CN115433634A - Alkali modified visual coloring flavor sustained-release particles and preparation method and application thereof - Google Patents
Alkali modified visual coloring flavor sustained-release particles and preparation method and application thereof Download PDFInfo
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- CN115433634A CN115433634A CN202210981193.8A CN202210981193A CN115433634A CN 115433634 A CN115433634 A CN 115433634A CN 202210981193 A CN202210981193 A CN 202210981193A CN 115433634 A CN115433634 A CN 115433634A
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- 239000002245 particle Substances 0.000 title claims abstract description 90
- 239000000796 flavoring agent Substances 0.000 title claims abstract description 48
- 235000019634 flavors Nutrition 0.000 title claims abstract description 48
- 230000000007 visual effect Effects 0.000 title claims abstract description 42
- 238000004040 coloring Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000003513 alkali Substances 0.000 title claims abstract description 22
- 238000013268 sustained release Methods 0.000 title description 13
- 239000012730 sustained-release form Substances 0.000 title description 13
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 16
- 239000011147 inorganic material Substances 0.000 claims abstract description 16
- 239000012670 alkaline solution Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000008187 granular material Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 9
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- 238000000034 method Methods 0.000 claims description 30
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
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- 238000004519 manufacturing process Methods 0.000 claims description 11
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 10
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- 229910000278 bentonite Inorganic materials 0.000 claims description 8
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 8
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 8
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 8
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- 229910052901 montmorillonite Inorganic materials 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 5
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- 229940005550 sodium alginate Drugs 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 244000215068 Acacia senegal Species 0.000 claims description 4
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- 235000013073 Acorus gramineus Nutrition 0.000 claims description 4
- 244000037364 Cinnamomum aromaticum Species 0.000 claims description 4
- 235000014489 Cinnamomum aromaticum Nutrition 0.000 claims description 4
- 229920000858 Cyclodextrin Polymers 0.000 claims description 4
- 229920000084 Gum arabic Polymers 0.000 claims description 4
- 240000000851 Vaccinium corymbosum Species 0.000 claims description 4
- 235000003095 Vaccinium corymbosum Nutrition 0.000 claims description 4
- 235000017537 Vaccinium myrtillus Nutrition 0.000 claims description 4
- 235000010489 acacia gum Nutrition 0.000 claims description 4
- 239000000205 acacia gum Substances 0.000 claims description 4
- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 claims description 4
- 235000021014 blueberries Nutrition 0.000 claims description 4
- 239000010634 clove oil Substances 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 4
- 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 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 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
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 claims description 4
- 235000012141 vanillin Nutrition 0.000 claims description 4
- 235000010418 carrageenan Nutrition 0.000 claims description 3
- 239000000679 carrageenan Substances 0.000 claims description 3
- 229920001525 carrageenan Polymers 0.000 claims description 3
- 229940113118 carrageenan Drugs 0.000 claims description 3
- 150000004666 short chain fatty acids Chemical class 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000007598 dipping method Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 25
- 239000003086 colorant Substances 0.000 abstract description 4
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 29
- 230000000052 comparative effect Effects 0.000 description 17
- 239000003205 fragrance Substances 0.000 description 17
- 239000000779 smoke Substances 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 9
- 238000005469 granulation Methods 0.000 description 7
- 230000003179 granulation Effects 0.000 description 7
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 6
- 229960002715 nicotine Drugs 0.000 description 6
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 6
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- 239000000126 substance Substances 0.000 description 5
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 4
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 4
- 239000011324 bead Substances 0.000 description 4
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- 238000010586 diagram Methods 0.000 description 4
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- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
