CN103205312A - Preparation method of aromatic wood spice for cigarettes - Google Patents
Preparation method of aromatic wood spice for cigarettes Download PDFInfo
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- CN103205312A CN103205312A CN2013101275026A CN201310127502A CN103205312A CN 103205312 A CN103205312 A CN 103205312A CN 2013101275026 A CN2013101275026 A CN 2013101275026A CN 201310127502 A CN201310127502 A CN 201310127502A CN 103205312 A CN103205312 A CN 103205312A
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- pistacia weinmannifolia
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 62
- 235000013599 spices Nutrition 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000002023 wood Substances 0.000 title abstract 7
- 125000003118 aryl group Chemical group 0.000 title description 2
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000199 molecular distillation Methods 0.000 claims abstract description 12
- 238000000899 pressurised-fluid extraction Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 241000115499 Pistacia weinmaniifolia Species 0.000 claims description 57
- 235000004760 Pistacia weinmaniifolia Nutrition 0.000 claims description 57
- 238000004821 distillation Methods 0.000 claims description 15
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000000470 constituent Substances 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000005194 fractionation Methods 0.000 claims description 2
- 239000003205 fragrance Substances 0.000 abstract description 32
- 239000000779 smoke Substances 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 11
- 239000002304 perfume Substances 0.000 abstract description 7
- 230000000391 smoking effect Effects 0.000 abstract description 6
- 235000002637 Nicotiana tabacum Nutrition 0.000 abstract description 2
- 239000010779 crude oil Substances 0.000 abstract 2
- 241000208125 Nicotiana Species 0.000 abstract 1
- 238000011156 evaluation Methods 0.000 abstract 1
- 239000000796 flavoring agent Substances 0.000 description 27
- 235000013355 food flavoring agent Nutrition 0.000 description 21
- 239000003921 oil Substances 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 7
- 235000019634 flavors Nutrition 0.000 description 6
- 241001647745 Banksia Species 0.000 description 5
- 241000220317 Rosa Species 0.000 description 5
- 235000013372 meat Nutrition 0.000 description 5
- 238000009738 saturating Methods 0.000 description 5
- FAMPSKZZVDUYOS-UHFFFAOYSA-N alpha-Caryophyllene Natural products CC1=CCC(C)(C)C=CCC(C)=CCC1 FAMPSKZZVDUYOS-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- NPNUFJAVOOONJE-ZIAGYGMSSA-N β-(E)-Caryophyllene Chemical compound C1CC(C)=CCCC(=C)[C@H]2CC(C)(C)[C@@H]21 NPNUFJAVOOONJE-ZIAGYGMSSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000001953 sensory effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NVEQFIOZRFFVFW-UHFFFAOYSA-N 9-epi-beta-caryophyllene oxide Natural products C=C1CCC2OC2(C)CCC2C(C)(C)CC21 NVEQFIOZRFFVFW-UHFFFAOYSA-N 0.000 description 2
- SXVPOSFURRDKBO-UHFFFAOYSA-N Cyclododecanone Chemical compound O=C1CCCCCCCCCCC1 SXVPOSFURRDKBO-UHFFFAOYSA-N 0.000 description 2
- 241000543704 Pistacia Species 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- NPNUFJAVOOONJE-UHFFFAOYSA-N beta-cariophyllene Natural products C1CC(C)=CCCC(=C)C2CC(C)(C)C21 NPNUFJAVOOONJE-UHFFFAOYSA-N 0.000 description 2
- UAHWPYUMFXYFJY-UHFFFAOYSA-N beta-myrcene Chemical compound CC(C)=CCCC(=C)C=C UAHWPYUMFXYFJY-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229940117948 caryophyllene Drugs 0.000 description 2
- NPNUFJAVOOONJE-UONOGXRCSA-N caryophyllene Natural products C1CC(C)=CCCC(=C)[C@@H]2CC(C)(C)[C@@H]21 NPNUFJAVOOONJE-UONOGXRCSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- 239000001169 1-methyl-4-propan-2-ylcyclohexa-1,4-diene Substances 0.000 description 1
