CN107700278A - A kind of cigarette paper additive with sweet larynx effect and its application - Google Patents
A kind of cigarette paper additive with sweet larynx effect and its application Download PDFInfo
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- CN107700278A CN107700278A CN201710767857.XA CN201710767857A CN107700278A CN 107700278 A CN107700278 A CN 107700278A CN 201710767857 A CN201710767857 A CN 201710767857A CN 107700278 A CN107700278 A CN 107700278A
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- cigarette
- cigarette paper
- additive
- rose
- sweet
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- ZDDWLHRUTKJCJO-UHFFFAOYSA-N COc1ccccc1C(Oc(c1c2)cc(CCCO)c2OC)=CC1=O Chemical compound COc1ccccc1C(Oc(c1c2)cc(CCCO)c2OC)=CC1=O ZDDWLHRUTKJCJO-UHFFFAOYSA-N 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D1/00—Cigars; Cigarettes
- A24D1/02—Cigars; Cigarettes with special covers
-
- 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/02—Material of vegetable origin
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/14—Carboxylic acids; Derivatives thereof
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/60—Waxes
Abstract
The invention discloses a kind of cigarette paper additive with sweet larynx effect and its application.By rose honey, benzyl carbinol, phenylethyl propionate, phenyl ethyl formate, vanillic aldehyde, Ethyl vanillin, rose flavones U, royal jelly, propane diols, Absolute Oil of Beeswax, Rosa Damascana, Yunnan olive extract and water it is well mixed after obtain product.Rose flavones U therein, it is isolated new flavone compound from the waste residue after production Rosa Damascana, there is following structural formula：It is named as：7 (3 hydroxypropyl) 8,2 ' dimethoxy flavones.In cigarette paper preparation process, the additive is coated with by the 1~2% of cigarette paper weight, the sweet sense of cigarette smoke is remarkably reinforced, and flue gas becomes more smooth smoothness when passing through throat, throat's excitant substantially reduces, and can be obviously improved throat's comfortableness of cigarette smoking.The additive amount of the present invention is few, and adding technology is easily realized, the influence to cigarette chemical balance is small, will not cause the obvious change to cigarette style.
Description
Technical field
The invention belongs to cigarette additive technical field, is specifically related to a kind of cigarette paper with sweet larynx effect and adds
Add agent.Meanwhile the concrete application the invention further relates to the additive in production of cigarettes.
Background technology
Cigarette paper is a kind of thin page type paper specialized in winding tobacco and make cigarette, is characterized in：Paper is close, soft thin
It is greasy, opacity is high, there is higher machine direction tensile strength, certain gas permeability and suitable burning velocity.It is prepared by cigarette paper
Technique is mainly：Using bleaching jute pulp as primary raw material, partial bleaching wood pulp or straw pulp are mixed, through high shiny beating, is filled with
Calcium carbonate and a small amount of combustion adjuvant (to coordinate the burning velocity of cigarette paper and tobacco filament), after being manufactured paper with pulp on fourdrinier machine, most
After cut rolling up dish for steel, form finished product.Cigarette paper carry except traditional parcel pipe tobacco, regulation cigarette burning, improve cigarette ash wrappage,
, can also be to cigarette product during reduction cigarette smoking outside the function such as harmful components such as caused tar content, side-stream smoke CO
Suction quality improved, the functional study of this respect increasingly causes the concern of researcher.
With growing to even greater heights for world's anti-smoking campaign, various countries' tobacco business reduces the tar content of cigarette one after another；With
The continuous low tar of cigarette, only developing cigarette odor-absorbing compensation technique could still obtain higher while tar is reduced
Suction quality, maintain the quality and feature of existing product.Therefore, tobacco enterprise is reducing tar and is improving taking out for cigarette product
During inhaling quality, it is required for developing corresponding cigarette odor-absorbing compensation technique.Because cigarette paper perfuming technology easily realizes industry
Change, and chemical balance on cigarette influences small, therefore improves the suction quality of cigarette in tobacco industry by cigarette paper
It is widely applied.Thus the various new technologies developed：Inclusion compound perfuming technology, capsule perfuming technology, microporous polymer add
Fragrant technology, ion exchange resin perfuming technology, adsorbent perfuming technology etc. are widely used, and have developed panoramic
Functional cigarette paper, for improving cigarette smoking quality.