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- 239000013589 supplement Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000001055 blue pigment Substances 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 description 2
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
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- 241000228347 Monascus <ascomycete fungus> Species 0.000 description 1
- FLAQQSHRLBFIEZ-UHFFFAOYSA-N N-Methyl-N-nitroso-4-oxo-4-(3-pyridyl)butyl amine Chemical compound O=NN(C)CCCC(=O)C1=CC=CN=C1 FLAQQSHRLBFIEZ-UHFFFAOYSA-N 0.000 description 1
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- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- UIMOJFJSJSIGLV-JNHMLNOCSA-N carumonam Chemical compound O=C1N(S(O)(=O)=O)[C@H](COC(=O)N)[C@@H]1NC(=O)C(=N/OCC(O)=O)\C1=CSC(N)=N1 UIMOJFJSJSIGLV-JNHMLNOCSA-N 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 235000019645 odor Nutrition 0.000 description 1
- 239000001053 orange pigment Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- AXFBAIOSECPASO-UHFFFAOYSA-N pentacyclo[6.6.2.02,7.04,16.011,15]hexadeca-1(14),2(7),3,5,8(16),9,11(15),12-octaene Chemical compound C1=C(C=C23)C4=C5C3=CC=CC5=CC=C4C2=C1 AXFBAIOSECPASO-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
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- 238000012827 research and development Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical compound O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 description 1
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- 230000002459 sustained effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- A24D1/04—Cigars; Cigarettes with mouthpieces or filter-tips
-
- 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
- A24D1/20—Cigarettes specially adapted for simulated smoking devices
-
- 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
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/02—Manufacture of tobacco smoke filters
- A24D3/0204—Preliminary operations before the filter rod forming process, e.g. crimping, blooming
- A24D3/0212—Applying additives to filter materials
- A24D3/0225—Applying additives to filter materials with solid additives, e.g. incorporation of a granular product
-
- 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
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/17—Filters specially adapted for simulated smoking devices
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)
- Fats And Perfumes (AREA)
- Seasonings (AREA)
Abstract
The invention provides an alkali modified visual coloring flavor slow-release granule as well as a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) Mixing and stirring an inorganic material and an alkaline solution, then washing with water, and mixing with a thickening agent, a pigment and an auxiliary agent to obtain a suspension; (2) Dropwise adding the suspension obtained in the step (1) into a calcium salt solution, standing to obtain a first material, washing with water, and soaking with an acid solution to obtain visible particles; (3) And (3) mixing the visual particles obtained in the step (2) with essence and/or spice to obtain the alkali modified visual coloring flavor slow-release particles. The alkali modified visual coloring aroma slow-release particles provided by the invention have the advantages of good appearance effect, high granularity, high uniformity, low pulverization rate, high product quality, high biological safety and good flavoring effect, and can endow the particles with bright colors, improve the aesthetic feeling of the appearance, and simultaneously cooperate with the control of color and type feeling matching of essence, thereby improving the use experience.
Description
Technical Field
The invention belongs to the field of cigarette manufacturing, particularly relates to alkali modified visual coloring flavor sustained-release particles and a preparation method and application thereof, and particularly relates to alkali modified visual coloring flavor sustained-release particles with a good appearance effect and a preparation method and application thereof.
Background
With the advance of tar and harm reduction, the tar content in cigarette smoke is continuously reduced, and the requirements on cigarette aroma enhancement and supplement technologies are higher and higher, so that the research and development of the filter tip aroma enhancement and supplement method are rapidly developed, and the technologies including tow aroma enhancement, aroma line, bead explosion, dropping pill, microcapsule, nanoparticle and the like are developed and applied. However, these techniques have certain disadvantages, such as poor long-term storage fragrance stability of filament bundles and aromatic threads, high cost of bead blasting and dropping pills, and introduction of other unpleasant odors, and potential safety hazard of lung inhalation of microcapsules and nanoparticles. New technologies of flavor slow-release particles have recently been developed in the industry, such as flavor slow-release agent particles for cigarette filters (201510300776. X, 201610488221.7), porous solid flavor beads for cigarettes (201910888311.9), large particle solid flavor bead cigarette filter sticks (201810886849.1, 2018000887493.3, 201810887483.x, 2019000314422.9, 201910314412.5, 201810885888.x, 201811016014.7) and the like.
