CN107485047A - A kind of preparation method of essence spice for cigarette temperature control sustained-release micro-capsule - Google Patents
A kind of preparation method of essence spice for cigarette temperature control sustained-release micro-capsule Download PDFInfo
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- CN107485047A CN107485047A CN201710501071.3A CN201710501071A CN107485047A CN 107485047 A CN107485047 A CN 107485047A CN 201710501071 A CN201710501071 A CN 201710501071A CN 107485047 A CN107485047 A CN 107485047A
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- Prior art keywords
- oil
- cigarette
- essence
- solution
- essence spice
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 62
- 235000013599 spices Nutrition 0.000 title claims abstract description 54
- 239000003094 microcapsule Substances 0.000 title claims abstract description 38
- 238000013268 sustained release Methods 0.000 title claims abstract description 29
- 239000012730 sustained-release form Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920001661 Chitosan Polymers 0.000 claims abstract description 48
- 239000000686 essence Substances 0.000 claims description 67
- 239000000243 solution Substances 0.000 claims description 41
- 239000003921 oil Substances 0.000 claims description 27
- 239000000796 flavoring agent Substances 0.000 claims description 15
- 235000013355 food flavoring agent Nutrition 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 229920000858 Cyclodextrin Polymers 0.000 claims description 10
- CBOQJANXLMLOSS-UHFFFAOYSA-N ethyl vanillin Chemical compound CCOC1=CC(C=O)=CC=C1O CBOQJANXLMLOSS-UHFFFAOYSA-N 0.000 claims description 10
- IFYYFLINQYPWGJ-UHFFFAOYSA-N gamma-decalactone Chemical compound CCCCCCC1CCC(=O)O1 IFYYFLINQYPWGJ-UHFFFAOYSA-N 0.000 claims description 10
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 claims description 5
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 claims description 5
- 240000008632 Cota tinctoria Species 0.000 claims description 5
- PQMOXTJVIYEOQL-UHFFFAOYSA-N Cumarin Natural products CC(C)=CCC1=C(O)C(C(=O)C(C)CC)=C(O)C2=C1OC(=O)C=C2CCC PQMOXTJVIYEOQL-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- FSOGIJPGPZWNGO-UHFFFAOYSA-N Meomammein Natural products CCC(C)C(=O)C1=C(O)C(CC=C(C)C)=C(O)C2=C1OC(=O)C=C2CCC FSOGIJPGPZWNGO-UHFFFAOYSA-N 0.000 claims description 5
- 244000262613 Michelia alba Species 0.000 claims description 5
- 235000003415 Michelia alba Nutrition 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000007853 buffer solution Substances 0.000 claims description 5
- 239000001524 citrus aurantium oil Substances 0.000 claims description 5
- 239000010636 coriander oil Substances 0.000 claims description 5
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N coumarin Chemical compound C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 claims description 5
- -1 ethyl malt Chemical compound 0.000 claims description 5
- 229940073505 ethyl vanillin Drugs 0.000 claims description 5
- IFYYFLINQYPWGJ-VIFPVBQESA-N gamma-Decalactone Natural products CCCCCC[C@H]1CCC(=O)O1 IFYYFLINQYPWGJ-VIFPVBQESA-N 0.000 claims description 5
- 229930007744 linalool Natural products 0.000 claims description 5
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- MJTPMXWJHPOWGH-UHFFFAOYSA-N 2-Phenoxyethyl isobutyrate Chemical compound CC(C)C(=O)OCCOC1=CC=CC=C1 MJTPMXWJHPOWGH-UHFFFAOYSA-N 0.000 claims description 4
- 241000212322 Levisticum officinale Species 0.000 claims description 4
- 235000004357 Mentha x piperita Nutrition 0.000 claims description 4
- 241001479543 Mentha x piperita Species 0.000 claims description 4
- 239000010630 cinnamon oil Substances 0.000 claims description 4
- 239000003925 fat Substances 0.000 claims description 4
- 239000001645 levisticum officinale Substances 0.000 claims description 4
- 239000001771 mentha piperita Substances 0.000 claims description 4
- 239000001738 pogostemon cablin oil Substances 0.000 claims description 4
- 229940098465 tincture Drugs 0.000 claims description 4
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000002023 wood Substances 0.000 claims description 4
- 240000002045 Guettarda speciosa Species 0.000 claims description 3
- 235000001287 Guettarda speciosa Nutrition 0.000 claims description 3
- 235000009421 Myristica fragrans Nutrition 0.000 claims description 3
- 235000012308 Tagetes Nutrition 0.000 claims description 3
- 241000736851 Tagetes Species 0.000 claims description 3
- 239000010621 dill oil Substances 0.000 claims description 3
- 239000010649 ginger oil Substances 0.000 claims description 3
- 239000001115 mace Substances 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 2
- 150000002469 indenes Chemical class 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 239000002262 Schiff base Substances 0.000 abstract description 6
- 150000004753 Schiff bases Chemical class 0.000 abstract description 5
- 230000007935 neutral effect Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 abstract description 2
- 235000019198 oils Nutrition 0.000 description 20