- CHBNMKPHUSAEJE-KQLJZIGXSA-N 2,6,6-trimethyl-3-(2,6,6-trimethyl-3-bicyclo[3.1.1]hept-1-enyl)-3-[(3R)-2,6,6-trimethyl-3-bicyclo[3.1.1]hept-1-enyl]bicyclo[3.1.1]hept-1-ene Chemical compound C12=C([C@@H](CC(C1(C)C)C2)C1(C(=C2C(C(C1)C2)(C)C)C)C1C(=C2C(C(C1)C2)(C)C)C)C CHBNMKPHUSAEJE-KQLJZIGXSA-N 0.000 description 1
- IBVJWOMJGCHRRW-UHFFFAOYSA-N Delta22-Carene Natural products C1CC(C)=CC2C(C)(C)C12 IBVJWOMJGCHRRW-UHFFFAOYSA-N 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 208000004232 Enteritis Diseases 0.000 description 1
- BFZNMUGAZYAMTG-UHFFFAOYSA-N Ethyl octynecarboxylate Chemical compound CCCCCCC#CC(=O)OCC BFZNMUGAZYAMTG-UHFFFAOYSA-N 0.000 description 1
- 208000010201 Exanthema Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical class OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 235000003445 Pistacia Nutrition 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- VYBREYKSZAROCT-UHFFFAOYSA-N alpha-myrcene Natural products CC(=C)CCCC(=C)C=C VYBREYKSZAROCT-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- IBVJWOMJGCHRRW-BDAKNGLRSA-N delta-2-carene Chemical compound C1CC(C)=C[C@@H]2C(C)(C)[C@H]12 IBVJWOMJGCHRRW-BDAKNGLRSA-N 0.000 description 1
- ISXDVFNOXYQPIA-UHFFFAOYSA-N dibutyl pentanedioate Chemical compound CCCCOC(=O)CCCC(=O)OCCCC ISXDVFNOXYQPIA-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010642 eucalyptus oil Substances 0.000 description 1
- 229940044949 eucalyptus oil Drugs 0.000 description 1
- 201000005884 exanthem Diseases 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- BXWQUXUDAGDUOS-UHFFFAOYSA-N gamma-humulene Natural products CC1=CCCC(C)(C)C=CC(=C)CCC1 BXWQUXUDAGDUOS-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- QBNFBHXQESNSNP-UHFFFAOYSA-N humulene Natural products CC1=CC=CC(C)(C)CC=C(/C)CCC1 QBNFBHXQESNSNP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000077 insect repellent Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- CCRCUPLGCSFEDV-UHFFFAOYSA-N methyl cinnamate Chemical class COC(=O)C=CC1=CC=CC=C1 CCRCUPLGCSFEDV-UHFFFAOYSA-N 0.000 description 1
- CCRCUPLGCSFEDV-BQYQJAHWSA-N methyl trans-cinnamate Chemical class COC(=O)\C=C\C1=CC=CC=C1 CCRCUPLGCSFEDV-BQYQJAHWSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000007875 phellandrene derivatives Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 229930006978 terpinene Natural products 0.000 description 1
- 150000003507 terpinene derivatives Chemical class 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- OGLDWXZKYODSOB-UHFFFAOYSA-N α-phellandrene Chemical compound CC(C)C1CC=C(C)C=C1 OGLDWXZKYODSOB-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Fats And Perfumes (AREA)
- Seasonings (AREA)
Abstract
The invention discloses a preparation method of a balsamiferous wood spice for cigarettes. The method comprises the steps of extracting leaves, branches or barks of the fresh-scented wood which are dried and crushed to 5-20 meshes by an accelerated solvent extraction method to obtain fresh-scented wood leaf crude oil, distilling the fresh-scented wood leaf crude oil in a molecular distillation device under the condition of high vacuum degree, collecting heavy component separation products, and dissolving the heavy component separation products in 70% alcohol and propylene glycol by volume ratio to prepare the tobacco fresh-scented wood essence perfume. Through smoking evaluation comparison, the faint scent wood essence spice for the cigarette can obviously enhance the richness and the fineness of the smoke fragrance of the cigarette, mainly increases the faint scent, the spicy fragrance, the costustoot, the fruity fragrance and the flower fragrance of the cigarette, has soft fragrance, is light and elegant in penetrability, and has good compatibility with the smoke fragrance of the cigarette.