However, the existing technology for manufacturing the aroma slow-release particles has some defects: granulating by adopting a common extrusion method, a spray drying method, a granulator granulation method and the like, wherein the obtained granules have small granularity, low roundness and slightly poor hardness; if the granularity or roundness is improved, the production cycle is greatly prolonged, and if the hardness of the particles is ensured, the density is increased and the essence adsorption capacity is reduced; by adopting the improved large-particle granulation method, although the granularity and the roundness of the obtained particles are obviously improved, the production period is as long as 2-4 days, and the batch preparation capability is weak. In addition, the particles prepared by the prior art have dark color, or colorless/light color, or poor color uniformity, so the appearance character is not good, and the particles are not suitable for manufacturing visual filters. Therefore, how to provide a filter tip aroma enhancement and supplement product with good appearance effect, simple and quick preparation process and good essence adsorption capacity becomes a problem to be solved urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide alkali modified visual coloring fragrance sustained-release particles and a preparation method and application thereof, and particularly provides alkali modified visual coloring fragrance sustained-release particles with good appearance effect and a preparation method and application thereof. The alkali modified visual coloring flavor slow-release granule provided by the invention has the advantages of good appearance effect, high granularity, high uniformity, low breakage rate, high product quality, high biological safety and good flavoring effect, can endow the granule with bright color, improves the appearance aesthetic feeling, and can be matched with the type feeling of the color and the essence to control the matching, thereby improving the use experience.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of alkali modified visual coloring flavor slow-release particles, which comprises the following steps:
(1) Mixing and stirring an inorganic material and an alkaline solution, then washing with water, and mixing with a thickening agent, a pigment and an auxiliary agent to obtain a suspension;
(2) Dropwise adding the turbid liquid obtained in the step (1) into a calcium salt solution, standing to obtain a first material, washing the first material with water, and soaking the first material with an acid solution to obtain visible particles;
(3) And (3) mixing the visual particles obtained in the step (2) with essence and/or spice to obtain the alkali modified visual coloring flavor slow-release particles.
In the method, the suspension is dropwise added into the calcium salt solution, so that the suspension liquid drops expand and are solidified into particles, and the solidified particles not only have higher porosity than the stirring granulation adsorption material, but also are beneficial to storage and slow release of the fragrance components; but also the expansion and solidification operation leaves operable space for the addition of other auxiliary agents, and other materials without adsorption pores can construct particle pores in the particle expansion process, thereby reducing the influence of the addition of other substances on the slow release effect of the particle fragrance; the product is modified by alkaline substances, so that the dyeing effect of the particles can be effectively improved, the color of the particles is uniform, bright and beautiful, special colors such as azure, bright yellow and the like are obtained, the color can be controlled to be matched with the variety of essence, and the use experience is improved; the method can eliminate partial auxiliary components in the product by soaking in acid solution, improve product porosity and perfuming effect, and avoid damage to pigment without influence on dyeing effect; the final product has good appearance effect, high granularity and uniformity, low fragmentation rate, high product quality, high biological safety and good flavoring effect.
Preferably, the inorganic material in step (1) includes any one or a combination of at least two of bentonite, molecular sieve or diatomite, such as a combination of bentonite and molecular sieve, a combination of molecular sieve and diatomite or a combination of bentonite and diatomite, but not limited to the above-listed combinations, and other combinations not listed in the above-mentioned combination range are also applicable, and the combination of bentonite and diatomite is preferred.
Preferably, the bentonite comprises any one of montmorillonite, clay or modified bentonite.
Preferably, the molecular sieve comprises a zeolite.
Preferably, the alkaline solution in step (1) includes any one or a combination of at least two of an aqueous ammonia solution, a sodium hydroxide solution, and an ammonia-ammonium chloride mixed solution, such as a combination of an aqueous ammonia solution and a sodium hydroxide solution, a combination of a sodium hydroxide solution and an ammonia-ammonium chloride mixed solution, or a combination of an ammonia-ammonium chloride mixed solution and an aqueous ammonia solution, but is not limited to the above-listed combinations, and other combinations not listed within the above-mentioned combination range are also applicable, and a combination of an aqueous ammonia solution and a sodium hydroxide solution is preferred.
Preferably, the pH value of the alkaline solution in the step (1) is 11-13.
Preferably, the time for mixing and stirring with the alkaline solution in the step (1) is 1-5h.
The pH of the alkaline solution may be 11, 11.5, 12, 12.5 or 13, and the mixing time with the alkaline solution may be 1 hour, 2 hours, 3 hours, 4 hours or 5 hours, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Preferably, the thickening agent in step (1) comprises any one or combination of at least two of sodium alginate, gum arabic, cyclodextrin or carrageenan, such as combination of sodium alginate and gum arabic, combination of gum arabic and cyclodextrin or combination of cyclodextrin and carrageenan, etc., but is not limited to the above-listed combination, and other combinations not listed in the above-mentioned combination range are also applicable.
