, is made up of the method for following step: choosing of (1) fruit: get at least three kinds of fruit in watermelon, "Hami" melon, banana, pomegranate, dragon fruit, pears, apple, orange, shaddock, cumquat, lemon, grape, fig, hawthorn, mulberries, peach, loquat, Kiwi berry, lichee, persimmon, pawpaw, longan, wax-apple, panax ginseng fruit or mangosteen; (2) sterilization of fruit: cleaned by selected fruit clear water, dry, the ethanol with 75% carries out surface sterilization to fruit, then ultraviolet disinfection more than 30 minutes; (3) be cut into sheet or bulk after son being removed in the peeling and corning of fruits stoning after sterilization, in the fruit cut, mix at least one in white granulated sugar, brown sugar, honey or rock sugar and mix, then to load totally and in the container of sterilizing in advance, capping; The amount of described white granulated sugar, brown sugar, honey or rock sugar is 10 ~ 30% of fruit total amount; (4) fermentation of fruit: the container that fruit is housed being placed in temperature is 20 ~ 25 DEG C, humidity is spontaneous fermentation 1 ~ 3 month in the environment of 60 ~ 70%; (5) filter with double gauze after fermentation ends and remove fruit residue, collect filtrate under 8000 ~ 11000 revs/min of conditions centrifugal 15 minutes in centrifuges, get supernatant and carry out freeze drying, remove moisture, namely obtain required tobacco aromatics.
CN104544395A discloses a kind of plant fruit fermenation raw liquid, its preparation method: category-A fruit: get green plum 3-5 part, red bayberry 2-4 part, strawberry 2-3 part, raspberry 3-6 part, avocado 1-2 part cleans up and dry, ferment; Category-B fruit: get blueberry 5-6 part, mulberries 3-4 part, cherry 5-7 part, plum 3-5 part, prune 2-3 part, wax-apple 1-2 part cleans up and dry, add the maltose of 2 parts of weight, ferment; C class fruit: really 4-5 part, mangosteen 2-3 part, Kiwi berry 1-2 part are fermented to get butter; Plant: get the ginseng of artificial growth 4-5, matrimony vine, burdock with, the root of kudzu vine (peeling), ferment after cleaning up; Fermentation ends process: get category-A fruit ferment filtrate 5 parts, category-B fruit ferment filtrate 2 parts, C class fruit ferments 1 part, and plant fermentation filtrate 3 parts, mixes, and puts into airtight fermenter at once and continues fermentation 1 month, both obtained plant fruit fermenation raw liquid finished product.
CN102669658A discloses a kind of preparation method of plant enzyme food, it is characterized in that comprising following processing step: 1) select without rotting, the fresh fruit of free from extraneous odour, vegetables, bacterium mushroom, book on Chinese herbal medicine, the natural plant raw material of cereal and flower class, clean up, surface moisture is sloughed in drying, broken, section, stripping and slicing, or making beating enzymolysis, add the vinegar accounting for natural plant raw material weight 0 ~ 10% again, the salt of 0 ~ 10% and/or the glucide of 0 ~ 70%, then ferment, fermentation temperature controls less than 45 DEG C, ferment 0.5 ~ 36 month, plant enzyme base-material is converted into after fermentation, plant enzyme base-material is through infiltration, sedimentation, be separated and filter, obtain one time fermentation plant enzyme stoste or former sauce, 2) step 1 is got) the one time fermentation plant enzyme stoste that obtains or former sauce, add auxiliary material composite, auxiliary material is one or more mixture in compound sugar, vegetable active extract, trace element, natural complex, amino acid and dietary fiber, then ferment, fermentation temperature controls less than 45 DEG C, ferment 0.5 ~ 36 month, obtain secondary fermentation stoste or the storage of former sauce, 3) step 2 is got) the secondary fermentation stoste that obtains or former sauce storage filling and sealing obtain liquid or sauce shape plant enzyme food or composite plant enzyme food, or, freeze drying concentrated through low temperature obtains solid plant enzyme food or composite plant enzyme food.
But the electronic cigarette spices fragrance component made of single fruit extract is single, the fragrance made of various fruits mixture extract is inharmonious again, and ignores the utilization of fruit ferment remaining fermentation residue after extraction.How to make full use of the natural fruital of all kinds of fruit, the problem preparing appropriate electronic tobacco aromatics not can solve always.
