CN115449432B - Color-changeable spice, preparation method and application thereof - Google Patents
Color-changeable spice, preparation method and application thereof Download PDFInfo
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- CN115449432B CN115449432B CN202211155570.9A CN202211155570A CN115449432B CN 115449432 B CN115449432 B CN 115449432B CN 202211155570 A CN202211155570 A CN 202211155570A CN 115449432 B CN115449432 B CN 115449432B
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- 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
- C11B9/02—Recovery or refining of essential oils from raw materials
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention discloses a preparation method of a color-changeable spice, which comprises the following steps: (1) preparing bougainvillea spectabilis 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 bougainvillea spectabilis spice, namely the color-changeable spice. The invention also discloses the color-changeable 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 a color-changeable spice, a preparation method and application thereof.
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
Aiming at the problems of insufficient functional variety and the like of the existing essence and spice for cigarettes, the invention provides a color-changeable 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.
The percentages used in the present invention are mass percentages unless otherwise indicated.
The first aspect of the invention discloses a method for preparing a color-changeable spice, which comprises the following steps:
(1) Crushing and sterilizing fresh purple-red bougainvillea to obtain bougainvillea Mei Jiangye, fermenting for a period of time by using a azospirillum W712 microbial inoculum, and sterilizing to obtain bougainvillea fermentation slurry;
(2) Heating and extracting the bougainvillea spectabilis fermented slurry obtained in the step (1) with 10-20 times of 95% ethanol at 50-65 ℃, 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 20-30wt% ethanol, 50-60deg.C ethanol, 80-90wt% ethanol and 95wt% ethanol solution with the volume of 3-5 times of column volume; collecting and combining 20-30wt% ethanol and 50-60deg.C ethanol section ethanol solution eluent;
(4) Concentrating the eluent under reduced pressure to obtain the color-changeable bougainvillea spectabilis spice, namely the color-changeable spice.
Preferably, the preparation method of the azospirillum W712 microbial inoculum in the step (1) comprises the following steps: every 1000mL of fermentation culture solution of the azoospermia W712 after the expansion fermentation culture is centrifuged for 10min at 3000rpm/min, the sediment is washed by sterile water, and the sediment is evenly oscillated by 20mL of sterile water, and is diluted by 10 times when in use, thus obtaining the azoospermia W712 bacterial agent. The azoospira W712 is isolated from tobacco rhizosphere soil samples of a base of Yunnan Kunming tobacco, and is named as azoospira sp.W712 in microbiological classification, and is preserved in China general microbiological culture Collection center (CGMCC) for 10 months and 13 days in 2021, with the preservation number of CGMCC 1.18567 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 azospirillum W712 microbial inoculum of the step (1) comprises the following steps: inoculating 10-20 mL of azospirillum W712 microbial inoculum to each 100g of triangle Mei Jiangye, fermenting for 24-72 h, and sterilizing in a sterilizing pot at 121 ℃ for 30min to obtain the bougainvillea spectabilis fermentation slurry.
The invention also discloses a color-changeable spice prepared by the preparation method.
Preferably, the color-changing perfume is a pink clear liquid with a solids content of 60wt% to 80wt%.
In a third aspect the invention discloses the use of the variable colour 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 triangle Mei Xiangliao by 2-5 times with distilled water; 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; mixing the diluted color-changeable bougainvillea spectabilis spice with a coating liquid matrix according to a ratio of 1: mixing uniformly in a mass ratio to obtain a color-changeable bougainvillea spectabilis spice coating liquid; the color-changeable bougainvillea spectabilis spice coating liquid is coated on the cigarette paper in a spraying, roller shaft embossing or fixed-point spraying mode to obtain color cigarette paper containing the color-changeable bougainvillea spectabilis spice;
(2) In tipping paper: diluting the color-changeable triangle Mei Xiangliao 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 0.1-1 wt% of the mass of the mixed solution to obtain an ink matrix; mixing the diluted color-changeable bougainvillea spectabilis spice with an ink matrix according to a proportion of 1: mixing uniformly in a mass ratio to obtain color ink with color changeable bougainvillea spectabilis 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 color-changeable bougainvillea spectabilis 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 bougainvillea spectabilis flavor to obtain color-changeable bougainvillea spectabilis Mei Xiangliao freeze-dried powder; mixing the obtained spice freeze-dried powder with a granule excipient according to a mass ratio of 1:1 to 1:10, after uniformly mixing, placing the mixture in a fluidized bed for spray granulation, and spraying an adhesive solution with the concentration of 4-10wt% in the granulation process to obtain color-changeable bougainvillea spectabilis spice particles; adding the obtained color-changeable bougainvillea spectabilis spice particles into a transparent cavity of a multi-element composite filter rod or a filter rod silk bundle 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 bougainvillea spectabilis flavor to obtain color-changeable bougainvillea spectabilis Mei Xiangliao 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 bouquet spice through a tow production process and a filter tip forming process; or diluting the color-changeable triangle Mei Xiangliao freeze-dried powder 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 color-changeable triangle plum flavors; the fiber master batch is one of acetic acid diacetic acid tablets and polylactic acid.