Preferably, the auxiliary agent in step (1) includes any one of sodium carbonate, sodium thiosulfate or potassium carbonate or a combination of at least two of them, such as a combination of sodium carbonate and sodium thiosulfate, a combination of sodium carbonate and potassium carbonate or a combination of potassium carbonate and sodium thiosulfate, etc., but is not limited to the above-listed combinations, and other combinations not listed in the above-mentioned combination range are also applicable.
Preferably, the feed-liquid ratio of the inorganic material to the alkaline solution in the step (1) is 1 (10-50) g/mL.
Preferably, the mass ratio of the inorganic material to the thickening agent in the step (1) is (8-18): 1.
Preferably, the mass ratio of the inorganic material to the auxiliary agent in the step (1) is (10-50): 1.
Preferably, the mass ratio of the inorganic material to the pigment in the step (1) is (30-300): 1.
Preferably, the dropping rate of the step (2) is 10-150 drops/min, and the volume of each drop of suspension is 0.04-0.1mL.
Preferably, the mass fraction of the calcium salt solution in the step (2) is 0.5-15%.
Preferably, the time period for the standing in the step (2) is at least 30min.
Preferably, the acid in step (2) is a short chain fatty acid, and the short chain fatty acid includes any one or a combination of at least two of acetic acid, propionic acid or isobutyric acid, such as a combination of acetic acid and propionic acid, a combination of propionic acid and isobutyric acid, or a combination of isobutyric acid and acetic acid, but is not limited to the above-listed combinations, and other combinations not listed in the above-listed combinations are also applicable.
Preferably, the mass fraction of the acid solution in the step (2) is 0.1-5%.
Preferably, the soaking time of the step (2) with the acid solution is 10-60min.
Wherein the stock solution ratio of inorganic material and alkaline solution is 1:10g/mL, 1:15g/mL, 1:20g/mL, 1:25g/mL, 1:30g/mL, 1:35g/mL, 1:40g/mL, 1:45g/mL, etc., and the mass ratio of inorganic material to thickener may be 8: the volume of each drop of the suspension may be 0.04mL, 0.05mL, 0.06mL, 0.07mL, 0.08mL, 0.09mL, or 0.1mL, etc., the mass fraction of the calcium salt solution may be 0.5%, 1%, 3%, 5%, 7%, 9%, 11%, 13%, or 15%, etc., the standing time may be 30min, 40min, 50min, 60min, 70min, 80min, or 90min, etc., the mass fraction of the acid solution may be 0.1%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%, etc., the soaking time with the acid solution may be 10min, 20min, 30min, 40min, 50min, or 60min, etc., but the above-mentioned values are not limited thereto, and other values not mentioned in the above-mentioned range of values are also applicable.
Preferably, the specific step of mixing in step (3) comprises spraying the perfume onto the surface of the visible particles or immersing the visible particles in a perfume solution.
Preferably, the essence in step (3) comprises any one or a combination of at least two of clove oil, grass-leaved sweetflag oil or cassia oil, such as clove oil and grass-leaved sweetflag oil, clove oil and cassia oil or grass-leaved sweetflag oil and cassia oil, but not limited to the above-listed combinations, and other combinations not listed in the above-mentioned combination range are also applicable.
Preferably, the flavor includes any one or combination of at least two of blueberry powder, radix angelicae pubescentis powder or vanillin, such as a combination of blueberry powder and radix angelicae pubescentis powder, a combination of radix angelicae pubescentis powder and vanillin, or a combination of blueberry powder and vanillin, and the like, but is not limited to the above-listed combinations, and other combinations not listed in the above-listed combination range are also applicable.
In a second aspect, the invention provides the alkali-modified visual coloring flavor slow-release particles prepared by the preparation method.