Summary of the invention:
In order to overcome the above-mentioned technical problem existed in prior art, the present inventor, through further investigation and great many of experiments, provides following technical scheme.
On the one hand, the invention provides a kind of electronic cigarette spices, this electronic cigarette spices comprises natural fruit ferment and ferment residue cut.
Preferably, this electronic cigarette spices also comprises rich aromatic small-molecule substance.
Preferably, described fruit ferment is natural fruit and vegetables ferment.
On the other hand, provide the preparation method of described electronic cigarette spices, the method comprises the following steps:
(1) choose fresh fruit mixing by a certain percentage, after physical squeezing, leave standstill filtration obtain fruit mix extract, extract from fruit is inoculated bacterial classification, at normal temperatures sealed fermenting, obtain fruit ferment;
(2) by fruit ferment food-grade extraction into ethyl acetate, get extract and filter after the remaining bacterial classification of filtering through supermembrane, concentrate to obtain ferment concentrate;
(3) by extraction after aqueous phase dewater dry after obtain fermentation residue;
(4) by this residue through destructive distillation device destructive distillation, distillate gas respectively with water, ethanol, propane diols and glycerine absorb, collect each destructive distillation cut absorbing liquid;
(5) choose optimum destructive distillation cut absorbing liquid by test of smokeing panel test, it is mixed i.e. obtained electronic cigarette spices with ferment concentrate.
In a preferred embodiment, selected fresh fruit is respectively with weight ratio: apple: 10 ~ 60 parts, pears: 10 ~ 60 parts, grape: 10 ~ 60 parts, orange: 10 ~ 60 parts, red date: 10 ~ 60 parts.
Preferably, in mixed fruit extract, add saccharomycete, ferment.
Preferably, based on the weighing scale of mixed fruit extract, added saccharomycete is 0.2 ~ 2% weight.
In a preferred embodiment, the described fermentation of step (1) is 18 ~ 25 DEG C of bottom fermentations 7 ~ 15 days.
In still another aspect of the invention, additionally provide a kind of concentrate being rich in the small-molecule substance of fragrance, described concentrate can be used as electronic cigarette fragrance component, and this concentrate obtains by the following method:
(1) choose by a certain percentage fresh fruit clean, stoning, after physical squeezing, leave standstill filtration obtain fruit mix extract, add saccharomycete in the ratio of extract mass percent 0.2 ~ 2%, 18 ~ 25 DEG C of bottom fermentations 7 ~ 15 days, obtain fruit ferment concentrate;
(2) by fruit ferment food-grade extraction into ethyl acetate, extract filters away after remaining bacterial classification through supermembrane and concentrates to obtain ferment concentrate;
(3) aqueous phase after extraction is obtained fermentation residue after dewatering and drying;
(4) residue is added in destructive distillation tank, pass into nitrogen after vacuumizing, according to the heating rate of 5 DEG C/min, destructive distillation tank temperature is risen to 150 DEG C from normal temperature 25 DEG C, at 150 DEG C of insulation 1 ~ 1.5h, destructive distillation tank is warming up to 250 DEG C by aforementioned heating rate subsequently, at 250 DEG C of insulation 1 ~ 1.5h;
(5) after heating terminates, pass into nitrogen and take destructive distillation product out of destructive distillation tank, absorb with water, ethanol, propane diols and glycerine respectively, collect cut; Raw material and absorbing liquid mass ratio are 1: (1 ~ 4); The i.e. obtained concentrate being rich in the small-molecule substance of fragrance.
In another aspect of the invention, provide a kind of electronic cigarette liquid, it comprises electronic cigarette spices mentioned above 1 ~ 5%w, glycerine 5 ~ 20%w, propane diols 80 ~ 90%w, and all the other are flavoring essence, ethanol or water.
The content of described flavoring essence is preferably 0.01-0.5%w.
In an especially preferred embodiment, described flavoring essence is for as shown in the formula the compound shown in (I):
R
1, R
2, R
3, R
4, R
5be independently from each other C1-C6 alkyl, C1-C6 alkoxyl and H, and R
1, R
2, R
3, R
4, R
5in at least 3 be not hydrogen.Preferably, R
1, R
2, R
3, R
4, R
5be independently from each other C2-C5 alkyl, C2-C5 alkoxyl and H, and R
1, R
2, R
3, R
4, R
5in at least 4 be not hydrogen.