Yunnan tobacco product fragrance is sufficient, strong, and strength is moderate, and suction satisfaction is strong.But portioned product and outside the province
Competition brand compare, due to consumer taste hobby otherness, partly outside the province market there is also suction comfortableness to be slightly short of,
The problem of excitant, dry sensation slightly appear, it is badly in need of carrying out the improvement and lifting of product suction quality, the development significance of correlation technique
It is great.
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
With return sweet larynx effect cigarette paper additive, with reduce throat's excitant of flue gas, lifting cigarette smoking when throat relax
Adaptive.
The present invention also aims to provide concrete application of the described additive in cigarette paper production.
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 cigarette paper additive with sweet larynx effect, is made up of the raw material of following mass percents：Rose
Honey 9%~12%, benzyl carbinol 0.2%~0.3%, phenylethyl propionate 0.15%~0.2%, phenyl ethyl formate 0.08%~
0.1%, vanillic aldehyde 0.04%~0.06%, Ethyl vanillin 0.1%~0.15%, rose flavones-U 0.2%~0.3%, honeybee
Royal jelly 2%~4%, propane diols 9%~12%, Absolute Oil of Beeswax 0.8%~1.2%, Rosa Damascana 0.2%~0.3% and Yunnan olive
Olive extract 1.5%~2%, surplus are water；Each raw material is well mixed and fully dissolved, obtained shallow yellow transparent solution,
As required cigarette paper additive.
In additive formulations composition：Propane diols is cosolvent, can increase the dissolubility of each component in formula, make in formula
Each component can fully dissolve, and avoid directly preparing the microprecipitation occurred and muddiness with water.
Benzyl carbinol, phenyl ethyl formate, phenylethyl propionate, vanillic aldehyde, Ethyl vanillin are monomer perfume.Benzyl carbinol has clear
The rose sample fragrance of a flower of sweet tea；Phenyl ethyl formate has the pure and fresh fragrance of a flower and fruit aroma；Phenylethyl propionate is in fragrant and sweet red rose like fragrant
Gas, there is fruit bottom note, like dense honey and strawberry flavor；Vanillic aldehyde and Ethyl vanillin have strong vanilla fragrance and
The sweet taste road of sweet chocolate.
Rose honey and royal jelly thermal decomposition product react acid, and can rise to neutralize with the alkaline matter in flue gas and make
With can reduce the miscellaneous gas and excitant of cigarette, increase the mellow and full sense of cigarette smoke.
Absolute Oil of Beeswax, Rosa Damascana and Yunnan olive extract are natural extract.Absolute Oil of Beeswax have it is gentle fragrant and sweet and
The fragrant bottom rhythm of wax, has the smell as with book on Chinese herbal medicine as Coumarins.Rosa Damascana has that strong rose feature is fragrant and sweet, fragrance
Sweet tea and it is full, possess thick and heavy graceful inside information.Yunnan olive extract has clearing heat, relieving sore-throat, moistening lung for removing phlegm, the effect of promoting the production of body fluid to quench thirst.
Described rose flavones-U, it is isolated new 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：7- (3- hydroxypropyls) -8,2 '-dimethoxy flavone, English name
For：7- (3-hydroxypropyl) -6,2 '-dimethoxy-flavone, popular name are rose flavones-U.Cigarette can substantially be increased
The sweet sense of flue gas, have the function that to promote the production of body fluid, Hui Tian.