In a third aspect, the invention also provides the application of the alkali modified visual coloring flavor slow-release particles in preparing cigarettes.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides alkali modified visual coloring flavor slow-release particles, which are characterized in that suspension liquid drops are expanded and solidified into particles by adopting a method of dropwise adding suspension liquid into a calcium salt solution, and the solidified particles not only have higher porosity compared with a stirring granulation adsorption material, but also are beneficial to storage and slow release of flavor components; but also the expansion and solidification operation leaves operable space for the addition of other auxiliary agents, and other materials without adsorption pores can construct particle pores in the particle expansion process, thereby reducing the influence of the addition of other substances on the slow release effect of the particle fragrance; the product is modified by alkaline substances, so that the dyeing effect on the particles can be effectively improved, the particles are uniform, bright and beautiful in color, special colors such as azure, bright yellow and the like are obtained, the color can be controlled to be matched with the variety of the essence, and the use experience is improved; the method can eliminate partial auxiliary components in the product by soaking in acid solution, improve product porosity and perfuming effect, and avoid damage to pigment without influence on dyeing effect; the final product has good appearance effect, high granularity and uniformity, low fragmentation rate, high product quality, high biological safety and good flavoring effect. The product can be applied to cigarettes, including conventional cigarettes and heating cigarettes, and can endow the product with more vivid characteristics to obtain consumer acceptance through the sustained and effective release of aroma components and the strengthening of aroma memory through the color matched with aroma characteristics.
Drawings
FIG. 1 is an appearance view of modified visually coloring flavor-releasing particles provided in examples 1 to 3, example 1, example 2 and example 3 being sequentially from left to right;
FIG. 2 is an appearance diagram of a modified visual flavor-releasing particle provided in comparative example 1;
FIG. 3 is an appearance diagram of a modified visual flavor-releasing particle provided in comparative example 2;
FIG. 4 is an appearance diagram of a modified visual flavor-releasing particle provided in comparative example 3;
FIG. 5 is a schematic structural view of a visual filter cigarette made in a sensory evaluation;
fig. 6 is an appearance diagram of a visual filter cigarette manufactured in sensory evaluation.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
In the following examples, brilliant blue pigment and orange edible pigment were obtained from Jiangsu Meyzobium Biotech Inc., the monascus red pigment is purchased from Ministry of agriculture and sidelines products of Sedan and Zhencang province in Pinnan county.
Example 1
The embodiment provides an alkali modified visual coloring flavor sustained-release particle, and the preparation method comprises the following steps:
the preparation method comprises the following steps of (1) smashing an inorganic material (a mixture of montmorillonite and diatomite in a mass ratio of 1) into powder, mixing the powder with an ammonia water-sodium hydroxide mixed solution with a pH value of 12 (ammonia water and sodium hydroxide molar ratio is 1.
Example 2
The embodiment provides an alkali modified visual coloring flavor slow-release granule, which is prepared by the following steps:
the preparation method comprises the following steps of grinding montmorillonite into powder, mixing the powder with an ammonia water solution with a pH value of 11 (material-liquid ratio is 1.
Example 3
The embodiment provides an alkali modified visual coloring flavor slow-release granule, which is prepared by the following steps:
grinding zeolite into powder, mixing with a sodium hydroxide solution with a pH value of 13 (material-liquid ratio is 1.
Example 4
This example provides an alkali-modified visually colored flavor-releasing granule, which is prepared in the same manner as in example 1, except that diatomaceous earth is replaced with an equal amount of montmorillonite.
Example 5
The embodiment provides an alkali modified visual coloring flavor slow-release granule, and the preparation method is the same as that of the embodiment 1 except that the montmorillonite is replaced by the same amount of diatomite.
Example 6
This example provides an alkali-modified visually colored flavor-releasing granule, which is prepared in the same manner as in example 1 except that ammonia water is replaced with sodium hydroxide in an equal amount.
Example 7
The embodiment provides an alkali-modified visual coloring flavor slow-release granule, and the preparation method is the same as that of the embodiment 1 except that the same amount of ammonia water is used for replacing sodium hydroxide.
Example 8
This example provides modified visually colored flavor-releasing particles prepared according to the method of example 1, except that the parameters of the drop addition are 170 drops/min, and the volume of each drop is 0.12 mL.
Example 9
This example provides modified visually coloured flavour-releasing particles prepared in accordance with example 1 except that acetic acid was replaced by an equal amount of sulphuric acid.
Comparative example 1
This comparative example provides a modified visual flavor release particle, which was identical to example 1 except that no brilliant blue pigment was added in the preparation steps.
