CN107467712A - It is a kind of with the tobacco sauce additive of antibacterial activity and its application - Google Patents
It is a kind of with the tobacco sauce additive of antibacterial activity and its application Download PDFInfo
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- CN107467712A CN107467712A CN201710628091.7A CN201710628091A CN107467712A CN 107467712 A CN107467712 A CN 107467712A CN 201710628091 A CN201710628091 A CN 201710628091A CN 107467712 A CN107467712 A CN 107467712A
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- tobacco
- tobacco sauce
- cigarette
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention discloses a kind of with the tobacco sauce additive of antibacterial activity and its application.The additive is by glycerine, benzyl carbinol, phenethyl acetate, vanillic aldehyde, fanesol, and phenylethyl propionate and rose flavones S are made after mixing in proportion.Described rose flavones S, it is the isolated neoflavonoid from the waste residue after production Rosa Damascana, is named as：The methoxy flavone of 6 methylol of 2' hydroxyls 7, there is following structural formula：The additive of addition 5% 8%, the putrid and deteriorated of tobacco sauce are effectively suppressed in tobacco sauce, can significantly extend the shelf-life of tobacco sauce.Throat's comfortableness of cigarette smoking can also be significantly improved, reduce stimulation of the smoking to human body throat.Increase the exquisiteness of flue gas and sweet sense, flue gas becomes submissiveer by throat and when entering nasal cavity.Simple production process of the present invention, raw material sources are extensive, and cost is low, improve the added value of rose processing, comprehensively utilize waste resource, have a good application prospect.
Description
Technical field
The invention belongs to technical field of tobacco chemistry, is specifically related to a kind of tool prepared using new flavone compound
There is the tobacco sauce additive of good antibacterial activity.Meanwhile the application the invention further relates to the additive in production of cigarettes.
Background technology
Tobacco sauce is the important auxiliary material of production of cigarettes, and rational charging can promote flavor and taste, the bad gas of reduction or place to go
Taste and excitant, make tobacco leaf limber up and reduce make it is broken.Conventional tobacco sauce has sugar, fruity inspissated juice, radix glycyrrhizae, extracting tobacco
Thing, plant extract, synthesis or natural perfume material, humectant etc..Tobacco sauce moisture is very high, and many in feed liquid
Composition is microorganism growth and breeds required nutritional ingredient, is very easy to cooperating microorganisms and occurs putrid and deteriorated.In feed liquid
Storage, transport and processing use during may go bad, so not only have a strong impact on that product safety and quality are steady
It is qualitative, while also brought irremediable economic loss with enterprise.Therefore, the putrid and deteriorated prevention and control of tobacco sauce are very heavy
Will.
Yunnan tobacco product fragrance is sufficient, strong, and strength is moderate, and suction satisfaction is strong.But and brand is competed outside the province
Compare, due to the otherness of consumer taste hobby, some consumers are slightly short of there is also comfortableness is aspirated, excitant, done
Dry sense distinct issues.
The content of the invention
A kind of prepared in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide using new flavone compound
Tobacco sauce additive with good antibacterial activity.
It is putrid and deteriorated in suppression tobacco sauce the present invention also aims to provide described additive, and improve cigarette
Application in smoking quality.
The purpose of the present invention is achieved by the following technical programs.
Unless otherwise indicated, percentage of the present invention is percetage by weight.
A kind of tobacco sauce additive with antibacterial activity, is made up of the raw material of following weight parts：Glycerine 96.9~
98.8 parts, 0.5~1.5 part of benzyl carbinol, 0.2~0.5 part of phenethyl acetate, 0.1~0.2 part of vanillic aldehyde, fanesol 0.1~
0.2 part, 0.1~0.2 part of phenylethyl propionate and rose flavones-S0.2~0.5 part；It is required after each raw material is well mixed
Additive；
Wherein, described rose flavones-S, it is isolated flavonoid from the waste residue after production Rosa Damascana
Thing, there is following structural formula：
The compound is light yellow gum thing, is named as：2'- hydroxyl -6- methylol -7- methoxy flavones, English are entitled：
2'-hydroxy-6-hydroxymethyl-7-dimethoxy-flavone, popular name are：Rose flavones-S.