- 238000002411 thermogravimetry Methods 0.000 description 15
- 239000000047 product Substances 0.000 description 7
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 6
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229940093503 ethyl maltol Drugs 0.000 description 4
- 125000003454 indenyl group Chemical class C1(C=CC2=CC=CC=C12)* 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 244000061176 Nicotiana tabacum Species 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 210000000697 sensory organ Anatomy 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 239000001116 FEMA 4028 Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- 229960004853 betadex Drugs 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000000391 smoking effect Effects 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 241000270666 Testudines Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000010628 chamomile oil Substances 0.000 description 1
- 235000019480 chamomile oil Nutrition 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 239000001627 myristica fragrans houtt. fruit oil Substances 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- SBNFWQZLDJGRLK-UHFFFAOYSA-N phenothrin Chemical compound CC1(C)C(C=C(C)C)C1C(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 SBNFWQZLDJGRLK-UHFFFAOYSA-N 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- ODLHGICHYURWBS-LKONHMLTSA-N trappsol cyclo Chemical compound CC(O)COC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)COCC(O)C)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1COCC(C)O ODLHGICHYURWBS-LKONHMLTSA-N 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
- Fats And Perfumes (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a kind of preparation method of essence spice for cigarette temperature control sustained-release micro-capsule, this method easily generates schiff bases in neutral medium using the amino of chitosan molecule with the reaction with carbonyl, cyclo-dextrin-modified chitosan is made through reducing in the schiff bases of generation, essence spice for cigarette is included, prepare essence spice for cigarette temperature control sustained-release micro-capsule, and it is applied in binary combined filter tip rod, in sucking process, essence spice for cigarette is released at 65 DEG C~160 DEG C, reaches high-quality suction effect.
Description
Technical field
The invention belongs to cigarette additive preparing technical field, and in particular to a kind of essence spice for cigarette temperature control sustained-release micro-capsule
Preparation method.
Background technology
Flavouring essence for tobacco species is various, and most to be easy to the aromatic liquid material of volatilization, how can either obtain perfuming drop
Burnt effect, and can enough improve the utilization rate and validity period of flavouring essence for tobacco, into the popular domain of tobacco scientific and technical personnel research.Profit
With microcapsules technology, by essence cladding wherein, the effect of sustained release protection is served so that essence fragrance remaining time greatly improves.
Chitosan is the product of chitosan moiety or whole deacetylations ,-the OH contained ,-NH2Make it have excellent absorption, huge legendary turtle
Conjunction, crosslinking and bridging action.Beta-schardinger dextrin is to form oligosaccharide by β-Isosorbide-5-Nitrae-glucosides key connection by 7 glucose units, its
Inner chamber is hydrophobic, can combine to form Host-guest inclusion complex with some small molecules.There to be hydrophobic cavity by physico-chemical process
Cyclodextrin be connected on chitosan and obtain cyclodextrin grafting fiber chitosan, have cyclodextrin and chitosan double grading concurrently, remain
The pardon of cyclodextrin and the adsorptivity of chitosan, for the capsule material of essence spice for cigarette microencapsulation, there is higher application value.
Although the microencapsulation of essence spice for cigarette has had research, single in the presence of research essence and flavoring agent, cyclodextrin embedding effect is relative
Preferably, the composition of the essence spice for cigarette but in actual use is considerably complicated, is a complex mixture, with single wall material
Embedding, effect are very limited.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of essence spice for cigarette temperature control sustained-release micro-capsule
Preparation method；Schiff bases easily is generated with the reaction with carbonyl in neutral medium using the amino of chitosan molecule, generation
Cyclo-dextrin-modified chitosan is made through reducing in schiff bases, and essence spice for cigarette is included, prepares essence spice for cigarette micro-capsule,
The release temperature and burst size of embedding essence spice for cigarette are judged by thermogravimetric analysis；Micro-capsule is added to cigarette composite tip stick
In, evaluate the feasibility that uses of micro-capsule by organoleptic properties.