Comparative example 2
The comparative example provides modified visual fragrance sustained-release granules which are prepared by adopting a common granulation method, and the preparation method comprises the following steps:
mixing montmorillonite with sodium alginate, sodium carbonate and water (the mixture ratio of the materials is the same as that in example 1, and the addition amount of the water is the paste of the slurry), so as to obtain slurry; stirring the mixture for 2 hours by adopting a stirring granulation method, and then granulating on a swinging granulator; and mixing the obtained particles with menthol to obtain the visual fragrance sustained-release particles, thus obtaining the modified visual fragrance sustained-release particles.
Comparative example 3
The comparative example provides a modified visual flavor sustained-release granule, which is prepared by adopting a spherical mold compression molding method, and the preparation method comprises the following steps:
mixing and grinding montmorillonite, sodium alginate, sodium carbonate and water (the mixture ratio of the materials is consistent with that in example 1, and the adding amount of the water is to make the slurry pasty) to obtain slurry; sieving the slurry, pouring the slurry into a spherical mold for compression molding, drying at the temperature of below 25 ℃ for 24 hours, and drying at the temperature of 45 ℃ for 3 hours to obtain a spherical blank; calcining the spherical embryo body at 1300 ℃ for 4 hours to obtain slow-release particles; and soaking the obtained particles in orange pigment solution, drying, and mixing with menthol to obtain the modified visual fragrance sustained-release particles.
In the products of examples 1-3 and comparative example 1, the particles of example 1 are azure, the particles of example 2 are bright yellow, and the particles of example 3 are pale pink (the appearance of the products of examples 1-3 is shown in fig. 1, and example 1, example 2 and example 3 are in order from left to right); while comparative example 1 is white (as shown in fig. 2); the appearance of comparative example 2 is shown in fig. 3, the morphology difference between the products is large, and the products are not round and have poor appearance; the appearance of comparative example 3 is shown in fig. 4, and although the roundness and uniformity of the particles are good, the color between the particles is not uniform, most of the particles are white, part of the particles are yellowish to yellow, the dyeing effect is poor, the appearance is poor, the manufacturing period is as long as 3 days, and the mass production capacity is limited by the number of molds; the product particles disclosed by the invention have better appearance effect, are mellow and have small difference, can be endowed with bright and beautiful colors, are more attractive, can be matched with the type feeling of essence, and can be used for improving the use experience.
Appearance evaluation:
the products provided in examples 1 to 5 and 8 and comparative examples 2 to 3 were evaluated for appearance properties by the following methods:
(1) The particle size and roundness detection method comprises the following steps: the alkali-modified visually colored flavor-releasing particles and a steel ruler were placed on a flat plate (white plate for dark particles and blue plate for light particles). Using high-pixel imaging equipment to collect pictures, and then adopting Image J software to analyze the pictures so as to obtain the particle projection area (mm) 2 ) And then, calculating the particle size and the roundness of the particles, wherein the particle size is represented by a particle projection area, and the roundness of the particles is represented by a circle area ratio (circle area ratio = projection area/maximum circle area).
(2) The particle breakage rate detection method comprises the following steps: the alkali modified visual coloring fragrance slow-release particles are put into a box with a cover, and the volume of the particles accounts for less than 10% of the volume of the box. After the box cover is covered, the box is placed into a rotating box, and then the collision condition possibly met by the particles in the storage and transportation process is simulated by adopting a rotating box method according to YC/T151.2-2001 standard. After the rotation, the particles in the box are taken out and sieved, and the weight difference of the particles before and after the rotation is weighed and calculated, so that the particle crushing rate in the rotation process is obtained. And evaluating the hardness of the particles and the applicability of the particles in the processes of production, storage and transportation by using the particle crushing rate.
The results are as follows:
the data show that compared with the common granulation method, the product provided by the invention can obviously improve the granularity, the uniformity and the roundness of the product, reduce the crushing rate and obviously improve the product quality; meanwhile, the roundness of the product can be obviously improved by controlling the dripping parameters, and the appearance effect is improved; in comparative example 3, although the appearance and quality of the product are also excellent, the production cycle of the ball die press molding method is long, and the mass production capability is poor.
