CN115612556B - Natural spice, preparation method thereof and application thereof in tobacco - Google Patents
Natural spice, preparation method thereof and application thereof in tobacco Download PDFInfo
- Publication number
- CN115612556B CN115612556B CN202211147283.3A CN202211147283A CN115612556B CN 115612556 B CN115612556 B CN 115612556B CN 202211147283 A CN202211147283 A CN 202211147283A CN 115612556 B CN115612556 B CN 115612556B
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- color
- spice
- morning glory
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- ethanol
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- 235000013599 spices Nutrition 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 235000002637 Nicotiana tabacum Nutrition 0.000 title description 5
- 241000208125 Nicotiana Species 0.000 title 1
- 240000001549 Ipomoea eriocarpa Species 0.000 claims abstract description 124
- 235000005146 Ipomoea eriocarpa Nutrition 0.000 claims abstract description 124
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 97
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000000855 fermentation Methods 0.000 claims abstract description 26
- 230000004151 fermentation Effects 0.000 claims abstract description 26
- 239000002304 perfume Substances 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 239000003480 eluent Substances 0.000 claims abstract description 7
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- 238000011068 loading method Methods 0.000 claims abstract description 5
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
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- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 8
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 8
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- 238000004108 freeze drying Methods 0.000 claims description 7
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 244000061176 Nicotiana tabacum Species 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000001963 growth medium Substances 0.000 description 4
- 244000063299 Bacillus subtilis Species 0.000 description 3
- 235000014469 Bacillus subtilis Nutrition 0.000 description 3
- 241000191998 Pediococcus acidilactici Species 0.000 description 3
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 3
- 239000011449 brick Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 229920001353 Dextrin Polymers 0.000 description 2
- 239000004375 Dextrin Substances 0.000 description 2
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 description 2
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 244000038561 Modiola caroliniana Species 0.000 description 2
- 235000010703 Modiola caroliniana Nutrition 0.000 description 2
- 241001547082 Pseudobacillus Species 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
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- 239000003381 stabilizer Substances 0.000 description 2
- 235000019640 taste Nutrition 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- WLYGSPLCNKYESI-RSUQVHIMSA-N Carthamin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1[C@@]1(O)C(O)=C(C(=O)\C=C\C=2C=CC(O)=CC=2)C(=O)C(\C=C\2C([C@](O)([C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(O)=C(C(=O)\C=C\C=3C=CC(O)=CC=3)C/2=O)=O)=C1O WLYGSPLCNKYESI-RSUQVHIMSA-N 0.000 description 1
- DYQVDISPPLTLLR-HJQYTNQXSA-N Carthamin Natural products CC[C@H]1O[C@H]([C@H](O)[C@@H](O)[C@@H]1O)[C@]2(O)C(=C(C=C/3C(=O)C(=C(O)[C@](O)([C@@H]4O[C@H](CO)[C@@H](O)[C@H](O)[C@H]4O)C3=O)C(=O)C=Cc5ccc(O)cc5)C(=O)C(=C2O)C(=O)C=Cc6ccc(O)cc6)O DYQVDISPPLTLLR-HJQYTNQXSA-N 0.000 description 1
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- 240000007218 Ipomoea hederacea Species 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 239000005434 MCC/mannitol excipient Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 244000172533 Viola sororia Species 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- UESYMIFUVPHBHL-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O.CC(O)=O.CC(O)=O UESYMIFUVPHBHL-UHFFFAOYSA-N 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 238000009629 microbiological culture Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000027939 micturition Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- -1 polysiloxane Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 235000010352 sodium erythorbate Nutrition 0.000 description 1
- 239000004320 sodium erythorbate Substances 0.000 description 1
- RBWSWDPRDBEWCR-RKJRWTFHSA-N sodium;(2r)-2-[(2r)-3,4-dihydroxy-5-oxo-2h-furan-2-yl]-2-hydroxyethanolate Chemical compound [Na+].[O-]C[C@@H](O)[C@H]1OC(=O)C(O)=C1O RBWSWDPRDBEWCR-RKJRWTFHSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000019614 sour taste Nutrition 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
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
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
- A24B15/303—Plant extracts other than tobacco
-
- 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
-
- 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
- A24D3/04—Tobacco smoke filters characterised by their shape or structure
- A24D3/048—Tobacco smoke filters characterised by their shape or structure containing additives
-
- 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
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/14—Printing inks based on carbohydrates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/12—Coatings without pigments applied as a solution using water as the only solvent, e.g. in the presence of acid or alkaline compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
Abstract
The invention discloses a preparation method of natural perfume, which comprises the following steps: (1) preparing morning glory fermentation slurry; (2) preparing a crude extract; (3) Loading and adsorbing the crude extract by using macroporous adsorption resin, and then sequentially carrying out gradient elution by using ethanol solutions with different concentrations; collecting and combining 10-20wt% ethanol and 40-50wt% ethanol section ethanol solution eluent; (4) Concentrating the eluent under reduced pressure to obtain the color-changeable morning glory spice which is the natural spice. The invention also discloses the natural spice and application thereof in cigarette materials.