Compound shown in formula (I) is obtained through carrying out alkanoyl modification in amylene oxide ring α position by natural extract.Described alkanoyl modification can be undertaken by the alkanoyl method of this area routine.Such flavoring essence shown in formula (I) still belongs to the first time report in the art.
Described natural extract can extract from tobacco, vanilla, tealeaves etc.
The present inventor finds, adding of this flavoring essence, can the fragrance of strengthening electronic tobacco juice especially effectively, and can effectively offset the burning produced in electronic cigarette liquid use procedure, and general flavoring essence or unmodified simple natural extract are difficult to take into account this two kinds of performances.In addition, the use of this flavoring essence can improve the richness of tobacco aroma, and improves the property sent out thoroughly of fragrance.With generally use compared with essence such as Nicotiana tabacum extract, tea extract or medicinal extract, the sense organ comfort level of electronic cigarette can be significantly improved, such as according to GB5606.4-2005 carry out sensory evaluating smoking test time, the score value of fragrance hamony can improve more than 50%.Such effect is that those skilled in the art institute is unforeseeable.Infer its reason, may be that to reduce natural extract intrinsic overgenerous with penetrating odor because alkanoyl modification is carried out in α position, improve the compatibility with other composition in electronic cigarette liquid simultaneously.
Technique effect of the present invention is: the present invention proposes fruit ferment to be used for electronics tobacco tar preparation field first, has enriched and has only adopted fruit extract to prepare the method for electronics tobacco tar in the past.In addition, fruit ferment remaining fermentation residue after extraction has also been rich in a large amount of sugar, pectin and thalline.Wherein contain the materials such as abundant carbohydrate, pectin, protein.Usually can there is complicated chemical change in this kind of material, as the reactions such as pyrolysis, polymerization, condensation generate a large amount of Small molecular aroma substance, be the fragrance precursor material that in cigarette flavouring, a class is important when cigarette burning.But not there is the high-temp combustion cracking process of traditional cigarette due to electronic cigarette, this kind of material can not well be utilized up to now in electronic cigarette.The present invention is by retorting technique, and this kind of large molecule of at high temperature cracking obtains the Small molecular cut being rich in fragrance.By this step process, namely enrich spices fragrance, also taken full advantage of the rear residue of fermentation, saved resource.Fruit ferment remaining fermentation residue after extraction is carried out described destructive distillation do not report in the art or enlighten.
Detailed description of the invention:
The present invention is described further below in conjunction with embodiment, but does not limit the present invention.
Embodiment 1
Take fresh fruit in mass ratio: apple 50 parts, pears 50 parts, grape 30 parts, orange 30 parts.Clean, physical squeezing is carried out in stoning, filters precipitation after being left standstill by press juice.Get filtering liquid 20g, 1.0% added saccharomycete 0.2g in mass ratio, 25 DEG C of bottom fermentations 10 days.After fermentation ends, take out fruit ferment filter.Get 50ml filtrate and add 50 × 2ml food-grade extraction into ethyl acetate, extract is through supermembrane filtration sterilization.With after to obtain ferment concentrate through decompression low temperature is concentrated.Sterilization is boiled in stoste heating, dewaters after drying and obtain fermentation residue.Get 10g fermentation residue and put into the destructive distillation of destructive distillation tank, distillate gas and absorb with water, ethanol, propane diols and glycerine respectively, collect cut.
Embodiment 2
Take fresh fruit in mass ratio: apple: 50 parts, red date 50 parts, 30 parts, lemon, orange 30 parts.Clean, physical squeezing is carried out in stoning, filtering precipitation after being left standstill by press juice.Get filtering liquid 20g, 1.0% added saccharomycete 0.2g in mass ratio, 25 DEG C of bottom fermentations 10 days.After fermentation ends, take out fruit ferment filter.Get 50ml filtrate and add 50 × 2ml food-grade extraction into ethyl acetate, extract is through supermembrane filtration sterilization.With after to obtain ferment concentrate through decompression low temperature is concentrated.Sterilization is boiled in stoste heating, dewaters after drying and obtain fermentation residue.Get 10g fermentation residue and put into the destructive distillation of destructive distillation tank, distillate gas and absorb with water, ethanol, propane diols and glycerine respectively, collect cut.