The 7- (3- hydroxypropyls) -8 is prepared, the method for 2 '-dimethoxy flavone, is comprised 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 160~200 mesh, the weight of used silica gel
For 6~10 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 8:The eluent that 2 chloroform-acetone affords uses high performance liquid chromatography
Isolate and purify, UV-detector Detection wavelength is 358nm, collects 30~45min chromatographic peak, is evaporated, produces after repeatedly adding up
The 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 80~100 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), the purifying of described high performance liquid chromatography separation is water-soluble as 45~65% methanol using volumetric concentration
Liquid is mobile phase, and 15~25mL/min of flow velocity, with 21.2 × 250mm, 5 μm of ZorbaxPrepHT GF reverse phase preparative columns are solid
Determine phase, UV-detector Detection wavelength is 358nm, each 0.5~1.0mL of sample introduction, collects 38.6min chromatographic peak, repeatedly tired
It is evaporated after adding.
In cigarette paper preparation process, the additive, the sweet sense of cigarette smoke are coated with by the 1~2% of cigarette paper weight
It is remarkably reinforced, flue gas becomes more smooth smoothness when passing through throat, throat's excitant substantially reduces, and can be obviously improved cigarette smoking
Throat's comfortableness.
Cigarette paper preparation method：Fibrous raw material is discongested, is beaten, allocates long and short fiber ratio, function additive, addition
Filler, then through being dehydrated paper shaping, after the shaping of described paper, after additive of the present invention is added into shaping with spray pattern
In wet paper, addition is the 1~2% of cigarette paper dry weight；Again through squeezing, drying, batching, rewinding, you can obtain with the addition of this
The cigarette paper of invention additive.Cigarette paper is used to prepare cigarette, and to be not added with the identical cigarette paper of additive of the present invention work
Control, sensory evaluation is carried out according to GB5606.4-2005 standards, evaluation result shows：Present invention addition is added in cigarette paper
After agent, the sweet sense of cigarette mainstream flue gas is remarkably reinforced, and flue gas becomes more smooth smoothness when passing through throat, and throat's excitant is obvious
Reduce, throat's comfortableness of cigarette smoking can be obviously improved.
The beneficial effects of the invention are as follows：
1st, additive of the present invention makes simple, and each components in certain proportion is well mixed i.e. available, and the additive has strong
Sweet fragrance, it is very prominent to smell fragrant feature.Coating 1~2% just has obvious effect, cigarette cigarette in cigarette paper preparation process
The sweet sense of gas is remarkably reinforced, and flue gas becomes smooth smoothness when passing through throat, and throat's excitant substantially reduces, and can be obviously improved volume
Throat's comfortableness of cigarette suction.Also cigarette suction comfort can be alleviated to a certain extent to be slightly short of, excitant, drying slightly appear
The problem of.
2nd, additive of the present invention is added on cigarette paper in cigarette paper production process, and adding technology is easily realized, and
Additive amount is few, small by influence of the cigarette paper addition to cigarette chemical balance, will not cause changing the obvious of cigarette style
Become.
3rd, in addition to rose flavones-U, the raw material of additive of the present invention is available from the market, there is the production and supply of maturation,
Additive low manufacture cost.
4th, the key component rose flavones-U in additive is, raw material isolated in the waste residue after Rosa Damascana to produce
Source is very extensive, and cost is low；Waste resource can be comprehensively utilized by producing the compound, improve the added value of rose processing.Should
Flavone compound has prominent improvement sense of taste effect, has a kind of natural, light time sweet taste after entrance, flue gas can be allowed to pass through larynx
Become more smooth and smooth during portion.
Brief description of the drawings
Fig. 1 be rose flavones-U of the present invention carbon-13 nmr spectra (13C NMR)；
Fig. 2 be rose flavones-U of the present invention proton nmr spectra (1H NMR)；
The related figures of crucial HMBC that Fig. 3 is rose flavones-U 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.If not the raw material and equipment employed in embodiment refer in particular to, it is commercially available or this area
Conventional, the method in embodiment, it is the conventional method of this area unless otherwise instructed.