Description
Technical Field
The invention belongs to the technical field of essence and spice for cigarettes, and particularly relates to natural spice, a preparation method thereof and application thereof in tobacco.
Background
The cigarette is a kind of hobby that the smoker can smoke the cigarette to meet the physiological and psychological demands. The pH value of the cigarette smoke can reflect the smoke strength, the smoke irritation and the nicotine inhalation quantity felt by a smoker. A great deal of researches show that the pH value of the smoke of the traditional cigarette is mainly concentrated between 5.4 and 6.2.
The tar reduction of cigarettes is an important subject in cigarette production, and the smoke taste is light and the aroma is weakened along with the reduction of tar amount, so that the smoke concentration is increased and the cigarette aroma is improved by means of a feeding and flavoring technology. The natural perfume is one of the main sources of the essence perfume for cigarettes, and has the effects of increasing the smoke concentration, modifying the smoke fragrance and improving the smoke quality.
The natural perfume is mainly derived from plants, and has the characteristics of safety, no toxicity and special aromatic smell. Some pigments in the natural perfume are colored, so that the multi-color functions of bright color and the like of the cigarette material can be realized. The applicant found that some natural flavours containing pigments may change colour with changes in pH. The color natural perfume with the change of the pH value is developed and used in cigarette materials such as cigarette paper, tipping paper, tows and the like, so that the recognition degree of a cigarette product can be increased, a consumer can taste the smoke and the fragrance when smoking the cigarette, the visual enjoyment of the cigarette with the interesting change of the appearance of the cigarette along with the smoke can be obtained, and the attractive force to the consumer is improved.
The invention is proposed for this purpose.
Disclosure of Invention
The invention aims to solve the problems of insufficient functional variety of the existing essence and spice for cigarettes, and provides a natural spice which is applied to cigarette materials such as cigarette paper, tipping paper, tows, filter tip particles and the like, and can ensure that a consumer can feel color change of visual appearance of the cigarettes when smoking the cigarettes and improve interestingness and cigarette identification at the same time.
The percentages used in the present invention are mass percentages unless otherwise indicated.
The technical scheme of the invention is as follows:
the first aspect of the invention discloses a method for preparing natural perfume, comprising the following steps:
(1) Crushing and sterilizing fresh blue-purple morning glory to obtain morning glory slurry, fermenting for a period of time by using rhizosphere pseudomonas C1-9 microbial inoculum, and sterilizing to obtain morning glory fermentation slurry;
(2) Carrying out ultrasonic extraction on the morning glory fermentation slurry obtained in the step (1) by using 10-20 times of water, separating an extracting solution, and concentrating the obtained filtrate under reduced pressure until the volume is not changed any more to obtain a crude extracting solution;
(3) Loading and adsorbing the crude extract obtained in the step (2) by using macroporous adsorption resin, and then sequentially carrying out gradient elution by using 10-20wt% ethanol, 40-50wt% ethanol, 70-80wt% ethanol and 95wt% ethanol solution which are 3-5 times of column volume; collecting and combining 10-20wt% ethanol and 40-50wt% ethanol section ethanol solution eluent;
(4) Concentrating the eluent under reduced pressure to obtain the color-changeable morning glory spice which is the natural spice.