Description
Technical field
The invention belongs to the essence spice for cigarette technical field, be specifically related to a kind of molecular distillation technique that uses and prepare the method that cigarette is used Pistacia weinmannifolia spices.
Background technology
Meat flavor formulating technology is one of core technology that makes up cigarette brand feature, liquor style, and essence and flavoring agent is the key of meat flavor formulating technology.Though present domestic essence and flavoring agent enterprise is obtaining certain achievement aspect all kinds of essence and flavoring agent exploitations, still have big gap but compare with advanced international standard, mainly show higher to the degree of dependence of external essence and flavoring agent, lack the aspects such as meat flavor formulating technology that have autonomous core intellecture property.Statistics shows in addition, the usage quantity of the essence and flavoring agent of natural extract accounts for the major part of all kinds of essence and flavoring agent consumptions of present China, the use of characteristic natural perfume is the basis and key of cigarette meat flavor formulating technology, independent development has the characteristic natural perfume of particular functionality and the emphasis that is essence spice for cigarette research to its relevant extraction, separation, analysis and applied research, is the key point that realizes the cigarette enterprise meat flavor formulating technology principal status of public economy.Therefore, must when making great efforts to improve the smoking property of cigarette security, strengthen the research and development dynamics to Chinese style cigarette characteristic natural perfume, enrich cigarette perfume material kind, give the new quality characteristic of cigarette product and scientific and technological intension.
Pistacia weinmannifolia (Pistacia weinmannifolia) is Anacardiaceae pistache (Pistacia) shrub or dungarunga, is distributed in the ground such as Yunnan, Guizhou, Guangxi, Sichuan, Tibet of Burma and China's Mainland.These seeds are drought-resistant barren, well developed root system, and strong resistance is dry-hot valley area afforestation vanguard tree seed.Pistacia weinmannifolia is had many uses, and leaf contains perfume oil, can be used as medicine, and the effect of eliminating inflammation and expelling toxin and convergence is arranged; Temperature is stewed the water clothes, and is clearing heat and detoxicating; Cure mainly dysentery, enteritis, diarrhoea, ulcer temperature rash; The local resident often keeps away the fragrant material of worm with it as mosquito repellent; The fruit oil-containing can extract industrial chemicals, and bark contains tannin, is the process hides raw material.Pistacia weinmannifolia is tree-like attractive in appearance, and smell delicate fragrance has multiple food, medicinal function, and DEVELOPMENT PROSPECT is wide.
Pistacia weinmannifolia volatile oil main component has contained alkene, aromatic nucleus, ketone, phenol, alcohol, aldehyde and ester class etc., its main component has firpene (16.14%), (+)-2-carene (13.79%), r-terpinene (11.96%), terpinene 4 alcohol (10.86%), caryophyllene (5.05%), a-phellandrene (4.56%), 13-firpene (4.28%), n-terpinene (3.53%), trans-cinnamic acid methyl esters (80.53%), cyclododecanone (6.296%), l-methyl-4-sec.-propyl-2-cyclohexene-1-alcohol (1.31l%), eucalyptus oil (1.301%), pentanedioic acid dibutylester (1.095%) etc.Recent years, the scientific worker carried out about Pistacia weinmannifolia leaf volatile oil chemical ingredients and bioactive research thereof, for example, Cai Bao states in 2008 etc. have carried out detecting analysis to the Pistacia weinmannifolia aroma component, obtain 76 kinds of chemical ingredientss, account for 92.14% of total chromatographic peak area.Wherein the ester class is 22 kinds, accounts for 71.32% of peak area; 21 kinds of olefines account for peak area 25.59%; 12 kinds of alkanes account for peak area 1.91%; 5 kinds of aldehydes account for 0.53% of peak area; 5 kinds of alcohols account for 0.65% of peak area; Ketone and acid account for peak area 7.86%.They infer that styrol, second position myrcene, first position phellandrene, hesperidene, ethyl octynecarbonate, cinnamic acid methyl esters, caryophyllene, humulene are the main aroma component of Pistacia weinmannifolia.These aroma component major parts also are the important aroma components in the cigarette smoke, have special aroma component simultaneously again.But do not see the report that from Pistacia weinmannifolia, extracts the preparation essence spice for cigarette up to now as yet.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, utilize the characteristics of Pistacia weinmannifolia aroma component, the preparation method of a kind of cigarette with Pistacia weinmannifolia spices is provided.This method can keep the molecular structure of thermo-sensitivity flavor matter in the Pistacia weinmannifolia preferably, and the tobacco aromatics using of making can obviously strengthen the rich of cigarette smoke fragrance and fine and smooth sense, moderate cost, non-environmental-pollution, and easy realization of industrialization production.