Embodiment-1 --- compound rose flavones-U 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, be concentrated under reduced pressure into the 1/4 of volume；It is quiet
Put, filter out sediment, filter out MCI posts on the solution after precipitation and decolourize, be concentrated under reduced pressure to give 6.8kg medicinal extract；Medicinal extract 680g is taken to exist
1.2kg acetone solution is added in medicinal extract, 100 mesh silica gel 900g is then added and mixes sample, post is filled with 200 mesh silica gel 4.5kg, mixes sample
Upper prop afterwards；It is respectively 20 with volume ratio:1,9:1,8:2,7:3,6:4 and 1:1 chloroform-acetone mixed organic solvents gradient is washed
It is de-, gradient eluent, concentration are collected, is monitored through TLC, merges identical part, obtains 6 part A-F, wherein, to being collected into
Sample B (8:2) part 183g, then using 56% methanol as mobile phase, 20ml/min, 21.2 × 250mm, 5 μm of flow velocity
ZorbaxPrepHT GF reverse phase preparative columns are stationary phase, and UV-detector Detection wavelength is 358nm, each sample introduction 1.0mL, is received
Collect 38.6min chromatographic peak, be evaporated after repeatedly adding up, produce compound rose flavones-U.
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 363.1215 [M+Na]+(calculated value 363.1208), with reference to1H NMR
Composed with DEPT and determine that its molecular formula is C19H18O5, degree of unsaturation 11.
Hydroxyl (3428), carbonyl (1665) and aromatic ring (1618,1552 and 1463cm are shown in infrared spectrum-1) resonance
Absworption peak.And ultraviolet spectra there may be aromatic ring structure in 210,256,358nm 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 20 carbon and 20 hydrogen, including 1
1,2,4,5- quaternary phenyl ring (C-5~C-10, H-5, H-6), 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 hydroxypropyl (C-1 "~C-3 ", H2- 1 "~H2- 3 "), two
Individual methoxyl group (δC56.2q and 55.9q, δH3.81s and 3.79s).According to typical 2 phenyl ring, alpha, beta-unsaturated carbonyl and double
Key signals, it is flavone compound that can speculate the 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-6, C-7, C-9, C-10, and H-6 ' (such as Fig. 3) related to C-2 HMBC may further confirm that compound is
Flavonoid structure.
After the parent of compound determines, remaining substituent, hydroxypropyl and methoxyl group can be considered the substituent on flavones.Change
Two methoxyl group hydrogen (δ can be observed in (such as Fig. 3) in the HMBC spectrums of compoundH3.81 and 3.79) HMBC phases with C-6 and C-2'
Close, can speculate that two methoxyl groups are substituted in C-6 and C-2' positions respectively；According to H2-1″(δH2.72) and C-6, C-7, C-8, H2-2″
(δHAnd C-7, and H-8 (δ 1.89)H6.80) it is related to C-1 " HMBC, it can be verified that hydroxypropyl is substituted in C-7 positions.Typical case in addition
Phenyl ring on proton signal [H-5, δH7.19s；H-8,δH6.80s, H-3 ' δH6.93(d)7.6；H-4 ', δH7.36(t)7.6；
H-5 ', δH6.88(t)7.6；H-6 ', δH7.82 (d) 7.6] also the B rings of susceptible of proof chromocor compound of the present invention be 6,7- positions two
Substitution, C rings are that 2'- positions are monosubstituted.So far, the structure of compound is determined, Compound nomenclature is：7- (3- hydroxypropyls) -8,
2 '-dimethoxy flavone, popular name are rose flavones-U.