Preferably, the preparation method of the rhizosphere pseudomonas solanacearum C1-9 bacterial agent in the step (1) comprises the following steps: every 1000mL of the fermentation culture solution of the rhizosphere pseudoriver bacillus C1-9 subjected to the expanded fermentation culture is centrifuged at 3500rpm/min for 10min, the precipitate is washed by sterile water, and finally 20mL of sterile water is uniformly oscillated, and the rhizosphere pseudoriver bacillus C1-9 microbial inoculum is obtained after 10 times dilution during use. The rhizosphere pseudobacillus C1-9 is separated from tobacco rhizosphere soil of the tobacco of the Yunnan will be named as rhizosphere pseudobacillus (riverside) C1-9 by microbiological classification, which is preserved in China general microbiological culture collection center (CGMCC) at 8 months 9 of 2019, with the preservation number of CGMCC 1.13864 and address: the institute of microorganisms of national academy of sciences of China, national center for sciences of No. 1, north Chen West road, chat, of Beijing, city.
Preferably, the fermentation step of the rhizosphere pseudomonas solanacearum C1-9 microbial inoculum in the step (1) comprises the following steps: 10-20 mL of rhizosphere pseudomonas pseudolaris C1-9 microbial inoculum is inoculated to every 100g of morning glory pulp, and after fermentation is carried out for 24-72 hours, the morning glory fermentation pulp is obtained after sterilization for 30 minutes in a sterilizing pot at 121 ℃.
The second aspect of the invention discloses the natural perfume prepared by the preparation method.
Preferably, the natural perfume is blue-violet clear liquid with a solid content of 60wt% to 80wt%.
In a third aspect the invention discloses the use of said natural flavour in a smoking material; the cigarette material comprises cigarette paper, tipping paper, filter tip particles and tows.
Preferably, the application method steps are as follows:
(1) In cigarette paper: diluting the color-changeable morning glory spice with distilled water for 2-5 times; mixing fungus polysaccharide 5-15 weight portions, propylene glycol 55-65 weight portions and ethanol 25-35 weight portions through shaking for 1-5 hr to obtain coating liquid matrix; uniformly mixing the diluted color-changeable morning glory spice with a coating liquid matrix according to the mass ratio of 1:1 to obtain color-changeable morning glory spice coating liquid; the color-changeable morning glory spice coating liquid is coated on the cigarette paper in a spraying, roll shaft embossing or fixed-point spraying mode, so that the color cigarette paper containing the color-changeable morning glory spice is obtained;
(2) In tipping paper: diluting the color-changeable morning glory spice with distilled water for 2-5 times; mixing 5-15 parts of fungal polysaccharide, 55-65 parts of propylene glycol and 25-35 parts of ethanol for 1-5 hours, and adding an ink auxiliary agent accounting for 0.1-1 wt% of the mass of the mixed solution to obtain an ink matrix; uniformly mixing the diluted color-changeable morning glory spice with an ink matrix according to the mass ratio of 1:1 to obtain color ink of the color-changeable morning glory spice; printing on the tipping paper in a printing mode of gravure printing, flexography, roller shaft embossing or ink-jet printing to obtain color tipping paper containing the color-changeable morning glory spice; the ink auxiliary agent comprises one or more of a leveling agent, a defoaming agent and a slipping agent;
(3) In the cigarette filter particles: freeze-drying the color-changeable morning glory spice to obtain color-changeable morning glory spice freeze-dried powder; uniformly mixing the obtained spice freeze-dried powder and a granule excipient according to the mass ratio of 1:1-1:10, and then placing the mixture into a fluidized bed for spray granulation, wherein an adhesive solution with the concentration of 4-10wt% is sprayed in the granulation process, so as to obtain the color-changeable morning glory spice granules; adding the obtained color-changeable morning glory spice particles into a transparent cavity of a multi-element composite filter rod or into a filter rod tow gap; the granule excipient comprises one or more of sugar powder, dextrin, lactose, soluble starch, microcrystalline cellulose and mannitol;
(4) In cigarette tows: freeze-drying the color-changeable morning glory spice to obtain color-changeable morning glory spice freeze-dried powder; uniformly mixing the spice freeze-dried powder with the fiber master batch according to the mass ratio of 0.1-3 wt% of the fiber master batch of the tows, and forming color tows containing the color-changeable morning glory spice through a tow production process and a filter tip forming process; or diluting the freeze-dried powder of the color-changeable morning glory spice with ethanol, adding the diluted powder into the plasticizer glyceryl triacetate according to the proportion of 1-5wt%, and spraying the diluted powder into tows through a filter tip forming device to form color filter tips containing the color-changeable morning glory spice; the fiber master batch is one of acetic acid diacetic acid tablets and polylactic acid.