The purpose of the present invention is achieved by the following technical programs：
（1）150-200mg chitosans are dissolved in 100mL pH4.4-5.0 NaAc_HAc buffer solution, are designated as solution A；
1-2g hydroxypropyl-β-cyclodextrins are dissolved in 50mL water, are designated as B solution；Solution A is mixed with B solution, 1-2h is stirred at room temperature,
Add 250-300mg sodium borohydrides, mixture stirs 12-15h at room temperature, and pH is adjusted to neutrality with ammoniacal liquor, 3000-5000 rpm from
Heart 20-30min, 50-60 DEG C of vacuum drying, is made cyclo-dextrin-modified chitosan.
（2）By step（1）Cyclo-dextrin-modified chitosan is dissolved in volumetric concentration 1-2% acetum, be made concentration 25~
30mg/mL cyclo-dextrin-modified chitosan solution.
（3）At 30 DEG C~40 DEG C, essence spice for cigarette drop is added to step（2）Cyclo-dextrin-modified chitosan solution
In, 5~6h is stirred, it is molten to neutrality, wherein essence spice for cigarette and cyclo-dextrin-modified chitosan to adjust pH with sodium hydroxide solution
Liquid volume ratio is 1:1-1:3；
（4）Step（3）Obtained solution stands 24~48h at 4 DEG C, separates out and precipitates, true with distillation water washing, filter residue after suction filtration
After sky is dried, 20-40 mesh sieves are crossed, obtain essence spice for cigarette temperature control sustained-release micro-capsule.
The step（1）And step（3）Middle 800~1200r/min of speed of agitator.
The essence spice for cigarette liquid includes the essence and flavoring agent and solvent that mass percent is no more than 10%, and wherein essence is fragrant
Material include vanillic aldehyde, cumarin, phenoxyethyl isobutanoate, ethylmaltol, γ-decalactone, Ethyl vanillin, indenes punt-pole it is oily,
Mace oil, yellow chamomile caul-fat, coriander oil, linalool, mentha piperita oil, r- heptalactones, dill oil, Michelia alba leaf oil, neroli oil,
A kind of or arbitrarily than several, solvent in patchouli oil cinnamon oil, rue wood oil, tagetes oil, ginger oil, lovage oil, angelica grosseserrata root tincture
It is made up of absolute ethyl alcohol with propane diols by any ratio.
Step（1）And step（3）800~1200r/min of speed of agitator.
Step（3）Middle vacuum drying chamber drying temperature is 50 DEG C~60 DEG C, and drying time is 24~48h.
The micro-capsule of essence spice for cigarette prepared by the above method by thermogravimetric analysis, the temperature of thermogravimetric analysis for 40 DEG C~
160 DEG C, judge the release temperature and burst size of essence spice for cigarette in micro-capsule.
Uniformly added with the filter rod of essence spice for cigarette temperature control sustained-release micro-capsule, will be carried out with common tow filter rod it is compound,
It is made binary combined filter tip rod, the weight of essence spice for cigarette micro-capsule is 1-5mg/cig in binary combined filter tip rod.
Relative to prior art, the present invention has following remarkable advantage:
1st, cyclo-dextrin-modified chitosan is subjected to micro-capsule embedding, cyclo-dextrin-modified chitosan has ring paste concurrently to essence spice for cigarette
Essence and chitosan double grading, remain the pardon of cyclodextrin and the adsorptivity of chitosan, water-soluble in essence spice for cigarette
Perfume ingredient and fat-soluble perfume ingredient fully can be embedded and are adsorbed in cyclo-dextrin-modified chitosan, and composition is at different temperatures
Release, produce temperature control sustained-release effect；
2nd, the present invention easily generates schiff bases, generation in neutral medium using the amino of chitosan molecule with the reaction with carbonyl
Schiff bases cyclo-dextrin-modified chitosan is made through reducing, reaction condition is gentle, and the cyclo-dextrin-modified chitosan of preparation is used for cigarette
Included with essence and flavoring agent micro-capsule, temperature control sustained-release positive effect.