When the color-changeable bougainvillea spectabilis flavor is applied, conventional natural pigments or other color-changeable flavors can be added to prepare the color of the flavor with more color systems.
For better stability of the color-changeable bougainvillea spectabilis flavor, 0.02 to 1wt% of stabilizer can be added to enhance the color stability of the color-changeable bougainvillea spectabilis flavor, wherein the stabilizer comprises one or more of ascorbic acid, sodium erythorbate, rutin and malonic acid.
The invention has the following beneficial effects:
1. bougainvillea spep, the name of Bougainvillea spep, such as Rhododendron simsii, flos Aleuritopteris Crispi, rhododendron trifoliatum, and radix Puerariae, is a wood vine-like shrub of the genus She Zihua of Mirabiliaceae, and has effects of relieving dysentery, detumescence, and harmonizing qi and blood. The existing tobacco essence and spice production technology has not been reported in the development and application of pH color-changing and aroma-adding dual-function bougainvillea spectabilis spice.
2. According to the invention, after the azoospermi W712 is utilized to ferment and flavor the bougainvillea, the heating extraction and macroporous resin sectional refining treatment are carried out, so that the prepared color-changeable bougainvillea has special fresh and sweet fragrance, after being applied to cigarettes, the aroma of the cigarettes is enriched, the unique fragrance and sweet fragrance characteristics of the smoke are increased, and the color is changed along with the suction 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 color-changeable spice contains rich plant pigment, the plant pigment is pink at the pH of 7-8, when the pH is 1-6, the color is gradually deepened to dark purple along with the increase of acidity, and when the pH is 9-14, the color is gradually changed into yellow from pink along with the increase of alkalinity; therefore, when the color-changeable spice is applied to cigarette materials, the color-changeable spice is normally pink, and when the color-changeable spice is made into cigarettes and smoked, the color-changeable spice can be purple due to the influence of the pH of smoke due to the penetration of the smoke, so that the color-changeable effect is realized. The color-changeable spice of the invention can give special appearance to cigarettes, improve visual interest, increase richness of cigarette fragrance, reduce miscellaneous gases and clean aftertaste.
3. The preparation method of the color-changeable spice fully utilizes easily available plant resources, prepares the bougainvillea spectabilis 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, 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 color-changeable bougainvillea spectabilis spice comprises the following steps:
(1) Preparation of azoospermia W712 bacterial agent:
1) Expansion culture of azoospiram W712 strain: sterilizing the R2A liquid culture medium at 121 ℃ for 25 minutes, picking part of mycelium from the nitrogen fixing helicobacter W712 preservation culture medium, and inoculating the mycelium into the R2A liquid culture medium, and performing shake culture at 28 ℃ for 36 hours to obtain liquid strains;
2) Preparing a azoospiram W712 bacterial agent: transferring the liquid strain of the azoospermia W712 into a fermentation medium according to 10% of inoculation amount, shaking and culturing for 7 days at 28 ℃, centrifuging the obtained culture solution at 3000r/min for 10min per 1000mL, washing the precipitate with sterile water, shaking the precipitate uniformly with 20mL of sterile water, and diluting 10 times to obtain the azoospermia W712 microbial agent.
(2) And (3) fermenting plants: grinding and crushing fresh purple red bougainvillea spectabilis to obtain bougainvillea spectabilis Mei Jiangye, sterilizing in a sterilizing pot at 121 ℃ for 30min, inoculating 15mL of azospirillum W712 microbial inoculum to each 100g of bougainvillea spectabilis Mei Jiangye, and fermenting in a constant temperature and humidity box at 22 ℃ and 60% for 48h to obtain bougainvillea spectabilis fermentation slurry.