Conventional natural pigments or other color-changing flavors may also be added to formulate more color-based flavor colors when using color-changing morning glory flavors.
For better stability of the color-changeable morning glory spice, 0.02 to 1wt% of a stabilizer may be added thereto to enhance the color stability of the color-changeable morning glory spice, the stabilizer including one or more of ascorbic acid, sodium erythorbate, rutin, malonic acid, and the like.
The invention has the following beneficial effects:
1. semen Pharbitidis (academic name: pharbitis nil (L.) Choisy) is a genus Pharbitidis of the family Convolvulaceae; distributed in tropical and subtropical regions, flowers are ornamental, and seeds are common traditional Chinese medicines, and have the effects of draining water, promoting urination, expelling phlegm and killing insects. The prior production technology of the essence and spice for cigarettes has not been reported in the development and application of pH color-changing and aroma-giving dual-function morning glory spice.
2. The invention utilizes the strain rhizosphere pseudoHeterobacillus C1-9 to ferment and flavor the morning glory, and then ultrasonic extraction and macroporous resin sectional refining treatment are carried out, so that the prepared color-changeable morning glory spice not only has special fresh scent, but also enriches the smell scent of the cigarettes and increases the unique fragrance and floral scent characteristics of the smoke, and the color changes along with the smoking of the smoke, and the color is bright and pure; without fermentation, or fermentation using other species, has no or poor effect. Researches show that the morning glory red pigment contained in the natural perfume provided by the invention is blue-purple when the pH value of the natural perfume is 7-8, and turns into purple when the pH value of the natural perfume is 5-6; therefore, when the natural perfume is applied to cigarette materials, the natural perfume is normally blue-purple, and when the natural perfume is manufactured into cigarettes and smoked, the natural perfume can be purple-red due to the influence of the pH of smoke due to the penetration of the smoke, so that the color-changing effect is realized. The natural spice of the invention can give special appearance to cigarettes, improve visual interest, and simultaneously can make the cigarettes mellow and improve the smoking quality of the cigarettes.
3. The preparation method of the natural spice fully utilizes easily available plant resources, prepares the morning glory into the color-changeable spice for cigarettes for the first time, enriches the sources and the types of the spice for cigarettes, has low cost, has no harmful solvent introduction in the preparation process, is green and safe, and is easy to realize industrialization.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Example 1: a preparation method of a color-changeable morning glory spice comprises the following steps:
(1) Preparation of a rhizosphere pseudomonas C1-9 microbial inoculum:
1) Preparation of expanded culture of Pseudomonas rhizoaciens C1-9: sterilizing the R2A liquid culture medium at 121 ℃ for 25 minutes, picking part of mycelia from the preservation culture medium of the rhizosphere pseudomonas aeruginosa C1-9, inoculating the mycelia into the R2A liquid culture medium, and shake culturing at 30 ℃ for 48 hours to obtain liquid strains;
2) Preparing a rhizosphere pseudomonas C1-9 microbial agent: transferring the liquid strain of the rhizosphere pseudoriver bacillus C1-9 into a fermentation culture medium according to 10% of inoculation amount, culturing for 6 days at 28 ℃ in a shaking bottle, centrifuging every 1000mL of the obtained culture solution for 10min at 3500r/min, washing precipitate with sterile water, vibrating the precipitate uniformly with 20mL of sterile water, and diluting the precipitate by 10 times to obtain the rhizosphere pseudoriver bacillus C1-9 microbial inoculum;