3rd, compared with prior art is to the Land use systems of essence spice for cigarette, utilization rate is high, cost is low.
Brief description of the drawings
Fig. 1 is the essence spice for cigarette temperature control sustained-release micro-capsule thermogravimetric analysis figure of embodiment 1；
Fig. 2 is the essence spice for cigarette temperature control sustained-release micro-capsule thermogravimetric analysis figure of embodiment 2；
Fig. 3 is the essence spice for cigarette temperature control sustained-release micro-capsule thermogravimetric analysis figure of embodiment 3.
Embodiment
The present invention is further described with reference to embodiment, but protection scope of the present invention is not limited to this.
Embodiment 1：The preparation of No. 101 essence spice for cigarette temperature control sustained-release micro-capsules
（1）200mg chitosans are dissolved in 100mL pH4.4 NaAc_HAc buffer solution, are designated as solution A；By 2g hydroxypropyls
Group-beta-cyclodextrin is dissolved in 50mL water, is designated as B solution；Solution A is mixed with B solution, 1h is stirred at room temperature, adds 300mg boron hydrogen
Change sodium, 800r/min stirs 12h to mixture at room temperature, and pH is adjusted to neutrality, 3000rpm centrifugations with the ammoniacal liquor of volumetric concentration 5%
30min, 50 DEG C of vacuum drying 12h, is made cyclo-dextrin-modified chitosan；
（2）By step（1）The cyclo-dextrin-modified chitosan of preparation is dissolved in the acetum of volumetric concentration 1%, and concentration is made
30mg/mL cyclo-dextrin-modified chitosan solution；
（3）At 30 DEG C, No. 101 essence spice for cigarette drops are added to step（2）In cyclo-dextrin-modified chitosan solution, cigarette is used
Essence and flavoring agent and cyclo-dextrin-modified chitosan solution volume ratio 1:1,800r/min stirring 5h, in being adjusted to 1mol/L sodium hydroxides
Property；Wherein No. 101 essence spice for cigarette liquid include the essence and flavoring agent and 92% solvent of mass percent 8%, and essence and flavoring agent is perfume
Lan Su, cumarin, phenoxyethyl isobutanoate, ethylmaltol, γ-decalactone, Ethyl vanillin, indenes punt-pole oil, yellow chamomile
Oil, coriander oil, linalool, Michelia alba leaf oil, neroli oil, patchouli oil cinnamon oil, rue wood oil, tagetes oil, ginger oil, levisticum officinale
Oil, the mixture of angelica grosseserrata root tincture, solvent is by absolute ethyl alcohol and propane diols by volume 1:1 composition；
（4）Step（3）Obtained solution stands 48h at a temperature of 4 DEG C, separates out and precipitates, after suction filtration, with 10 times of steaming of weight of precipitate
Distilled water is washed, and filter residue is placed on vacuum drying temperature as 50 DEG C, drying time 48h, crosses 20 mesh sieves, obtains essence spice for cigarette
Temperature control sustained-release micro-capsule.
By the essence spice for cigarette temperature control sustained-release micro-capsule of above-mentioned preparation by thermogravimetric analysis, the temperature of thermogravimetric analysis is 40 DEG C
~160 DEG C, thermogravimetric analysis acquired results are shown in Fig. 1, from Fig. 1 it can be found that when temperature is less than 55 DEG C, almost without component
Loss；In 65 DEG C of beginnings, essence starts to volatilize, and during to 95 DEG C, essence volatilization reaches balance.
By 1mg/cig uniformly added with the filter rod of essence spice for cigarette temperature control sustained-release micro-capsule, enter with common tow filter rod
Row is compound, and binary combined filter tip rod is made, and carries out sense organ product suction, and product, which are inhaled, the results are shown in Table 1.