The method for preparing the 2'- hydroxyls -6- methylol -7- methoxy flavones, comprises the following steps：
(1) sample extraction：Waste residue after production Rosa Damascana is extracted 2~5 times with solvent supersonic, it is molten used in extraction every time
The weight of agent is 2~6 times of waste residue, each 30~60 minutes extraction times, merges extract solution, filtering, filtrate decompression is concentrated into
Just there is sediment precipitation, stand 20~60 minutes, filter out sediment and obtain sample extracting solution；
(2) MCI decolourizes：MCI posts on sample extracting solution, collect efflux and be concentrated under reduced pressure into medicinal extract；
(3) silica gel column chromatography：By silica gel column chromatography on medicinal extract, dress post silica gel is 200~250 mesh, the weight of used silica gel
For 3~10 times of medicinal extract weight；Gradient elution is carried out with chloroform-acetone solution, the volume proportion of chloroform-acetone solution is respectively
20:1、9:1、8:2、7:3、6:4 and 1:1, gradient eluent and the concentration of each gradient are collected, is monitored through TLC, merges identical portion
Point；
(4) high performance liquid chromatography separation：By 6:4 chloroform-acetone affords eluent using high performance liquid chromatography point
From purifying, UV-detector Detection wavelength is 365nm, collects 32.2min chromatographic peak, is evaporated after repeatedly adding up, produces the change
Compound.
Further, in step (1), described solvent is the aqueous acetone solution of volumetric concentration 70%~100%, volume is dense
The ethanol water of degree 70%~100% or the methanol aqueous solution of volumetric concentration 70%~100%.
In step (3), medicinal extract is first molten with the acetone or methanol of 1.5~3 times of amounts of medicinal extract weight before upper silica gel column chromatography
Solution, then with 100~150 mesh silica gel mixed samples of 0.8~1.2 times of medicinal extract weight amount, loading afterwards.
In step (3), during gradient elution, no component outflow is eluted to per secondary, i.e., is not had after solvent evaporated in cucurbit
There is component residue, then change next gradient.
In step (4), described high performance liquid chromatography separation purifying be using volumetric concentration as 32%~45% methanol-water
Solution is mobile phase, and 15~25mL/min of flow velocity, with 21.2 × 250mm, 5 μm of ZorbaxPrepHT GF reverse phase preparative columns are
Stationary phase, UV-detector Detection wavelength are 365nm, each 0.5~1.0mL of sample introduction, collect 32.2min chromatographic peak, repeatedly
It is evaporated after cumulative.
Used in tobacco sauce by 5%~8% addition of feed liquid weight, the putrid and deteriorated of tobacco sauce is effectively pressed down
System, it can significantly extend the shelf-life of tobacco sauce.
Specifically effect is：The control feed liquid of additive is not used in second day stored, pH value starts to be decreased obviously, and 7
Rate of change is up to 20.14% after it.After additive using the present invention, storing 30 days in, pH value does not change substantially, rate of change
Between 0.03%~1.50%.According to Food Microbiology standard method, bacterium, mould, yeast and large intestine in feed liquid are detected
The quantity situation of flora.The tobacco sauce of additive of the present invention be with the addition of after storing 30 days, bacterium, mould, yeast and large intestine
The quasi-microorganism of flora 4 does not all detect；Artificial smell distinguishes that result shows not having significant changes with the former state of new production.And it is not added with this
After storing 7 days, yeast, coliform, total number of bacteria and total number of molds substantially increase the control feed liquid of invention additive, increase
Amount is at least more than 10 times.Artificial smell distinguishes that result has also indicated that obvious tart flavour and sour taste, and the former state of new production are shown
Write change.
Meanwhile described additive can also be obviously improved the suction quality of cigarette.
The tobacco sauce that with the addition of additive of the present invention is used to prepare cigarette, method be by tobacco quality 0.5%~
1.0% is equably sprayed on pipe tobacco, then after the common process link such as perfuming, steel wire storage, rolls into cigarette, according to
GB5606.4-2005 standards carry out sensory evaluation, and evaluation result shows：The tobacco sauce that with the addition of additive of the present invention is used to roll up
In cigarette, it can also increase the exquisiteness of flue gas and sweet sense, flue gas becomes submissiveer by throat and when entering nasal cavity, and cigarette is taken out
Comfortableness is inhaled to get a promotion.
Compared with prior art, the present invention has advantage following prominent：
1st, the additive prepared by the present invention is used in tobacco sauce by quality 5%-8% additions, the corruption of tobacco sauce
Lose to go bad and be effectively suppressed, can significantly extend the shelf-life of tobacco sauce.