And (3) safety evaluation:
the products provided in examples 1-3 and comparative examples 2-3 (with the weight of the added particles being 0.135-0.145 g) were respectively put into a hollow filter cigarette to prepare a visual filter cigarette (the structure of the cigarette filter is that, starting from the end of the filter, 15mm tow segment +5mm hollow segment +10mm tow segment, alkali-modified visual coloring flavor slow-release particles are completely filled into the hollow segment), and the visual filter cigarette and a blank sample (the filter is a 30mm acetate filter without adding any particles) are subjected to smoke components released during burning, so that the safety of the visual particles is analyzed in comparison, and the detection method is as follows:
(1) The tar, nicotine and moisture of the cigarette are measured according to GB/T19609-2004, GB/T23203.1-2008 and GB-T23355-2009. And respectively measuring the release amount of 7 harmful components such as mainstream smoke CO, benzo [ alpha ] pyrene (Ba P), HCN, NNK, ammonia, phenol, crotonaldehyde and the like of the cigarette sample according to the measuring methods of GB/T23356-2009, GB/T21130-2007, YC/T253-2019, CRMN DEG 75, YC/T377-2019, YC/T255-2008 and YC/T254-2008, and calculating the hazard index H value of the cigarette sample by adopting a Shehler formula according to the method of tobacco and smoke chemical components. Since the physiological satisfaction of different cigarette samples is different, the different samples are compared in the transverse direction using the unit nicotine value according to the WHO evaluation method ("a certain component value of the unit nicotine = the component detection value/nicotine value").
(2) And carrying out biological evaluation on the smoke safety according to YQ/T42-2013, YQ 3-2011 and YQ/T43-2013.
The data show that the product provided by the invention does not bring negative effects to cigarette samples, improves the smoking safety of the cigarette samples, can selectively reduce the effects of CO, ammonia and BaP, has a certain reduction effect on NNK and crotonaldehyde, can obviously reduce the H value of nicotine per unit, reduces the harmfulness of smoke, can improve the IC50 value of 24H cells of the smoke through specific modification, and can reduce the biological toxicity of the smoke to a certain extent.
Sensory evaluation:
visual filter cigarettes were prepared by putting the products provided in examples 1-3, 6-7, 9 and comparative examples 2-3 into cavity filter cigarettes, respectively (the structure of the cigarette filter was that, starting from the end of the filter, 15mm tow segments +5mm cavity segments +10mm tow segments, alkali-modified visually colored flavor-releasing particles were completely filled into the cavity segments, the schematic structure thereof is shown in fig. 2, the appearance thereof is shown in fig. 3, and the blank sample was 30mm acetate filter without any particles added). And (3) evaluating the cigarettes and the blank samples by a person qualified for professional cigarette sensory evaluation by adopting a flavor profile analysis method, and recording the result. The 13 indexes of the smoke characteristics are scored (according to the scoring standard established by YC/T497-2014), and the perfuming strength and the suitability are evaluated. The score is divided into unit increments of 0.5, the score is divided into 10 points, and finally the result is averaged, and 1 decimal place is reserved. The results are as follows:
the data show that the product provided by the invention can effectively improve the quality of smoke, endow the cigarette with more obvious additional fragrance, and has no great negative influence on the harmony of the smoke.
Evaluation of fragrance sustained-release capability:
cigarette samples prepared by the sensory evaluation are taken as objects (filter flavoring is carried out on blank samples in a tow spraying mode), a rotary disc smoking machine (model RM20H manufactured by Borgwoldt KC Instrument company) is adopted, and tar, nicotine and moisture on the cigarette mouth-by-mouth smoke trapping filter sheet are measured by referring to GB/T19609-2004, GB/T23203.1-2008 and GB-T23355-2009. Referring to YCT 286-2009, the content of the flavor components on the cigarette mouth-by-mouth smoke trapping filter sheet is determined by an external menthol sample preparation mode (the flavor and the aroma in all particles are replaced by the same amount of menthol). The matching of the visual granular flavor slow-release capacity and the smoke is analyzed by adopting the ratio of the mouth-by-mouth flavor component ratio (single-mouth flavor component content/total flavor component content) to the mouth-by-mouth tar ratio (single-mouth tar content/total tar content):
according to the data, the matching performance of the fragrance component slow-release capacity and the mouth-to-mouth smoke concentration of the visual fragrance slow-release particles provided by the invention is good, except for the first mouth (ignition suction mouth), the ratio of the fragrance component concentration to the tar concentration is stabilized within the range of 0.82-1.17, the fragrance slow-release capacity is good, and the requirements of essence slow-release materials are met.