(2) And (3) fermenting plants: grinding and crushing fresh morning glory to obtain morning glory slurry, sterilizing in a sterilizing pot at 121 ℃ for 30min, inoculating 20mL of rhizosphere pseudomonas C1-9 microbial inoculum into each 100g of the morning glory slurry, fermenting in a constant temperature and humidity box at 22 ℃ and 60% for 48h, and sterilizing in a sterilizing pot at 121 ℃ for 30min to obtain morning glory fermentation slurry;
(3) Ultrasonic extraction: adding 12 times of water into the morning glory fermentation slurry for ultrasonic extraction for 60min; filtering the extractive solution, concentrating the filtrate at 50deg.C under reduced pressure until the volume is unchanged, to obtain crude extract of morning glory;
(4) Refining macroporous resin: loading the D101 macroporous adsorption resin with the mass of 6 times of the crude morning glory extract into a column, washing the column with distilled water, and loading and adsorbing the crude morning glory extract; then sequentially carrying out gradient elution by using 15wt% ethanol, 40wt% ethanol, 70wt% ethanol and 95wt% ethanol solution with the volume of 3 times of the column volume; collecting and combining 15wt% and 40wt% ethanol solution eluents, concentrating under reduced pressure at 50 ℃ to obtain blue-violet clear liquid with 80wt% of solid content, and adding ascorbic acid with 0.05% of liquid mass to mix uniformly to obtain the color-changeable morning glory spice with obvious faint scent.
Comparative example 1: the same as in example 1, but without the fermentation flavouring step.
The fresh morning glory is subjected to ultrasonic extraction and macroporous resin refining according to the steps (3) and (4) in the embodiment 1 to obtain the morning glory extract.
Comparative example 2: plant fermentation of fresh morning glory was performed as in example 1, but with Bacillus subtilis (strain number: CGMCC 4091) instead of Pseudomonas rhizoaci C1-9; then, the fresh morning glory is subjected to ultrasonic extraction and macroporous resin refining according to the steps (3) and (4) in the embodiment 1 to obtain the morning glory extract.
Comparative example 3: plant fermentation of fresh morning glory with Pediococcus acidilactici (strain number: CICC 10344) in place of Pseudomonas rhizoaci C1-9 was performed as in example 1; then, the fresh morning glory is subjected to ultrasonic extraction and macroporous resin refining according to the steps (3) and (4) in the embodiment 1 to obtain the morning glory extract.
Example 2: the use of the color-changeable morning glory spice and the morning glory extract obtained in the example 1, the comparative example 2 and the comparative example 3 in cigarette paper comprises the following steps:
(1) Preparation of color-changeable morning glory spice coating liquid
The color-changeable morning glory flavor and the morning glory extract prepared in example 1, comparative example 2, and comparative example 3 were diluted 3-fold with distilled water, respectively; respectively taking 10 parts of fungal polysaccharide, 60 parts of propylene glycol and 30 parts of ethanol, respectively oscillating for 2 hours, and uniformly mixing to obtain four coating liquid matrixes; uniformly mixing the diluted color-changeable morning glory spice and the morning glory extract with a coating liquid matrix according to the mass ratio of 1:1 to obtain four color-changeable morning glory spice coating liquids;
(2) Preparation and application of color cigarette paper containing color-changeable morning glory spice
In the cigarette paper printing process, pattern design is carried out, a template is engraved, roller shaft embossing is adopted, the four color-changeable morning glory spice coating liquids are respectively printed on cigarette paper to obtain four color cigarette papers containing the color-changeable morning glory spice, and then the four cigarette papers are further rolled into cigarettes to be used as test samples, and the test cigarettes, the control cigarette 1#, the control cigarette 2#, and the control cigarette 3#, respectively are marked; and comparing the cigarette paper which is not coated with any color-changeable morning glory spice coating liquid with blank cigarettes;
(3) The evaluation results are shown in Table 1.
In terms of appearance, compared with a blank cigarette, the cigarette paper of the test cigarette and the control cigarette has blue-violet pattern.