2nd, after the additive is added in tobacco sauce, cloud production cigarette suction comfort can be alleviated to a certain extent and slightly owed
Lack, excitant, dry sensation distinct issues, and cloud production cigarette style is coordinated, and does not have after addition to the style and features of cigarette product
Influence.The exquisiteness of flue gas and sweet sense can also be increased, flue gas becomes submissiveer by throat and when entering nasal cavity, and cigarette is taken out
Comfortableness is inhaled to get a promotion.
3rd, the Additive Production technique is simple, and each composition is well mixed in the ratio of setting.Additive it is main into
It is glycerine to divide, and accounts for the 96.9%~98.8% of formula rate, needs to add the 1%~2% of pipe tobacco weight during production of cigarettes
Propane diols or glycerine as humectant；And addition of the tobacco sauce in pipe tobacco is generally less than 2%.Additive of the present invention is
Make to add in feed liquid by 10% high addition, then 2% feed liquid is added in pipe tobacco, the propane diols being introduced into cigarette also only accounts for
19.4/10000ths~the 19.8 of pipe tobacco weight, will not be to the main chemistry of Cigarette well below the amount that glycerine can be added in pipe tobacco
Composition damages.In addition to principal component glycerine, benzyl carbinol, phenethyl acetate, vanillic aldehyde, fanesol, propionic acid in additive
The micro constitutents such as phenethyl ester, rose flavones-S are respectively provided with prominent antibacterial effect.
4th, the compound rose flavones-S in additive of the present invention, separated from the waste residue after production Rosa Damascana
Arrive, raw material sources are very extensive, and cost is low；Waste resource can be comprehensively utilized by producing the compound, improve the attached of rose processing
It is value added to have important practical significance.The compound on animals is nontoxic, safe to use, and compound shows good antibacterial activity,
More than 95% is reached to the bacteriostasis rate of bacterium, mould, yeast and the quasi-microorganism of coliform 4；And compound structure letter
It is single, if also it is easily achieved using process for artificial, and production cost is low.
Brief description of the drawings
Fig. 1 be flavone compound of the present invention carbon-13 nmr spectra (13C NMR)；
Fig. 2 be flavone compound of the present invention proton nmr spectra (1H NMR)；
Fig. 3 is the related figures of crucial HMBC of flavone compound of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with drawings and Examples pair
The present invention is described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.In the examples where no specific technique or condition is specified, according to document in the art described by skill
Art or condition are carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, are that can pass through purchase
Buy the conventional products of acquisition.
Embodiment 1 --- compound rose flavones-S preparation
The waste residue sample source after Rosa Damascana is produced in hotan, kind is Damask Rose.Take waste residue
100kg, with 95% ethanol 300L ultrasonic extractions 4 times, each 30min.Merge extract solution, filtering, filtrate decompression are concentrated into body
Long-pending 1/4；Stand, filter out sediment, filter out MCI posts on the solution after precipitation and decolourize, be concentrated under reduced pressure to give 6.5kg medicinal extract；Take
Medicinal extract 650g adds 1.2kg acetone dilution in medicinal extract, then adds 100 mesh silica gel 700g and mixes sample, with 200 mesh silica gel 2.5g
Post is filled, mixes upper prop after sample；It is respectively 20 with volume ratio:1,9:1,8:2,7:3,6:4 and 1:1 chloroform-acetone mixing is organic molten
Agent gradient elution, gradient eluent, concentration are collected, is monitored through TLC, merges identical part, obtains 6 part A-F, wherein,
To the sample E (6 being collected into:4) part 155g, then using 38% methanol as mobile phase, flow velocity 20ml/min, 21.2 × 250mm,
5 μm of ZorbaxPrepHT GF reverse phase preparative columns are stationary phase, and UV-detector Detection wavelength is 365nm, each sample introduction
1.0mL, 32.2min chromatographic peak is collected, be evaporated after repeatedly adding up, produce compound rose flavones-S.
The identification of compound structure：The structure of prepared compound is identified by the following method：
HRESI-MS shows that its quasi-molecular ion peak is 321.0744 [M+Na]+(calculated value 321.0739), with reference to1H NMR
Composed with DEPT and determine that its molecular formula is C17H14O5, degree of unsaturation 11.
Hydroxyl (3439), carbonyl (1670) and aromatic ring (1615,1452 and 1421cm are shown in infrared spectrum-1) resonance
Absworption peak.And ultraviolet spectra there may be aromatic ring structure in 210,262,365nm have absorption maximum to also illustrate that compound.