Embodiment 3
Take fresh fruit in mass ratio: apple: 50 parts, red date 50 parts, 10 parts, lemon, orange 30 parts.Clean, physical squeezing is carried out in stoning, filtering precipitation after being left standstill by press juice.Get filtering liquid 20g, 1.0% added saccharomycete 0.2g in mass ratio, 25 DEG C of bottom fermentations 10 days.After fermentation ends, take out fruit ferment filter.Get 50ml filtrate and add 50 × 2ml food-grade extraction into ethyl acetate, extract is through supermembrane filtration sterilization.With after to obtain ferment concentrate through decompression low temperature is concentrated.Sterilization is boiled in stoste heating, dewaters after drying and obtain fermentation residue.Get 10g fermentation residue and put into the destructive distillation of destructive distillation tank, distillate gas and absorb with water, ethanol, propane diols and glycerine respectively, collect cut.
Electronic cigarette liquid spices embodiment prepared is deployed into electronics tobacco tar respectively, is smoked panel test by six perfumers.Smoking result sees the following form 1:
As seen from Table 1, (1) is added with ethanol absorption cut electronic cigarette liquid in smokeing panel test and showing is the highest with the electronic cigarette liquid score of adding ferment concentrate, and mean scores is respectively 85.1 and 82.8.Smoked panel test by perfumer and describe binding analysis this table and find to add water to absorb the sweet soapy feeling of electronic cigarette liquid of cut heavier, the electronic cigarette liquid adding ethanol absorption cut has strong baking fragrant, be added with propane diols respectively to compare without obviously changing with without the electronic cigarette liquid added with the electronic cigarette liquid that glycerine absorbs cut, the electronic cigarette liquid adding ferment concentrate has strong fruital.This may be only absorbed by the water owing to resolving into Small molecular water-soluble saccharides containing a large amount of undecomposed fructose class when heating destructive distillation in fermentation residue, causes water to absorb the sweet soapy feeling of cut obvious.And the protein substance in residue generates Small molecular heterocyclic aroma substance through destructive distillation, this kind of material is absorbed by ethanol, thus creates and significantly toasts perfume (or spice).Due to the water-soluble and oil-soluble ingredients in cut respectively by water and ethanol absorb, then when making lyosoption with propane diols and glycerine, without excess fraction.So without significant change after causing latter two cut to add.
(2) the present inventor is according to the smoking result of table 1, does to smoke panel test contrasting, the results are shown in following table 2 with the electronic cigarette liquid that the electronic cigarette liquid and nothing that are added with ferment concentrate and ethanol fraction add:
As can be seen from Table 2, the electronic cigarette liquid being added with ethanol absorption cut and ferment concentrate can obviously improve electronic cigarette liquid aroma quality and pleasant impression.Such technique effect is that those skilled in the art institute is unforeseeable.
The open the present invention of this written description use-case, comprises optimal mode, and also enables those skilled in the art manufacture and use the present invention.Of the present inventionly the scope of granted patent can be defined by the claims, and other example that those skilled in the art expect can be comprised.If other example this has the structural element of the literal language not differing from claims, if or other example this comprises and the equivalent structure element of the literal language of claims without substantial differences, then other example this is intended to be within the scope of claims.Can not cause under inconsistent degree, be incorporated herein by reference to by all references part of reference herein.
Claims (10)
1. an electronic cigarette spices, this electronic cigarette spices comprises natural fruit ferment and ferment residue cut.
2. electronic cigarette spices according to claim 1, this electronic cigarette spices also comprises rich aromatic small-molecule substance.
3., according to the electronic cigarette spices of claim 1 or 2, wherein said fruit ferment is natural fruit and vegetables ferment.
4. the preparation method of the electronic cigarette spices according to aforementioned any one of claim, the method comprises the following steps:
(1) choose fresh fruit mixing by a certain percentage, after physical squeezing, leave standstill filtration obtain fruit mix extract, extract from fruit is inoculated bacterial classification, at normal temperatures sealed fermenting, obtain fruit ferment;
(2) by fruit ferment food-grade extraction into ethyl acetate, get extract and filter after the remaining bacterial classification of filtering through supermembrane, concentrate to obtain ferment concentrate;
(3) by extraction after aqueous phase dewater dry after obtain fermentation residue;
(4) by this residue through destructive distillation device destructive distillation, distillate gas respectively with water, ethanol, propane diols and glycerine absorb, collect each destructive distillation cut absorbing liquid;
(5) choose optimum destructive distillation cut absorbing liquid by test of smokeing panel test, it is mixed i.e. obtained electronic cigarette spices with ferment concentrate.