The applicant states that the alkali modified visual coloring flavor slow-release particles and the preparation method and application thereof are described by the above examples, but the invention is not limited to the above examples, i.e. the invention is not meant to be implemented only by relying on the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that, in the above embodiments, the various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, the present invention does not separately describe various possible combinations.
Claims (10)
1. A preparation method of alkali modified visual coloring flavor slow-release particles is characterized by comprising the following steps:
(1) Mixing and stirring an inorganic material and an alkaline solution, then washing with water, and mixing with a thickening agent, a pigment and an auxiliary agent to obtain a suspension;
(2) Dropwise adding the suspension obtained in the step (1) into a calcium salt solution, standing to obtain a first material, washing the first material with water, and soaking the first material with an acid solution to obtain visible particles;
(3) And (3) mixing the visual particles obtained in the step (2) with essence and/or spice to obtain the alkali modified visual coloring flavor slow-release particles.
2. The method according to claim 1, wherein the inorganic material in step (1) comprises any one of bentonite, molecular sieve or diatomite or a combination of at least two of them, preferably a combination of bentonite and diatomite;
preferably, the bentonite comprises any one of montmorillonite, clay or modified bentonite;
preferably, the alkaline solution in step (1) comprises any one of or a combination of at least two of an aqueous ammonia solution, a sodium hydroxide solution and an ammonia-ammonium chloride mixed solution, preferably a combination of the aqueous ammonia solution and the sodium hydroxide solution;
preferably, the pH value of the alkaline solution in the step (1) is 11-13;
preferably, the mixing and stirring time of the alkaline solution in the step (1) is 1-5h.
3. The preparation method according to claim 1 or 2, wherein the thickening agent in step (1) comprises any one or a combination of at least two of sodium alginate, gum arabic, cyclodextrin or carrageenan;
preferably, the auxiliary agent in step (1) comprises any one or a combination of at least two of sodium carbonate, sodium thiosulfate and potassium carbonate.
4. The method according to any one of claims 1 to 3, wherein the feed-to-liquid ratio of the inorganic material to the alkaline solution in step (1) is 1 (10 to 50) g/mL;
preferably, the mass ratio of the inorganic material to the thickening agent in the step (1) is (8-18): 1;
preferably, the mass ratio of the inorganic material to the auxiliary agent in the step (1) is (10-50): 1;
preferably, the mass ratio of the inorganic material to the pigment in the step (1) is (30-300): 1.
5. The method according to any one of claims 1 to 4, wherein the dropping in step (2) is carried out at a rate of 10 to 150 drops/min, and the volume of each drop of the suspension is 0.04 to 0.1mL;
preferably, the mass fraction of the calcium salt solution in the step (2) is 0.5-15%.
6. The method according to any one of claims 1 to 5, wherein the standing time in the step (2) is at least 30min;
preferably, the acid of step (2) is a short chain fatty acid comprising any one of acetic acid, propionic acid or isobutyric acid or a combination of at least two thereof;
preferably, the mass fraction of the acid solution in the step (2) is 0.1-5%;
preferably, the soaking time of the step (2) with the acid solution is 10-60min.
7. The method for preparing a perfume composition according to any one of claims 1 to 6, wherein the specific step of mixing in step (3) comprises spraying a perfume onto the surface of the visible particles or dipping the visible particles into a perfume solution.
8. The method for preparing the compound of any one of claims 1 to 7, wherein the essence of step (3) comprises any one or a combination of at least two of clove oil, grass-leaved sweetflag oil or cassia oil;
preferably, the spice comprises any one or a combination of at least two of blueberry powder, radix angelicae pubescentis powder or vanillin.
9. An alkali-modified visually coloring flavor-releasing granule produced by the production method according to any one of claims 1 to 8.
10. Use of the alkali-modified visually coloured flavor release particles according to claim 8 in the preparation of a cigarette.
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