Compound1H and13C H NMR spectroscopies (such as table 1, Fig. 1 and Fig. 2) show that it contains 17 carbon and 14 hydrogen, including 1
1,2,4,5- quaternary phenyl ring (C-5~C-10, H-5, H-8), 1 dibasic phenyl ring of 1,2- (C-1'~C-6', H-3'~
H-6'), 1 α, beta-unsaturated carbonyl (C-2, C-3, C-4, H-3), 1 methylol (δC63.5q δH4.65s), 1 methoxyl group
(δC55.9 δH3.81s), and 1 phenolic hydroxyl group (δH11.24s).According to typical 2 phenyl ring, alpha, beta-unsaturated carbonyl and
Double bond signal, it is flavone compound that can speculate compound.According to H-3 and C-2, C-4, C-10, C-1 ', H-5 and C-4, C-9,
C-10, H-8 and C-9, C-10, and H-6 ' (such as Fig. 3) related to C-2 HMBC may further confirm that compound is flavonoids knot
Structure.
After the parent of compound determines, remaining substituent, methylol, methoxyl group and phenolic hydroxyl group can be considered taking on flavones
Dai Ji.Methoxyl group hydrogen (δ can be observed in (such as Fig. 3) in the HMBC spectrums of compoundH3.81) with and C-7 (δC163.2) HMBC phases
Close, can speculate that the methoxyl group is substituted in C-7 positions respectively；According to methylol hydrogen H2-7(δH4.65) and C-5, C-6, C-7 HMBC phases
Close, it can be verified that methyl is substituted in C-6 positions；According to phenolic hydroxyl group hydrogen (δH11.24) it is related to C-1 ', C-2 ', C-3 ' HMBC, it can demonstrate,prove
Real phenolic hydroxyl group is substituted in C-2 ' positions.Proton signal (H-5, δ on typical phenyl ring in additionH7.01s；H-8,δH6.53s；H-3 ', δH6.91(d)7.6；H-4 ', δH7.29(t)7.6；H-5 ', δH6.88(t)7.6；H-6 ', δH7.71 (d) 7.6) also susceptible of proof sheet
The B rings of invention chromocor compound are that 6,7- positions two substitute, and C rings are that 2'- positions are monosubstituted.So far, the structure of compound is determined,
Compound nomenclature is：2'- hydroxyl -6- methylol -7- methoxy flavones, popular name are：Rose flavones-S.
Infrared, the ultraviolet and mass spectrometric data of compound：Purple light composes (methanol), λmax(logε)210(4.73)、262
(4.35)、365(3.82)nm；Infrared spectrum (pressing potassium bromide troche)：νmax3439、1670、1615、1552、1421、1402、
1369、1168、1062、853、763cm-1；1H and13C NMR datas (500 and 125MHz, (C5D5N), it is shown in Table -1；Cation mould
Formula ESIMS m/z335 [M+Na]+；Positive ion mode HRESIMS m/z321.0744 [M+Na]+(calculated value 321.0739,
C17H14NaO5)。
The compounds of this invention of table 1.1H NMR and13C NMR datas (C5D5N)
| No. | δC(mult.) | δH(mult,J,Hz) | No. | δC(mult.) | δH(mult,J,Hz) |
| 2 | 163.0s | 1′ | 116.5s | ||
| 3 | 109.1d | 6.73s | 2′ | 155.1s | |
| 4 | 177.0s | 3′ | 116.8d | 6.91(d)7.6 | |
| 5 | 130.1d | 7.01s | 4′ | 131.6d | 7.29(t)7.6 |
| 6 | 122.6s | 5′ | 121.1d | 6.88(t)7.6 | |
| 7 | 163.2s | 6′ | 128.7d | 7.71(d)7.6 | |
| 8 | 105.0d | 6.53s | 7′ | 63.5t | 4.65s |
| 9 | 154.6s | -OMe-7 | 55.9q | 3.81s | |
| 10 | 116.5s | Ar-OH | 11.24s |
Additive prepares embodiment 1
Additive in the present embodiment is prepared from the following materials：Glycerine 98.00%, benzyl carbinol 1.00%, acetic acid benzene
Ethyl ester 0.30%, vanillic aldehyde 0.15%, fanesol 0.15%, phenylethyl propionate 0.15%, rose flavones-S0.25%.Respectively into
It is additive samples 1 to divide after being uniformly mixed in proportion obtained shallow yellow transparent solution.