The compounds of this invention of table 1.1H NMR and13C NMR datas (CDCl3)
Infrared, the ultraviolet and mass spectrometric data of compound：Purple light composes (methanol), λmax(logε)358(3.73)、256
(3.95)、210(4.33)；Infrared spectrum (pressing potassium bromide troche)：νmax3428、2857、1665、1618、1552、1463、1150、
1258、1150、1064cm-1；1H and13C NMR datas (500 and 125MHz, solvent CDCl3), it is shown in Table -1；Positive ion mode
ESIMS m/z363[M+Na]+；Positive ion mode HRESIMS m/z363.1215 [M+Na]+(calculated value 363.1208,
C20H20NaO5)。
Additive prepares embodiment 1
Additive in the present embodiment is prepared from the following materials：Rose honey 10%, benzyl carbinol 0.25%, propionic acid
Phenethyl ester 0.15%, phenyl ethyl formate 0.1%, vanillic aldehyde 0.04%, Ethyl vanillin 0.12%, rose flavones-U 0.2%,
Royal jelly 4%, propane diols 10%, Absolute Oil of Beeswax 1%, Rosa Damascana 0.25%, Yunnan olive extract 2%, water 71.89%.Respectively
Components in certain proportion is well mixed, and is fully dissolved, and obtains the solution of light yellow clear, has strong sweet fragrance, i.e. this hair
Bright additive.The additive of the present embodiment of addition 1.2% in cigarette paper is rolled up in Yunnan brand.Cigarette is rolled into, according to
GB5606.4-2005 standards carry out sensory evaluation, and are not added with using in cigarette paper the cigarette of the additive as compareing.Evaluation knot
Fruit shows：Additive of the present invention is with the addition of in cigarette paper, cigarette flavor is full, fine and smooth, and flue gas becomes more suitable when passing through throat
It is sliding, smooth, return sweet tea sense and be remarkably reinforced, suction comfortableness gets a promotion.
Additive prepares embodiment 2
Additive in the present embodiment is prepared from the following materials：Rose honey 10%, benzyl carbinol 0.2%, propionic acid
Phenethyl ester 0.2%, phenyl ethyl formate 0.08%, vanillic aldehyde 0.04%, Ethyl vanillin 0.1%, rose flavones-U 0.25%,
Royal jelly 3%, propane diols 10%, Absolute Oil of Beeswax 1%, Rosa Damascana 0.3%, Yunnan olive extract 1.8%, water 73.23%.Respectively
Components in certain proportion is well mixed, and is fully dissolved, and obtains the solution of light yellow clear, has strong sweet fragrance, i.e. this hair
Bright additive.The additive of the present embodiment of addition 1.5% in cigarette paper is rolled up in Yunnan brand.Cigarette is rolled into, according to
GB5606.4-2005 standards carry out sensory evaluation, and are not added with using in cigarette paper the cigarette of the additive as compareing.Evaluation knot
Fruit shows：Additive of the present invention is with the addition of in cigarette paper, cigarette flavor is plentiful, and close fragrant and sweet feature is very prominent；Oral cavity pleasant impression
It is comfortable clean, there is light time sweet tea sense, larynx excitant reduces, the more smooth smoothness of flue gas, and suction comfortableness gets a promotion.
Additive prepares embodiment 3
Additive in the present embodiment is prepared from the following materials：Rose honey 12%, benzyl carbinol 0.2%, propionic acid
Phenethyl ester 0.2%, phenyl ethyl formate 0.1%, vanillic aldehyde 0.04%, Ethyl vanillin 0.12%, rose flavones-U 0.25%,
Royal jelly 3%, propane diols 12%, Absolute Oil of Beeswax 1.2%, Rosa Damascana 0.3%, Yunnan olive extract 2%, water 68.59%.Respectively
Components in certain proportion is well mixed, and is fully dissolved, and obtains the solution of light yellow clear, has strong sweet fragrance, i.e. this hair
Bright additive.The additive of the present embodiment of addition 2% in cigarette paper is rolled up in Yunnan brand.Cigarette is rolled into, according to
GB5606.4-2005 standards carry out sensory evaluation, and are not added with using in cigarette paper the cigarette of the additive as compareing.Evaluation knot
Fruit shows：Additive of the present invention is with the addition of in cigarette paper, cigarette smoke fragrance is plentiful, and close fragrant and sweet feature appears very much, has clear
Light to return sweet tea sense, larynx excitant reduces, the more smooth smoothness of flue gas, and suction comfortableness gets a promotion, but with this perfume of former cigarette slightly
It is uncoordinated.