Embodiment 2：The preparation of No. 113 essence spice for cigarette temperature control sustained-release micro-capsules
（1）150mg chitosans are dissolved in 100mL pH 5 NaAc_HAc buffer solution, are designated as solution A；By 1g hydroxypropyls
Group-beta-cyclodextrin is dissolved in 50mL water, is designated as B solution；Solution A is mixed with B solution, 2h is stirred at room temperature, adds 250mg boron hydrogen
Change sodium, 1000r/min stirs 15h to mixture at room temperature, and pH is adjusted to neutrality, 4000rpm centrifugations with the ammoniacal liquor of volumetric concentration 5%
25min, 60 DEG C of vacuum drying 12h, is made cyclo-dextrin-modified chitosan；
（2）By step（1）The cyclo-dextrin-modified chitosan of preparation is dissolved in the acetum of volumetric concentration 2%, and concentration is made
25mg/mL cyclo-dextrin-modified chitosan solution；
（3）At 40 DEG C, No. 113 essence spice for cigarette drops are added to step（2）In cyclo-dextrin-modified chitosan solution, cigarette is used
Essence and flavoring agent and cyclo-dextrin-modified chitosan solution volume ratio 1:2,1000r/min stirring 6h, are adjusted to 1mol/L sodium hydroxides
It is neutral；Wherein No. 113 essence spice for cigarette liquid include the essence and flavoring agent of mass percent 9% and 91% solvent, essence and flavoring agent are
Vanillic aldehyde, cumarin, phenoxyethyl isobutanoate, ethylmaltol, γ-decalactone, Ethyl vanillin, indenes punt-pole oil, nutmeg
Oil, yellow chamomile caul-fat, coriander oil, linalool, mentha piperita oil, r- heptalactones, Michelia alba leaf oil, neroli oil, lovage oil, solely
The mixture of tincture living, solvent is by absolute ethyl alcohol and propane diols by volume 2:1 composition；
（4）Step（3）Obtained solution stands 30h at a temperature of 4 DEG C, separates out and precipitates, after suction filtration, with 15 times of steaming of weight of precipitate
Distilled water is washed, and filter residue is placed on vacuum drying temperature as 60 DEG C, drying time 24h, crosses 30 mesh sieves, obtains essence spice for cigarette
Temperature control sustained-release micro-capsule.
By the essence spice for cigarette temperature control sustained-release micro-capsule of above-mentioned preparation by thermogravimetric analysis, the temperature of thermogravimetric analysis is 40 DEG C
~120 DEG C, thermogravimetric analysis acquired results are shown in Fig. 2, as can be seen from Figure 2：When temperature is less than 45 DEG C, almost without component
Loss；In 70 DEG C of beginnings, essence starts to volatilize, and during to 110 DEG C, essence volatilization reaches balance.
By 3mg/cig uniformly added with the filter rod of essence spice for cigarette temperature control sustained-release micro-capsule, enter with common tow filter rod
Row is compound, and binary combined filter tip rod is made, and carries out sense organ product suction, and product, which are inhaled, the results are shown in Table 1.
Embodiment 3：The preparation of No. 107 essence spice for cigarette temperature control sustained-release micro-capsules
（1）180mg chitosans are dissolved in 100mL pH 4.5 NaAc_HAc buffer solution, are designated as solution A；By 1.5g
Hydroxypropyl-β-cyclodextrin is dissolved in 50mL water, is designated as B solution；Solution A is mixed with B solution, 1.5h is stirred at room temperature, is added
260mg sodium borohydrides, 1200r/min stirs 13h to mixture at room temperature, and pH is adjusted to neutrality with the ammoniacal liquor of volumetric concentration 5%,
5000rpm centrifuges 20min, 55 DEG C of vacuum drying 12h, cyclo-dextrin-modified chitosan is made；
（2）By step（1）The cyclo-dextrin-modified chitosan of preparation is dissolved in the acetum of volumetric concentration 1.5%, and concentration is made
28mg/mL cyclo-dextrin-modified chitosan solution；
（3）At 40 DEG C, No. 107 essence spice for cigarette drops are added to step（2）In cyclo-dextrin-modified chitosan solution, cigarette is used
Essence and flavoring agent and cyclo-dextrin-modified chitosan solution volume ratio 1:3,1200r/min stirring 5h, are adjusted to 1mol/L sodium hydroxides
It is neutral；Wherein No. 107 essence spice for cigarette liquid include the essence and flavoring agent of mass percent 7% and 93% solvent, essence and flavoring agent are
Vanillic aldehyde, cumarin, ethylmaltol, γ-decalactone, Ethyl vanillin, indenes punt-pole oil, mace oil, yellow chamomile caul-fat, coriander
Oil, linalool, mentha piperita oil, r- heptalactones, dill oil, Michelia alba leaf oil, neroli oil, patchouli oil cinnamon oil, rue wood oil
Mixture, solvent is by absolute ethyl alcohol and propane diols by volume 1:2 compositions；
（4）Step（3）Obtained solution stands 24h at a temperature of 4 DEG C, separates out and precipitates, after suction filtration, with 12 times of steaming of weight of precipitate
Distilled water is washed, and filter residue is placed on vacuum drying temperature as 55 DEG C, drying time 30h, crosses 40 mesh sieves, obtains essence spice for cigarette
Temperature control sustained-release micro-capsule.