The additive samples 1 of addition 6% in the tobacco sauce of Yunnan brand cigarette.Storage 30 days after, manually smell distinguish,
PH value determines and microorganism detection result shows that the feed liquid does not occur to go bad；And compare in feed liquid 5 days that just there occurs obvious
It is rotten.
The tobacco sauce that with the addition of additive samples 1 is equably sprayed on pipe tobacco by the 0.6% of tobacco quality, then passed through
After the common process link such as perfuming, steel wire storage, cigarette is rolled into, sensory evaluation is carried out according to GB5606.4-2005 standards.Evaluation knot
Fruit shows：The tobacco sauce that with the addition of additive of the present invention is used in cigarette, can improve throat's comfortableness of cigarette smoking, reduce
Stimulation of the smoking to human body throat, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and the change into nasal cavity
Must be submissiveer, the suction comfortableness of cigarette gets a promotion.
Additive prepares embodiment 2
Additive in the present embodiment is prepared from the following materials：Glycerine 97.4%, benzyl carbinol 1.2%, acetic acid benzene second
Ester 0.4%, vanillic aldehyde 0.2%, fanesol 0.2%, phenylethyl propionate 0.2%, rose flavones-S0.4%.Each composition press than
Example, which is uniformly mixed, obtains additive samples 2.
The additive samples 2 of addition 5% in the tobacco sauce of Yunnan brand cigarette.Storage 30 days after, manually smell distinguish,
PH value determines and microorganism detection result shows that the feed liquid does not occur to go bad；And compare in feed liquid 5 days that just there occurs obvious
It is rotten.
The tobacco sauce that with the addition of additive samples 2 is equably sprayed on pipe tobacco by the 0.5% of tobacco quality, then passed through
After the common process link such as perfuming, steel wire storage, cigarette is rolled into, sensory evaluation is carried out according to GB5606.4-2005 standards.Evaluation knot
Fruit shows：The tobacco sauce that with the addition of additive of the present invention is used in cigarette, can improve throat's comfortableness of cigarette smoking, reduce
Stimulation of the smoking to human body throat, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and the change into nasal cavity
Must be submissiveer, the suction comfortableness of cigarette gets a promotion.
Additive prepares embodiment 3
Additive in the present embodiment is prepared from the following materials：Glycerine 97.7%, benzyl carbinol 0.8%, acetic acid benzene second
Ester 0.4%, vanillic aldehyde 0.2%, fanesol 0.2%, phenylethyl propionate 0.2%, rose flavones-S0.5%.Each composition press than
Example, which is uniformly mixed, obtains additive samples 3.
The additive samples 3 of addition 7% in the tobacco sauce of Yunnan brand cigarette.Storage 30 days after, manually smell distinguish,
PH value determines and microorganism detection result shows that the feed liquid does not occur to go bad；And compare in feed liquid 5 days that just there occurs obvious
It is rotten.
The tobacco sauce that with the addition of additive samples 3 is equably sprayed on pipe tobacco by the 0.8% of tobacco quality, then passed through
After the common process link such as perfuming, steel wire storage, cigarette is rolled into, sensory evaluation is carried out according to GB5606.4-2005 standards.Evaluation knot
Fruit shows：The tobacco sauce that with the addition of additive of the present invention is used in cigarette, can improve throat's comfortableness of cigarette smoking, reduce
Stimulation of the smoking to human body throat, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and the change into nasal cavity
Must be submissiveer, the suction comfortableness of cigarette gets a promotion.
Additive prepares embodiment 4
Additive in the present embodiment is prepared from the following materials：Glycerine 97.25%, benzyl carbinol 1.40%, acetic acid benzene
Ethyl ester 0.45%, vanillic aldehyde 0.18%, fanesol 0.18%, phenylethyl propionate 0.18%, rose flavones-S0.36%.Respectively into
Divide to be uniformly mixed in proportion and obtain additive samples 4.
The additive samples 4 of addition 6% in the tobacco sauce of Yunnan brand cigarette.Storage 30 days after, manually smell distinguish,
PH value determines and microorganism detection result shows that the feed liquid does not occur to go bad；And compare in feed liquid 5 days that just there occurs obvious
It is rotten.