In the aspect of smell, the control cigarette 1# prepared without any fermentation has no obvious smell when being smelled; the control cigarette 2# prepared by fermenting bacillus subtilis has obvious pungent odor when being smelled; the control cigarette 3# prepared by the fermentation of Pediococcus acidilactici has obvious sour taste when being smelled; the color-changeable morning glory spice prepared by utilizing the rhizosphere pseudomonas aeruginosa C1-9 has obvious faint scent, so that the test cigarette smell containing the color-changeable morning glory spice also has elegant fragrance.
In the aspect of cigarette smoking evaluation, when the cigarettes are ignited for smoking, compared with a blank cigarette, when the cigarettes are compared with the cigarettes 1# in smoking, the smoke flavor is not obviously increased, the miscellaneous gas is increased to some extent, and the smoke coordination is poor. When the control cigarette 2# prepared by fermenting bacillus subtilis is smoked, the smoke quantity is increased, but the miscellaneous gas and the irritation are obviously increased, and the smoke coordination is poor. When the control cigarette 3# prepared by the Pediococcus acidilactici fermentation is smoked, the smoke quantity is increased, the sour feel in the smoke is obviously increased, the miscellaneous gas and the stimulation are obvious, and the smoke coordination is poor. When the test cigarette prepared by fermenting the rhizosphere pseudomonas aeruginosa C1-9 is smoked, the faint scent and the flower fragrance in the smoke are obvious, the smoke fragrance is more mellow, the aftertaste is cleaner, and the smoking quality of the cigarette is obviously improved.
In terms of color change, the color of control cigarette # 1, which was not prepared without any fermentation, was not a pure bluish violet color, and the color changed but was not apparent and did not change to a reddish purple color during smoking. The starting colors of the control cigarettes 2# and 3# are blue-violet, and the color is dim; as the aspiration process proceeds, the color gradually changes to mauve, but the color change is not bright enough and the visual effect is not prominent enough. The initial color of the test cigarette is blue-violet, and the color is bright and pure; along with the suction process, the color gradually changes into bright and pure mauve; the color change is clear and the visual effect is prominent.
Table 1 functional evaluation of color cigarette paper coating liquids
Example 3: the use of the variable color morning glory fragrances, morning glory extracts obtained in example 1, comparative example 2, and comparative example 3 in tipping paper, comprises the following steps:
(1) Preparation of color-changeable morning glory spice ink
Taking the color-changeable morning glory spice prepared in the example 1, the comparative example 2 and the comparative example 3, respectively diluting the color-changeable morning glory spice and the morning glory extract by 2 times with distilled water, and adding carthamin to perform color blending to obtain a gray-green color-changeable morning glory spice solution; taking 15 parts of fungal polysaccharide, 55 parts of propylene glycol and 30 parts of ethanol, oscillating for 3 hours, mixing uniformly, and respectively adding 0.2wt% of leveling agent polysiloxane and 0.1wt% of slipping agent fatty acid amide into the mixed solution for mixing uniformly to obtain four parts of ink matrixes; and then uniformly mixing the color-changeable morning glory spice solution and the ink matrix according to the mass ratio of 1:1 to obtain the four color-changeable morning glory spice inks.
(2) Preparation and application of color tipping paper containing color-changeable morning glory spice
In the tipping paper printing process, the four kinds of color-changeable morning glory spice ink are printed on the tipping paper by adopting ink-jet printing, so that the color tipping paper containing the color-changeable morning glory spice is obtained, and then the tipping paper is further rolled into cigarettes.
(3) Evaluation results
The results are substantially the same as in example 2 in terms of olfactory note. In terms of color change, the pattern on the tipping paper is in a greenish gray color, the cigarette is lit for smoking, and after the smoke passes through the filter tip, the pattern on the tipping paper gradually changes to a brick red color. Only the pattern on the tipping paper of the test cigarette is bright and pure grey green, and the color gradually changes into bright and pure brick red along with the suction process; the color change is bright and the visual effect is prominent. The patterns on the tipping paper obtained in comparative example 1, comparative example 2 and comparative example 3 are not bright and pure enough in starting color, and gradually change into brick red along with the suction process; but the color is not bright and pure enough, and the visual effect is not outstanding enough.