By the above-mentioned essence spice for cigarette temperature control sustained-release micro-capsule for preparing by thermogravimetric analysis, the temperature of thermogravimetric analysis for 80 DEG C~
150 DEG C, thermogravimetric analysis acquired results are shown in Fig. 3, from Fig. 3 it can be found that when temperature is less than 70 DEG C, almost without component
Loss；In 75 DEG C of beginnings, essence starts to volatilize, and during to 140 DEG C, essence volatilization reaches balance.
By 5mg/cig uniformly added with the filter rod of essence spice for cigarette micro-capsule, compound, system is carried out with common tow filter rod
Binary combined filter tip rod is obtained, carries out sense organ product suction, product, which are inhaled, the results are shown in Table 1.
The sensory evaluating smoking's result statistical form of table 1
Note：It is average value to smoke panel test above to dividing, and the first row data are full marks value, and blank refers to that binary combined filter tip is not used
Rod
The cigarette that addition essence spice for cigarette micro-capsule filter rod is found in sensory evaluating smoking compared with the control, is smelt fragrant nothing and substantially changed,
Illustrate that target essence and flavoring agent has obtained effective embedding and release, microcapsules serve preferable upgrading effect to cigarette smoke.
Claims (4)
1. a kind of preparation method of essence spice for cigarette temperature control sustained-release micro-capsule, it is characterised in that comprise the following steps：
（1）150-200mg chitosans are dissolved in 100mL pH4.4-5.0 NaAc_HAc buffer solution, are designated as solution A；
1-2g hydroxypropyl-β-cyclodextrins are dissolved in 50mL water, are designated as B solution；Solution A is mixed with B solution, 1-2h is stirred at room temperature,
Add 250-300mg sodium borohydrides, mixture stirs 12-15h at room temperature, and pH is adjusted to neutrality with ammoniacal liquor, 3000-5000 rpm from
Heart 20-30min, 50-60 DEG C of vacuum drying, is made cyclo-dextrin-modified chitosan；
（2）By step（1）Cyclo-dextrin-modified chitosan is dissolved in volumetric concentration 1-2% acetum, be made concentration 25~
30mg/mL cyclo-dextrin-modified chitosan solution；
（3）At 30 DEG C~40 DEG C, essence spice for cigarette drop is added to step（2）In cyclo-dextrin-modified chitosan solution, stir
5~6h is mixed, pH is adjusted to neutrality, wherein essence spice for cigarette and cyclo-dextrin-modified chitosan solution volume with sodium hydroxide solution
Than for 1:1-1:3；
（4）Step（3）Obtained solution stands 24~48h at 4 DEG C, separates out and precipitates, true with distillation water washing, filter residue after suction filtration
After sky is dried, 20-40 mesh sieves are crossed, obtain essence spice for cigarette temperature control sustained-release micro-capsule.
2. the preparation method of essence spice for cigarette temperature control sustained-release micro-capsule according to claim 1, it is characterised in that：Step
（1）And step（3）Middle 800~1200r/min of speed of agitator.
3. preparation method according to claim 1, it is characterised in that：Essence spice for cigarette liquid does not surpass including mass percent
10% essence and flavoring agent and solvent is crossed, wherein essence and flavoring agent includes vanillic aldehyde, cumarin, phenoxyethyl isobutanoate, ethyl malt
Phenol, γ-decalactone, Ethyl vanillin, indenes punt-pole oil, mace oil, yellow chamomile caul-fat, coriander oil, linalool, mentha piperita oil,
R- heptalactones, dill oil, Michelia alba leaf oil, neroli oil, patchouli oil cinnamon oil, rue wood oil, tagetes oil, ginger oil, levisticum officinale
Oil, a kind of in angelica grosseserrata root tincture or arbitrarily than several, solvent is made up of absolute ethyl alcohol with propane diols by any ratio.
4. the preparation method of essence spice for cigarette temperature control sustained-release micro-capsule according to claim 1, it is characterised in that：Step
（4）In vacuum drying drying temperature be 50 DEG C~60 DEG C, drying time is 24~48h.
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