The tobacco sauce that with the addition of additive samples 4 is equably sprayed on pipe tobacco by the 0.8% of tobacco quality, then passed through
After the common process link such as perfuming, steel wire storage, cigarette is rolled into, sensory evaluation is carried out according to GB5606.4-2005 standards.Evaluation knot
Fruit shows：The tobacco sauce that with the addition of additive of the present invention is used in cigarette, can improve throat's comfortableness of cigarette smoking, reduce
Stimulation of the smoking to human body throat, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and the change into nasal cavity
Must be submissiveer, the suction comfortableness of cigarette gets a promotion.
Additive prepares embodiment 5
Additive in the present embodiment is prepared from the following materials：Glycerine 97.70%, benzyl carbinol 1.20%, acetic acid benzene
Ethyl ester 0.25%, vanillic aldehyde 0.20%, fanesol 0.20%, phenylethyl propionate 0.15%, rose flavones-S0.30%.Respectively into
Divide to be uniformly mixed in proportion and obtain additive samples 5.
The additive samples 5 of addition 8% in the tobacco sauce of Yunnan brand cigarette.Storage 30 days after, manually smell distinguish,
PH value determines and microorganism detection result shows that the feed liquid does not occur to go bad；And compare in feed liquid 5 days that just there occurs obvious
It is rotten.
The tobacco sauce that with the addition of additive samples 5 is equably sprayed on pipe tobacco by the 0.6% of tobacco quality, then passed through
After the common process link such as perfuming, steel wire storage, cigarette is rolled into, sensory evaluation is carried out according to GB5606.4-2005 standards.Evaluation knot
Fruit shows：The tobacco sauce that with the addition of additive of the present invention is used in cigarette, can improve throat's comfortableness of cigarette smoking, reduce
Stimulation of the smoking to human body throat, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and the change into nasal cavity
Must be submissiveer, the suction comfortableness of cigarette gets a promotion.
Additive prepares embodiment 6
Additive in the present embodiment is prepared from the following materials：Glycerine 98.05%, benzyl carbinol 0.6%, acetic acid benzene second
Ester 0.35%, vanillic aldehyde 0.20%, fanesol 0.15%, phenylethyl propionate 0.15%, rose flavones-S0.50%.Each composition
It is uniformly mixed in proportion and obtains additive samples 6.
The additive samples 6 of addition 7% in the tobacco sauce of Yunnan brand cigarette.Storage 30 days after, manually smell distinguish,
PH value determines and microorganism detection result shows that the feed liquid does not occur to go bad；And compare in feed liquid 5 days that just there occurs obvious
It is rotten.
The tobacco sauce that with the addition of additive samples 6 is equably sprayed on pipe tobacco by the 0.7% of tobacco quality, then passed through
After the common process link such as perfuming, steel wire storage, cigarette is rolled into, sensory evaluation is carried out according to GB5606.4-2005 standards.Evaluation knot
Fruit shows：The tobacco sauce that with the addition of additive of the present invention is used in cigarette, can improve throat's comfortableness of cigarette smoking, reduce
Stimulation of the smoking to human body throat, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and the change into nasal cavity
Must be submissiveer, the suction comfortableness of cigarette gets a promotion.
Additive prepares embodiment 7
Additive in the present embodiment is prepared from the following materials：Glycerine 98.9%, benzyl carbinol 1.5%, acetic acid benzene second
Ester 0.5%, vanillic aldehyde 0.2%, fanesol 0.2%, phenylethyl propionate 0.2%, rose flavones-S0.50%.Each composition press than
Example, which is uniformly mixed, obtains additive samples 7.
The additive samples 7 of addition 5% in the tobacco sauce of Yunnan brand cigarette.Storage 30 days after, manually smell distinguish,
PH value determines and microorganism detection result shows that the feed liquid does not occur to go bad；And compare in feed liquid 5 days that just there occurs obvious
It is rotten.
The tobacco sauce that with the addition of additive samples 7 is equably sprayed on pipe tobacco by the 0.5% of tobacco quality, then passed through
After the common process link such as perfuming, steel wire storage, cigarette is rolled into, sensory evaluation is carried out according to GB5606.4-2005 standards.Evaluation knot
Fruit shows：The tobacco sauce that with the addition of additive of the present invention is used in cigarette, can improve throat's comfortableness of cigarette smoking, reduce
Stimulation of the smoking to human body throat, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and the change into nasal cavity
Must be submissiveer, the suction comfortableness of cigarette gets a promotion.