(3) Heating and extracting: adding 12 times of 95% ethanol into bougainvillea spectabilis fermentation slurry, and heating and extracting at 60 ℃ for 4h; filtering the hot extract, concentrating the obtained filtrate under reduced pressure until the volume is unchanged, and obtaining triangle Mei Cu extract.
(4) Refining macroporous resin: loading the D101 macroporous adsorption resin column with the mass of the extracting solution of the triangle Mei Cu which is 6 times that of the triangle Mei Cu, and washing the column with distilled water, and then loading and adsorbing the extracting solution of the triangle Mei Cu; then sequentially carrying out gradient elution by using 20wt% ethanol, 50wt% ethanol, 80wt% ethanol and 95wt% ethanol solution with the volume of 3 times of the column volume; collecting and combining 20wt% and 50wt% ethanol solution eluents, concentrating under reduced pressure at 50deg.C to obtain pink clear liquid with solid content of 80deg.C, and adding malonic acid with liquid mass of 0.02% to mix uniformly to obtain color-changeable triangle Mei Xiangliao, wherein the perfume has obvious faint scent.
Comparative example 1: the same as in example 1, but without the fermentation flavouring step.
Heating and extracting fresh bougainvillea spectabilis in the steps (3) and (4) in the embodiment 1, and refining by macroporous resin to obtain the bougainvillea spectabilis extract.
Comparative example 2: plant fermentation was performed on fresh bougainvillea spectabilis with Bacillus simplex (strain number: CICC 10477) instead of Azospirillum azotemlobum W712 as in example 1; then, according to the step (3) and the step (4) in the embodiment 1, the fresh bougainvillea spectabilis is heated and extracted, and the bougainvillea spectabilis extract is obtained by refining with macroporous resin.
Comparative example 3: plant fermentation of fresh bougainvillea spectabilis was performed as in example 1, except that lactococcus (strain number: CICC 20415) was used instead of azospirillum W712; then, according to the step (3) and the step (4) in the embodiment 1, the fresh bougainvillea spectabilis is heated and extracted, and the bougainvillea spectabilis extract is obtained by refining with macroporous resin.
Example 2: the application of the color-changeable bougainvillea spectabilis flavor and bougainvillea spectabilis 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 bougainvillea spectabilis spice coating liquid
The color-changeable bougainvillea spectabilis flavor and bougainvillea spectabilis extract prepared in example 1, comparative example 2 and comparative example 3 were diluted 2-fold with distilled water, respectively; respectively taking 10 parts of fungal polysaccharide, 55 parts of propylene glycol and 35 parts of ethanol, oscillating for 3 hours, and uniformly mixing to obtain a coating liquid matrix; then mixing the diluted color-changeable bougainvillea spectabilis spice, bougainvillea spectabilis extract and a coating liquid matrix according to a ratio of 1: mixing uniformly in a mass ratio to obtain four color-changeable bougainvillea spectabilis spice coating liquids.
(2) Preparation and application of color cigarette paper containing color-changeable bougainvillea spectabilis spice
In the cigarette paper printing process, pattern design is carried out, fixed-point spray printing is adopted, the four color-changeable bougainvillea spectabilis spice coating liquids are respectively printed on cigarette paper to obtain four color cigarette papers containing the color-changeable bougainvillea spectabilis 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 No. 1, the control cigarette No. 2 and the control cigarette No. 3 are respectively marked; and comparing the cigarette paper which is not coated with any color-changeable bougainvillea spectabilis spice coating liquid with blank cigarettes;
(3) The evaluation results are shown in Table 1.
In terms of appearance, the cigarette papers of the test cigarettes and the control cigarettes all present pink pattern patterns compared with the blank cigarettes.
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 the bacillus simplex has obvious sour and stink smell during sniffing; the control cigarette 3# prepared by lactococcus fermentation has faint scent with grease miscellaneous gas during sniffing; and the color-changeable triangle Mei Xiangliao prepared by utilizing the azoospermia W712 smells special sweet fragrance, and has fresh and natural fragrance.
In the aspect of cigarette smoking, when the cigarettes are ignited for smoking, compared with a blank cigarette, when the cigarette 1# is smoked, the smoke aroma is not obviously increased, but the irritation is increased, and the smoking quality of the cigarettes is improved poorly. When the control cigarette 2# prepared by fermenting the bacillus simplex is smoked, the sour and fragrant of the smoke is increased, but the smoke enters the dry throat to be pricked, and the irritation is increased. When the control cigarette 3# prepared by lactococcus fermentation is smoked, the smoke fragrance is increased, but the smoke has lipid miscellaneous gas, and the smoke coordination is poor. When the test cigarette prepared by fermenting the azotobacter strain W712 is smoked, the sweet fragrance in the smoke is obviously increased, the richness of the smoke fragrance is increased, the aftertaste is clean, the miscellaneous gas is reduced, and the overall quality of the sensory evaluation of the cigarette is obviously improved.