5. preparation method according to claim 4, wherein selected fresh fruit is respectively with weight ratio: apple: 10 ~ 60 parts, pears: 10 ~ 60 parts, grape: 10 ~ 60 parts, orange: 10 ~ 60 parts, red date: 10 ~ 60 parts.
6. the preparation method according to claim 4 or 5, wherein adds saccharomycete, ferments in mixed fruit extract.
7. preparation method according to claim 6, wherein based on the weighing scale of mixed fruit extract, added saccharomycete is 0.2 ~ 2% weight.
8. the preparation method according to claim 5 or 6, wherein the described fermentation of step (1) is 18 ~ 25 DEG C of bottom fermentations 7 ~ 15 days.
9. be rich in a concentrate for the small-molecule substance of fragrance, described concentrate can be used as electronic cigarette fragrance component, and this concentrate obtains by the following method:
(1) choose by a certain percentage fresh fruit clean, stoning, after physical squeezing, leave standstill filtration obtain fruit mix extract, add saccharomycete in the ratio of extract mass percent 0.2 ~ 2%, 18 ~ 25 DEG C of bottom fermentations 7 ~ 15 days, obtain fruit ferment concentrate;
(2) by fruit ferment food-grade extraction into ethyl acetate, extract filters away after remaining bacterial classification through supermembrane and concentrates to obtain ferment concentrate;
(3) aqueous phase after extraction is obtained fermentation residue after dewatering and drying;
(4) residue is added in destructive distillation tank, pass into nitrogen after vacuumizing, according to the heating rate of 5 DEG C/min, destructive distillation tank temperature is risen to 150 DEG C from normal temperature 25 DEG C, at 150 DEG C of insulation 1 ~ 1.5h, destructive distillation tank is warming up to 250 DEG C by aforementioned heating rate subsequently, at 250 DEG C of insulation 1 ~ 1.5h;
(5) after heating terminates, pass into nitrogen and take destructive distillation product out of destructive distillation tank, absorb with water, ethanol, propane diols and glycerine respectively, collect cut; Raw material and absorbing liquid mass ratio are 1: (1 ~ 4); The i.e. obtained concentrate being rich in the small-molecule substance of fragrance.
10. an electronic cigarette liquid, it comprises electronic cigarette spices 1 ~ 5%w that according to any one of electronic cigarette spices according to any one of claim 1-3 or claim 4-8 prepared by method, glycerine 5 ~ 20%w, propane diols 80 ~ 90%w, all the other are flavoring essence, ethanol or water.
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| CN106617266A (en) * | 2016-12-19 | 2017-05-10 | 深圳瀚星翔科技有限公司 | Electronic cigarette smoke solution |
| CN107397250A (en) * | 2017-08-16 | 2017-11-28 | 湖北中烟工业有限责任公司 | A kind of preparation method of electronics tobacco tar |
| CN108618192A (en) * | 2017-03-22 | 2018-10-09 | 赖彦君 | A kind of 15 are formulated electronic cigarette tobacco tar and preparation method thereof |
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| CN113397205A (en) * | 2021-06-15 | 2021-09-17 | 谢同昌 | Preparation method of cigarette containing shaddock active ingredients |
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Cited By (8)
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| CN108618192A (en) * | 2017-03-22 | 2018-10-09 | 赖彦君 | A kind of 15 are formulated electronic cigarette tobacco tar and preparation method thereof |
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| CN111296886A (en) * | 2019-12-10 | 2020-06-19 | 颐中（青岛）实业有限公司 | Dry distillation spice and application thereof in novel tobacco products |
| CN111849632A (en) * | 2020-07-24 | 2020-10-30 | 云南养瑞科技集团有限公司 | Deep processing method of natural tobacco flavor raw material and application of natural tobacco flavor raw material in novel tobacco |
| CN113397205A (en) * | 2021-06-15 | 2021-09-17 | 谢同昌 | Preparation method of cigarette containing shaddock active ingredients |
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