Purpose of the present invention is achieved by following technical proposals.
Except as otherwise noted, the percentage ratio that adopts among the present invention is weight percentage.
A kind of cigarette comprises the steps: with the preparation method of Pistacia weinmannifolia spices
(1) Pistacia weinmannifolia leaf, branch or bark crushed after being dried are extremely crossed 20 mesh sieves, behind hydrochloric acid pre-treatment 30 min of massfraction 1%, be solvent with volume ratio acetone: water=1:1, under 125 ℃ of conditions, extract with accelerated solvent extraction, collect and obtain the limpid Pistacia weinmannifolia leaf oil of slightly carrying;
(2) will slightly carry the Pistacia weinmannifolia leaf oil and add in the feeder and outgas in advance, after the system vacuum degree reached the instrument necessary requirement, material entered molecular distillation apparatus with the feeding rate of 350~400 mLh and distills; Evaporating pressure 3~10 Pa, distillation temperature is 200~220 ℃, blade applicator rotating speed 300~400 r.min, 100 ℃ of feeding temperatures;
(3) under the vacuum condition of<10 Pa, lightweight part gas directly enters the intermediate condenser condensation, flows into light component collector; Heavy constituent enter the heavy constituent collector along the evaporator tube inwall; And heavy constituent are carried out secondary separation;
(4) heavy constituent of fractionation by distillation gained make Pistacia weinmannifolia spices stoste with the ethanol of 70% volume ratio and propylene glycol dissolving, and obtaining concentration with the ethanol of 70% volume ratio and propylene glycol dilution again is 20~50% cigarette usefulness Pistacia weinmannifolia spices finished product.
Molecular distillation is a kind of special distillation technique, and it is the non-equilibrium continuous process of distillation that carries out under condition of high vacuum degree condition (1~10 Pa), utilizes molecular free path different and material is separated.In the sepn process, mixture can volatilize under the temperature far below atmospheric boiling point, resolution increases significantly than conventional distillation, simultaneously can solve problems such as the indeterminable material decomposes of conventional distillation technique, polymerization, be suitable for separating the mixture of high boiling point, high viscosity, ripe quick property and biologically active.This method is for having good result separating of unstable aroma substance such as being rich in ester class, ketone, alcohols and olefines.The contriver has carried out a large amount of experiments to cigarette with Pistacia weinmannifolia, the result shows, the cigarette that obtains according to the inventive method can obviously strengthen the rich of cigarette smoke fragrance and fine and smooth sense with Pistacia weinmannifolia spices, have pleasant delicate fragrance, Xin Xiang, the banksia rose, fruital and the fragrance of a flower, fragrance is soft, the saturating property sent out lightly floats, and is good with cigarette smoke fragrance compatibleness.
Compared with prior art, the present invention has following outstanding advantage:
1. the present invention is the deep processing product of Pistacia weinmannifolia, and raw material is easy to get, the molecular distillation production process not with an organic solvent, environmental protection, moderate cost, easy realization of industrialization production has the excellent development application prospect.
2. the perfuming cigarette smoking result shows, cigarette of the present invention can obviously strengthen the rich of cigarette smoke fragrance and fine and smooth sense with Pistacia weinmannifolia spices, has pleasant delicate fragrance, Xin Xiang, the banksia rose, fruital and the fragrance of a flower, and fragrance is soft, the saturating property sent out lightly floats, and is good with cigarette smoke fragrance compatibleness.