In terms of color change, the comparative cigarette # 1, which was not prepared by any fermentation, was lighter in pink, less in staining, and the pattern color was darkened but not apparent during smoking, and did not turn to a pure mauve. The starting colors of the control cigarettes 2# and 3# are dark pink, the patterns are dense, and the color effect is poor; as the aspiration process proceeds, the color gradually turns to dark red, the hue is dull, and the visual effect is not prominent. The color-changeable triangle Mei Xiangliao applied to the test cigarettes has strong coloring power, clear pattern and lines, pink initial color and vivid and natural color tone; the color gradually changes to bright mauve along with the suction process; the color change difference is obvious, and the visual effect is outstanding.
Table 1 functional evaluation of color cigarette paper coating liquids
Example 3: the application of the color-changeable bougainvillea spectabilis flavor and bougainvillea spectabilis extract obtained in the example 1, the comparative example 2 and the comparative example 3 to tipping paper comprises the following steps:
(1) Preparation of color-changeable bougainvillea spectabilis spice ink
Taking the color-changeable bougainvillea spectabilis spice and the bougainvillea spectabilis extract prepared in the example 1, the comparative example 2 and the comparative example 3, respectively diluting by 2 times with distilled water, and adding gardenia blue pigment for color blending to obtain a color-changeable bougainvillea spectabilis spice solution with a magenta color; mixing 15 parts of fungal polysaccharide, 55 parts of propylene glycol and 30 parts of ethanol for 4 hours, adding defoaming agent silicone emulsion accounting for 0.2wt% of the mass of the mixed solution, and mixing uniformly to obtain four parts of ink matrix; and then respectively mixing the magenta color-changeable bougainvillea spectabilis spice solution and the ink matrix according to the proportion of 1: mixing uniformly in a mass ratio of 1 to obtain the four color-changeable bougainvillea spectabilis spice ink.
(2) Preparation and application of color tipping paper containing color-changeable bougainvillea spectabilis spice
In the tipping paper printing process, the four color-changeable bougainvillea spectabilis spice ink is printed on the tipping paper by adopting intaglio printing, so that the color tipping paper containing the color-changeable bougainvillea spectabilis spice is obtained, and then the tipping paper is further rolled into cigarettes.
(3) Evaluation of 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 begins to appear magenta, the cigarette is lit for smoking, and the pattern on the tipping paper gradually changes to indigo as the smoke passes through the filter tip. Only the pattern on the tipping paper of the test cigarette has a bright and pure magenta color, and the color gradually changes into bright and pure indigo blue along with the suction process; the color change is bright and the visual effect is prominent. The pattern on the tipping paper obtained in comparative example 1 has an insignificant initial color, poor tinting strength, gradually changed into pale indigo with the progress of the suction process, and poor pattern rendering effect; the patterns on the tipping papers obtained in comparative examples 2 and 3 were not bright and pure enough in starting color, and the colors were gradually changed to dark indigo colors along with the progress of the suction process, and were not bright and pure enough in color, and the visual effect was not outstanding enough.
Example 4: the application of the color-changeable bougainvillea spectabilis spice in cigarette filter tip particles comprises the following steps:
the color-changeable bougainvillea spectabilis spice and the bougainvillea spectabilis 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-70 ℃, the hydrazine cooling temperature is-20 ℃, the vacuum degree is 20Pa and the freeze drying final temperature is 22 ℃ to respectively obtain four color-changeable bougainvillea spectabilis Mei Xiangliao freeze-dried powders; according to a spray granulation process, four color-changeable triangular Mei Xiangliao freeze-dried powders and lactose are mixed according to a mass ratio of 1:2, after being evenly mixed, the mixture is placed in a fluidized bed, and adhesive solution with the mass of 5 weight percent of the freeze-dried powder of the variable color triangle Mei Xiangliao is sprayed in the granulating process, so that four variable color triangle plum spice particles are obtained.