Example 4: the application of the color-changeable morning glory spice in the cigarette filter tip particles specifically comprises the following steps:
the color-changeable morning glory spice and the morning glory extract prepared in the example 1, the comparative example 2 and the comparative example 3 are respectively subjected to freeze drying under the conditions that the freezing temperature is minus 60 ℃, the hydrazine cooling temperature is minus 20 ℃, the vacuum degree is 10Pa and the freeze drying final temperature is 25 ℃ to respectively obtain four color-changeable morning glory spice freeze-dried powders; according to a spray granulation process, uniformly mixing four kinds of color-changeable morning glory spice freeze-dried powder and dextrin according to a mass ratio of 1:3, placing the mixture in a fluidized bed, and spraying an adhesive solution with the mass of 8wt% of the color-changeable morning glory spice freeze-dried powder in the granulation process to obtain four kinds of color-changeable morning glory spice particles.
In the process of forming the composite cigarette filter tip, the four kinds of color-changeable morning glory spice particles are applied to a filter tip tow according to the amount of 2mg per millimeter of filter tip, or are added to the transparent cavity part of the composite filter tip in a concentrated manner, so that four kinds of cigarette filter tips containing the color-changeable morning glory spice particles are obtained, and then the four kinds of cigarette filter tips are further rolled into cigarettes; suction is then applied.
The smell results were substantially the same as in example 2. The color change was from blue-violet to purple and the four cigarettes were substantially the same as in example 2.
Example 5: the application of the color-changeable morning glory spice in the cigarette tows specifically comprises the following steps:
the color-changeable morning glory spice and the morning glory extract prepared in example 1, comparative example 2 and comparative example 3 were freeze-dried at a freezing temperature of-50 ℃, a hydrazine cooling temperature of-10 ℃, a vacuum degree of 20Pa and a freeze-drying final temperature of 28 ℃ respectively to obtain four color-changeable morning glory spice freeze-dried powders.
(1) After the acetate fiber master batch acetate diacetic tablet is prepared into slurry, 0.5 weight percent of the four color-changeable morning glory spice freeze-dried powders are respectively added and uniformly mixed, four blue-violet tows containing the color-changeable morning glory spice are formed through a tow production process, a filter tip rod containing the color-changeable morning glory spice is formed through a filter tip rod forming device, and then four cigarettes are further rolled. When the cigarette is lit for smoking, the smoke passes through the filter rod and the color of the filter rod tows changes. The smell results were substantially the same as in example 2. The color change was from blue-violet to purple and the four cigarettes were substantially the same as in example 2.
(2) The four kinds of color-changeable morning glory spice freeze-dried powder are respectively added with a small amount of ethanol for dilution and dissolution, and then are respectively added into plasticizer triacetin according to the proportion of 1wt%, so as to obtain four kinds of blue-violet triacetin containing the color-changeable morning glory spice, and the four kinds of color-changeable morning glory spice freeze-dried powder are sprayed into common tows through a filter tip forming device to form four kinds of filter tips containing the color-changeable morning glory spice, and are further rolled into cigarettes. When the cigarette is lit for smoking, the smoke passes through the filter rod and the color of the filter rod tows changes.
The smell results were substantially the same as in example 2. The color change was from blue-violet to purple and the four cigarettes were substantially the same as in example 2.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (4)
1. Use of a natural perfume in a cigarette material; the natural perfume is blue-violet clear liquid, and the solid content of the natural perfume is 60-80 wt%; the cigarette material comprises cigarette paper, tipping paper, filter tip particles and tows; the preparation method of the natural perfume is characterized by comprising the following steps:
(1) Crushing and sterilizing fresh blue-purple morning glory to obtain morning glory slurry, fermenting for a period of time by using rhizosphere pseudomonas C1-9 microbial inoculum, and sterilizing to obtain morning glory fermentation slurry;
(2) Carrying out ultrasonic extraction on the morning glory fermentation slurry obtained in the step (1) by using 10-20 times of water, separating an extracting solution, and concentrating the obtained filtrate under reduced pressure until the volume is not changed any more to obtain a crude extracting solution;
(3) Loading and adsorbing the crude extract obtained in the step (2) by using macroporous adsorption resin, and then sequentially carrying out gradient elution by using 10-20wt% ethanol, 40-50wt% ethanol, 70-80wt% ethanol and 95wt% ethanol solution which are 3-5 times of column volume; collecting and combining 10-20wt% ethanol and 40-50wt% ethanol section ethanol solution eluent;
(4) Concentrating the eluent under reduced pressure to obtain the color-changeable morning glory spice which is the natural spice.