Additive prepares embodiment 4
Additive in the present embodiment is prepared from the following materials：Rose honey 12%, benzyl carbinol 0.3%, propionic acid
Phenethyl ester 0.2%, phenyl ethyl formate 0.1%, vanillic aldehyde 0.06%, Ethyl vanillin 0.15%, rose flavones-U 0.3%, honeybee
Royal jelly 4%, propane diols 12%, Absolute Oil of Beeswax 1.2%, Rosa Damascana 0.2%, Yunnan olive extract 1.8%, water 67.69%.Respectively
Components in certain proportion is well mixed, and is fully dissolved, and obtains the solution of light yellow clear, has strong sweet fragrance, i.e. this hair
Bright additive.The additive of the present embodiment of addition 1.6% in cigarette paper is rolled up in Yunnan brand.Cigarette is rolled into, according to
GB5606.4-2005 standards carry out sensory evaluation, and are not added with using in cigarette paper the cigarette of the additive as compareing.Evaluation knot
Fruit shows：With the addition of additive of the present invention in cigarette paper, the comfortableness of the throat of cigarette smoking be improved significantly, flue gas is more
Smooth smoothness, the distinctive fresh and sweet perfume (or spice) of cloud and mist are strengthened, and oral cavity pleasant impression is comfortable, are returned sweet tea sense and are protruded.
Additive prepares embodiment 5
Additive in the present embodiment is prepared from the following materials：Rose honey 9%, benzyl carbinol 0.2%, propionic acid benzene
Ethyl ester 0.15%, phenyl ethyl formate 0.1%, vanillic aldehyde 0.04%, Ethyl vanillin 0.1%, rose flavones-U 0.2%, queen bee
Slurry 2%, propane diols 9%, Absolute Oil of Beeswax 0.8%, Rosa Damascana 0.2%, Yunnan olive extract 1.5%, water 76.71%.Respectively into
Divide and mix in proportion, and fully dissolve, obtain the solution of light yellow clear, there is strong sweet fragrance, i.e., it is of the invention
Additive.The additive of the present embodiment of addition 1.0% in cigarette paper is rolled up in Yunnan brand.Cigarette is rolled into, according to
GB5606.4-2005 standards carry out sensory evaluation, and are not added with using in cigarette paper the cigarette of the additive as compareing.Evaluation knot
Fruit shows：Additive of the present invention is with the addition of in cigarette paper, the comfortableness of the throat of cigarette smoking is obviously improved, excitant drop
Low, honey is fragrant and oral cavity is returned sweet tea sense and protruded, but perfume quantity is slightly inadequate.
Additive prepares embodiment 6
Additive in the present embodiment is prepared from the following materials：Rose honey 10%, benzyl carbinol 0.25%, propionic acid
Phenethyl ester 0.2%, phenyl ethyl formate 0.1%, vanillic aldehyde 0.05%, Ethyl vanillin 0.12%, rose flavones-U 0.25%,
Royal jelly 3%, propane diols 10%, Absolute Oil of Beeswax 1%, Rosa Damascana 0.25%, Yunnan olive extract 1.8%, water 72.98%.
Each components in certain proportion is well mixed, and is fully dissolved, and obtains the solution of light yellow clear, has strong sweet fragrance, i.e., originally
The additive of invention.The additive of the present embodiment of addition 1.5% in cigarette paper is rolled up in Yunnan brand.Cigarette is rolled into, is pressed
Sensory evaluation is carried out according to GB5606.4-2005 standards, and is not added with using in cigarette paper the cigarette of the additive as compareing.Evaluation
As a result show：Additive of the present invention is with the addition of in cigarette paper, cigarette flavor is plentiful, and this fragrant harmony of tobacco is good, flue gas more
Delicate and smooth, reduction throat irritant effects are obvious, and pleasant impression is clean, and oral cavity is returned sweet tea sense and protruded.