Embodiment
Be described in further detail below in conjunction with the present invention of embodiment.Should be appreciated that specific embodiment described herein only in order to explain the present invention, does not limit protection scope of the present invention.
Embodiment 1
The Pistacia weinmannifolia leaf powder that airing is dried is broken to 15~20 orders or the Pistacia weinmannifolia branch that airing is dried is crushed to 15~20 orders, sample is behind hydrochloric acid pre-treatment 30 min of massfraction 1%, be solvent with V (acetone): V (water)=1:1, extract with accelerated solvent extraction at 125 ℃, collect and obtain the limpid Pistacia weinmannifolia leaf oil of slightly carrying.To slightly carry in the Pistacia weinmannifolia leaf oil adding charging bottle and outgasing in advance.After the system vacuum degree reached the equipment necessary requirement, material entered molecular distillation apparatus with speed 350~400 mLh setting flow velocity from feeder and distills.Evaporating pressure 3~10 Pa, distillation temperature is 200~220 ℃, blade applicator rotating speed 300~400 r.min, 100 ℃ of feeding temperatures; Discard lightweight component separated product, reclaim the heavy component product of distillation; Molecular distillation Separation and Recovery gained heavy constituent product of distillation is made cigarette with Pistacia weinmannifolia essence and flavoring agent stoste with the dissolving of an amount of ethanol and propylene glycol, and obtaining concentration with the ethanol of 70% volume ratio and propylene glycol dilution again is 30% cigarette usefulness Pistacia weinmannifolia essence and flavoring agent finished product.
Prepared Pistacia weinmannifolia essence and flavoring agent finished product is added in the cigarette bed material by reinforced mode with 3.0% ratio, make corresponding perfuming cigarette again, smoke panel test through 30 professional cigarette sensory evaluating smoking personnel, consistently think, rich and the fine and smooth sense of the fragrance of the cigarette smoke of interpolation Pistacia weinmannifolia essence and flavoring agent obviously is better than contrasting cigarette, mainly is delicate fragrance, Xin Xiang, the banksia rose, fruital and the fragrance of a flower that has increased cigarette, and fragrance is soft, the saturating property sent out lightly floats elegant, and is good with cigarette smoke fragrance compatibleness.
Through measuring, seven chemical index of cigarette mainstream flue gas that add the Pistacia weinmannifolia essence and flavoring agent do not have considerable change.
Embodiment 2
The Pistacia weinmannifolia leaf powder that airing is dried is broken to 15~20 orders or the Pistacia weinmannifolia branch that airing is dried is crushed to 15~20 orders, sample is behind hydrochloric acid pre-treatment 30 min of massfraction 1%, be solvent with V (acetone): V (water)=1:1, extract with accelerated solvent extraction at 125 ℃, collect and obtain the limpid Pistacia weinmannifolia leaf oil of slightly carrying.To slightly carry in the Pistacia weinmannifolia leaf oil adding charging bottle and outgasing in advance.After the system vacuum degree reached necessary requirement, material entered molecular distillation apparatus with speed 350~400 mLh setting flow velocity from feeder and distills.Evaporating pressure 5~10 Pa, distillation temperature is 200~220 ℃, blade applicator rotating speed 300~400 r.min, 130 ℃ of feeding temperatures; Discard the lightweight component from product, reclaim the heavy component product of distillation; The molecular distillation separated product is made cigarette with Pistacia weinmannifolia essence and flavoring agent stoste with the dissolving of small amount of ethanol and propylene glycol, and obtaining concentration with the ethanol of 70% volume ratio and propylene glycol dilution again is 25% cigarette usefulness Pistacia weinmannifolia essence and flavoring agent finished product.
Prepared Pistacia weinmannifolia essence and flavoring agent finished product is added in the cigarette table perfume (or spice) by reinforced mode with 2.5% ratio, make corresponding perfuming cigarette again, smoke panel test through 30 professional cigarette sensory evaluating smoking personnel, consistently think, rich and the fine and smooth sense of the fragrance of the cigarette smoke of interpolation Pistacia weinmannifolia essence and flavoring agent obviously is better than contrasting cigarette, mainly is delicate fragrance, Xin Xiang, the banksia rose and the fruital that has increased cigarette, and fragrance is soft, the saturating property sent out lightly floats elegant, and is good with cigarette smoke fragrance compatibleness.