2. The use according to claim 1, wherein the preparation method of the bacterial agent of the rhizosphere pseudomonas solanacearum C1-9 in the step (1) comprises the following steps: every 1000mL of the fermentation culture solution of the rhizosphere pseudoriver bacillus C1-9 subjected to the expanded fermentation culture is centrifuged at 3500rpm for 10min, the precipitate is washed by sterile water, and finally the precipitate is uniformly vibrated by 20mL sterile water, and the rhizosphere pseudoriver bacillus C1-9 microbial inoculum is obtained after 10 times dilution during use.
3. The use according to claim 1, wherein the fermentation step of the bacterial agent C1-9 of pseudomonas rhizoinstance in step (1) is: and inoculating 10-20 mL of a rhizosphere pseudomonas pseudolaris C1-9 microbial inoculum to every 100g of the morning glory pulp, fermenting for 24-72 h, and sterilizing in a sterilizing pot at 121 ℃ for 30min to obtain the morning glory fermentation pulp.
4. Use according to claim 1, characterized in that the application method steps are as follows:
(1) In cigarette paper: diluting the color-changeable morning glory spice by 2-5 times with distilled water; mixing 5-15 parts of fungal polysaccharide, 55-65 parts of propylene glycol and 25-35 parts of ethanol uniformly by shaking for 1-5 hours to obtain a coating liquid matrix; uniformly mixing the diluted color-changeable morning glory spice with a coating liquid matrix according to the mass ratio of 1:1 to obtain color-changeable morning glory spice coating liquid; the color-changeable morning glory spice coating liquid is coated on the cigarette paper in a spraying, roll shaft embossing or fixed-point spraying mode, so that the color cigarette paper containing the color-changeable morning glory spice is obtained;
(2) In tipping paper: diluting the color-changeable morning glory spice by 2-5 times with distilled water; mixing 5-15 parts of fungal polysaccharide, 55-65 parts of propylene glycol and 25-35 parts of ethanol for 1-5 hours, and adding an ink auxiliary agent accounting for 0.1-1wt% of the mass of the mixed solution to obtain an ink matrix; uniformly mixing the diluted color-changeable morning glory spice with an ink matrix according to the mass ratio of 1:1 to obtain color ink of the color-changeable morning glory spice; printing on the tipping paper in a printing mode of gravure printing, flexography, roller shaft embossing or ink-jet printing to obtain color tipping paper containing the color-changeable morning glory spice;
(3) In the cigarette filter particles: freeze-drying the color-changeable morning glory spice to obtain color-changeable morning glory spice freeze-dried powder; uniformly mixing the obtained spice freeze-dried powder and a granule excipient according to the mass ratio of 1:1-1:10, and then placing the mixture in a fluidized bed for spray granulation, wherein an adhesive solution with the concentration of 4-10wt% is sprayed in the granulation process, so that the color-changeable morning glory spice granules are obtained; adding the obtained color-changeable morning glory spice particles into a transparent cavity of a multi-element composite filter rod or into a filter rod tow gap;
(4) In cigarette tows: freeze-drying the color-changeable morning glory spice to obtain color-changeable morning glory spice freeze-dried powder; uniformly mixing the spice freeze-dried powder with the fiber master batch according to the mass ratio of 0.1-3 wt% of the fiber master batch of the tows, and forming color tows containing the color-changeable morning glory spice through a tow production process and a filter tip forming process; or diluting the freeze-dried powder of the color-changeable morning glory spice with ethanol, adding the diluted powder into the plasticizer glyceryl triacetate according to the proportion of 1-5 wt%, and spraying the diluted powder into tows through a filter tip forming device to form the color filter tip containing the color-changeable morning glory spice.
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