Sensory evaluating smoking tests：
The cigarette sample that embodiment 1-7 is prepared to additive carries out sensory evaluating smoking by GB5606.4-2005 method, smokes panel test
It the results are shown in Table -2.It can be seen that by the smoking result of table 2, total point of embodiment 1-7 is above control sample more than 91.Should
After additive is added in tobacco sauce, it can also increase the exquisiteness of flue gas and sweet sense, flue gas is by throat and into nasal cavity
Become submissiveer, the suction comfortableness of cigarette gets a promotion.Illustrate benzyl carbinol, phenethyl acetate, perfume (or spice) in additive of the present invention
The micro constitutents such as Lan Su, fanesol, phenylethyl propionate, rose flavones-S also have when adding appropriate and changed in addition to antibacterial action
The effect of kind cigarette smoking quality.
Table 2, embodiment 1-7 cigarette sample smoking results
Claims (7)
1. a kind of tobacco sauce additive with antibacterial activity, is made up of the raw material of following weight parts：Glycerine 96.9~98.8
Part, 0.5~1.5 part of benzyl carbinol, 0.2~0.5 part of phenethyl acetate, 0.1~0.2 part of vanillic aldehyde, 0.1~0.2 part of fanesol,
0.1~0.2 part of phenylethyl propionate and rose flavones-S0.2~0.5 part；By the addition as required after well mixed of each raw material
Agent；
Wherein, described rose flavones-S, it is isolated flavone compound from the waste residue after production Rosa Damascana, has
There is following structural formula：
The compound is light yellow gum thing, is named as：2'- hydroxyl -6- methylol -7- methoxy flavones, English are entitled：2'-
hydroxy-6-hydroxymethyl-7-dimethoxy-flavone。
2. additive according to claim 1, it is characterised in that：Described 2'- hydroxyl -6- methylol -7- methoxyl groups are yellow
The preparation method of ketone, comprises the following steps：
(1) sample extraction：Waste residue after production Rosa Damascana is extracted 2~5 times with solvent supersonic, extracts solvent for use every time
Weight is 2~6 times of waste residue, each 30~60 minutes extraction times, merges extract solution, filtering, filtrate decompression, which is concentrated into, just to be had
Sediment separates out, and stands 20~60 minutes, filters out sediment and obtain sample extracting solution；
(2) MCI decolourizes：MCI posts on sample extracting solution, collect efflux and be concentrated under reduced pressure into medicinal extract；
(3) silica gel column chromatography：By silica gel column chromatography on medicinal extract, dress post silica gel is 200~250 mesh, and the weight of used silica gel is leaching
3~10 times of cream weight；Gradient elution is carried out with chloroform-acetone solution, the volume proportion of chloroform-acetone solution is respectively 20:
1、9:1、8:2、7:3、6:4 and 1:1, gradient eluent and the concentration of each gradient are collected, is monitored through TLC, merges identical part；
(4) high performance liquid chromatography separation：By 6:It is pure using high performance liquid chromatography separation that 4 chloroform-acetone affords eluent
Change, UV-detector Detection wavelength is 365nm, collects 32.2min chromatographic peak, is evaporated after repeatedly adding up, produces the compound.
3. additive according to claim 2, it is characterised in that：In step (1), described solvent is volumetric concentration 70%
The first of~100% aqueous acetone solution, the ethanol water of volumetric concentration 70%~100% or volumetric concentration 70%~100%
Alcohol solution.
4. additive according to claim 2, it is characterised in that：In step (3), medicinal extract is before upper silica gel column chromatography, first
Dissolved with the acetone or methanol of 1.5~3 times of amounts of medicinal extract weight, then with 100~150 mesh of 0.8~1.2 times of amount of medicinal extract weight
Silica gel mixed sample, afterwards loading.
5. additive according to claim 2, it is characterised in that：In step (4), described high performance liquid chromatography separation is pure
Change condition is：Using the methanol aqueous solution that volumetric concentration is 32%~45% as mobile phase, 15~25mL/min of flow velocity, with 21.2 ×
250mm, 5 μm of ZorbaxPrepHT GF reverse phase preparative columns are stationary phase, and UV-detector Detection wavelength is 365nm, is entered every time
0.5~1.0mL of sample, 32.2min chromatographic peak is collected, be evaporated after repeatedly adding up.
6. the additive described in claim 1 is in the application for preventing that tobacco sauce is putrid and deteriorated, extends in the tobacco sauce shelf-life.
7. application of the additive in cigarette smoking quality is lifted described in claim 1.
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