Through measuring, the cigarette mainstream flue gas hazardness index that adds the Pistacia weinmannifolia essence and flavoring agent does not have considerable change.
Embodiment 3
The Pistacia weinmannifolia leaf powder that airing is dried is broken to 15~20 orders or the Pistacia weinmannifolia branch that airing is dried is crushed to 15~20 orders, sample is behind hydrochloric acid pre-treatment 30 min of massfraction 1%, be solvent with V (acetone): V (water)=1:1, extract with accelerated solvent extraction at 125 ℃, collect and obtain the limpid Pistacia weinmannifolia leaf oil of slightly carrying.To slightly carry in the Pistacia weinmannifolia leaf oil adding charging bottle and outgasing in advance.After the system vacuum degree reached necessary requirement, material entered molecular distillation apparatus with speed 350~400 mLh setting flow velocity from feeder and distills.Evaporating pressure 5 ~ 10 Pa, distillation temperature is 200~220 ℃, blade applicator rotating speed 300~400 r.min, 130 ℃ of feeding temperatures; Discard the lightweight component from product, reclaim the heavy component product of distillation; The molecular distillation separated product is made cigarette with Pistacia weinmannifolia essence and flavoring agent stoste with the ethanol of a small amount of 70% volume ratio and propylene glycol dissolving, and obtaining concentration with ethanol and propylene glycol dilution again is 40% cigarette usefulness Pistacia weinmannifolia essence and flavoring agent finished product.
Prepared Pistacia weinmannifolia essence and flavoring agent finished product is added in the stem feed liquid by reinforced mode with 1.5% ratio, make corresponding perfuming cigarette again, smoke panel test through 30 professional cigarette sensory evaluating smoking personnel, consistently think, rich and the fine and smooth sense of the fragrance of the cigarette smoke of interpolation Pistacia weinmannifolia essence and flavoring agent obviously is better than contrasting cigarette, mainly is delicate fragrance, Xin Xiang, the banksia rose, fruital and the fragrance of a flower that has increased cigarette, and fragrance is soft, the saturating property sent out lightly floats elegant, and is good with cigarette smoke fragrance compatibleness.
Through measuring, the cigarette mainstream flue gas hazardness index that adds the Pistacia weinmannifolia essence and flavoring agent does not have considerable change.
It may be noted that the above only for preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. the preparation method of a cigarette usefulness Pistacia weinmannifolia spices comprises the steps:
(1) Pistacia weinmannifolia leaf, branch or bark crushed after being dried are extremely crossed 20 mesh sieves, behind hydrochloric acid pre-treatment 30 min of massfraction 1%, be solvent with volume ratio acetone: water=1:1, under 125 ℃ of conditions, extract with accelerated solvent extraction, collect and obtain the limpid Pistacia weinmannifolia leaf oil of slightly carrying;
(2) will slightly carry the Pistacia weinmannifolia leaf oil and add in the feeder and outgas in advance, after the system vacuum degree reached the instrument necessary requirement, material entered molecular distillation apparatus with the feeding rate of 350~400 mLh and distills; Evaporating pressure 3~10 Pa, distillation temperature is 200~220 ℃, blade applicator rotating speed 300~400 r.min, 100 ℃ of feeding temperatures;
(3) under the vacuum condition of<10 Pa, lightweight part gas directly enters the intermediate condenser condensation, flows into light component collector; Heavy constituent enter the heavy constituent collector along the evaporator tube inwall; And heavy constituent are carried out secondary separation;
(4) heavy constituent of fractionation by distillation gained make Pistacia weinmannifolia spices stoste with the ethanol of 70% volume ratio and propylene glycol dissolving, and obtaining concentration with the ethanol of 70% volume ratio and propylene glycol dilution again is 20~50% cigarette usefulness Pistacia weinmannifolia spices finished product.
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CN2013101275026A CN103205312A (en) | 2013-04-12 | 2013-04-12 | Preparation method of aromatic wood spice for cigarettes |
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