Additive prepares embodiment 7
Additive in the present embodiment is prepared from the following materials：Rose honey 10%, benzyl carbinol 0.2%, propionic acid
Phenethyl ester 0.15%, phenyl ethyl formate 0.09%, vanillic aldehyde 0.04%, Ethyl vanillin 0.12%, rose flavones-U 0.3%,
Royal jelly 4%, propane diols 10%, Absolute Oil of Beeswax 1%, Rosa Damascana 0.3%, Yunnan olive extract 2%, water 71.8%.Respectively into
Divide and mix in proportion, and fully dissolve, obtain the solution of light yellow clear, there is strong sweet fragrance, i.e., it is of the invention
Additive.The additive of the present embodiment of addition 1.6% in cigarette paper is rolled up in Yunnan brand.Cigarette is rolled into, according to
GB5606.4-2005 standards carry out sensory evaluation, and are not added with using in cigarette paper the cigarette of the additive as compareing.Evaluation knot
Fruit shows：Additive of the present invention is with the addition of in cigarette paper, throat's dry sensation of cigarette smoke and spine sense substantially mitigate, flue gas
More mellow and fuller and smooth by throat, pleasant impression is comfortably clean, returns sweet tea sense and protrudes, the distinctive fresh and sweet perfume (or spice) of cloud and mist is strengthened.
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, additive prepares total point of embodiment 1-7 more than 91, is above pair
Product in the same old way.Additive of the present invention is added in cigarette paper can improve throat's comfortableness of cigarette smoking, and flue gas passes through throat's time-varying
Must be more smooth, reduce the spine sense of throat.
Table -2, additive embodiment 1-7 cigarette sample smoking results
Claims (6)
1. a kind of cigarette paper additive with sweet larynx effect, is made up of the raw material of following mass percents：Rose anthophorids
Honey 9%~12%, benzyl carbinol 0.2%~0.3%, phenylethyl propionate 0.15%~0.2%, phenyl ethyl formate 0.08%~
0.1%, vanillic aldehyde 0.04%~0.06%, Ethyl vanillin 0.1%~0.15%, rose flavones-U 0.2%~0.3%, honeybee
Royal jelly 2%~4%, propane diols 9%~12%, Absolute Oil of Beeswax 0.8%~1.2%, Rosa Damascana 0.2%~0.3% and Yunnan olive
Olive extract 1.5%~2%, surplus are water；
Wherein, described rose flavones-U, it is isolated new flavonoid from the waste residue after production Rosa Damascana
Thing, there is following structural formula：
The Compound nomenclature is：7- (3- hydroxypropyls) -8,2 '-dimethoxy flavone, English are entitled：7-(3-
hydroxypropyl)-6,2′-dimethoxy-flavone；
Each raw material is well mixed and fully dissolved, obtained shallow yellow transparent solution, as required cigarette paper additive.
2. cigarette paper additive according to claim 1, it is characterised in that described rose flavones-U preparation method,
Comprise 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 160~200 mesh, and the weight of used silica gel is leaching
6~10 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 8:The eluent that 2 chloroform-acetone affords uses high performance liquid chromatography separation
Purifying, UV-detector Detection wavelength is 358nm, collects 30~45min chromatographic peak, is evaporated after repeatedly adding up, produces the change
Compound.
3. cigarette paper additive according to claim 2, it is characterised in that：In step (1), described solvent is that volume is dense
The aqueous acetone solution of degree 70%~100%, the ethanol water of volumetric concentration 70%~100% or volumetric concentration 70%~
100% methanol aqueous solution.
4. cigarette paper additive according to claim 2, it is characterised in that：In step (3), medicinal extract is in upper silica gel column chromatography
Before, first dissolved with the acetone or methanol of 1.5~3 times of medicinal extract weight amount, then with the 80 of 0.8~1.2 times of amount of medicinal extract weight~
100 mesh silica gel mixed samples, afterwards loading.
5. cigarette paper additive according to claim 2, it is characterised in that：In step (4), described high performance liquid chromatography
It is 15~25mL/min of flow velocity using the methanol aqueous solution that volumetric concentration is 45~65% as mobile phase to isolate and purify, with 21.2 ×
250mm, 5 μm of ZorbaxPrepHT GF reverse phase preparative columns are stationary phase, and UV-detector Detection wavelength is 358nm, is entered every time
0.5~1.0mL of sample, 38.6min chromatographic peak is collected, be evaporated after repeatedly adding up.
6. application of the cigarette paper additive described in claim 1 in production of cigarettes, it is specially：In cigarette paper preparation process
In, it is coated with the additive by the 1~2% of cigarette paper weight.
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