In the process of forming the composite cigarette filter stick, the four color-changeable bouquet spice particles are applied to the filter stick filament bundle according to the amount of 2mg per millimeter of filter stick, or are added to the transparent cavity part of the composite filter stick in a concentrated manner, so that four cigarette filter sticks containing the color-changeable bouquet spice particles are obtained, and then the four cigarette filter sticks are further rolled into cigarettes and are smoked.
The smell results were substantially the same as in example 2. The color change was from pink to purple and the four cigarettes were substantially the same as in example 2.
Example 5
The application of the color-changeable bougainvillea spectabilis spice in cigarette tows specifically comprises the following steps:
the color-changeable bougainvillea spectabilis spice and bougainvillea spectabilis extract prepared in example 1, comparative example 2 and comparative example 3 were freeze-dried at a freezing temperature of-60 ℃, a hydrazine cooling temperature of-10 ℃, a vacuum degree of 20Pa and a freeze-drying final temperature of 22 ℃ to obtain four color-changeable bougainvillea spectabilis Mei Xiangliao freeze-dried powders.
(1) After the acetate fiber master batch acetate diacetic acid tablet is made into slurry, 1.5 weight percent of the four color-changeable triangle Mei Xiangliao freeze-dried powders are respectively added and uniformly mixed, four pink tows containing color-changeable triangle plum flavor are formed through a tow production process, a filter tip containing color-changeable triangle plum flavor is formed through a filter tip 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 pink to purple and the four cigarettes were substantially the same as in example 2.
(2) The four color-changeable triangle Mei Xiangliao freeze-dried powders are respectively added with a small amount of ethanol for dilution and dissolution, and then are respectively added into the plasticizer triacetin according to the proportion of 2wt%, so as to obtain four pink triacetin containing color-changeable triangle plum flavor, the four pink triacetin containing color-changeable triangle plum flavor is sprayed into common tows through a filter rod forming device, so that four filter rods containing color-changeable triangle plum flavor are formed, and then the filter rods are further rolled into cigarettes, and when the cigarettes are lighted for smoking, the smoke passes through the filter rods 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 pink 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 (7)
1. A method for preparing a color-changeable perfume, comprising the steps of:
(1) Crushing and sterilizing fresh purple-red bougainvillea to obtain bougainvillea Mei Jiangye, fermenting for a period of time by using a azospirillum W712 microbial inoculum, and sterilizing to obtain bougainvillea fermentation slurry;
(2) Heating and extracting the bougainvillea spectabilis fermented slurry obtained in the step (1) with 10-20 times of 95% ethanol at 50-65 ℃, 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 20-30wt% ethanol, 50-60deg.C ethanol, 80-90wt% ethanol and 95wt% ethanol solution with the volume of 3-5 times of column volume; collecting and combining 20-30wt% ethanol and 50-60deg.C ethanol section ethanol solution eluent;
(4) Concentrating the eluent under reduced pressure to obtain the color-changeable bougainvillea spectabilis spice, namely the color-changeable spice.
2. The preparation method of the nitrogen-fixing helicobacter W712 bacterial agent according to claim 1, wherein the preparation method of the nitrogen-fixing helicobacter W712 bacterial agent in step (1) comprises the following steps: every 1000mL of the fermentation culture solution of the azoospermia W712 after the expansion fermentation culture is centrifuged for 10min at 3000rpm, the sediment is washed by sterile water, and the sediment is evenly oscillated by 20mL of sterile water, and is diluted by 10 times when in use, thus obtaining the azoospermia W712 microbial agent.
3. The method according to claim 1, wherein the fermentation of the azospirillum W712 of step (1) comprises: inoculating 10-20 mL of azospirillum W712 microbial inoculum to each 100g of triangle Mei Jiangye, fermenting for 24-72 h, and sterilizing in a sterilizing pot at 121 ℃ for 30min to obtain the bougainvillea spectabilis fermentation slurry.
4. A color changeable perfume prepared by the preparation method according to any one of claims 1 to 3.
5. The color-changing perfume according to claim 4, wherein the color-changing perfume is a pink clear liquid having a solids content of 60wt% to 80wt%.
6. Use of a variable colour flavour according to claim 4 in a cigarette material; the cigarette material comprises cigarette paper, tipping paper, filter tip particles and tows.
7. Use according to claim 6, characterized in that the application method steps are as follows:
(1) In cigarette paper: diluting the color-changeable triangle Mei Xiangliao by 2-5 times with distilled water; 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; mixing the diluted color-changeable bougainvillea spectabilis spice with a coating liquid matrix according to a ratio of 1: mixing uniformly in a mass ratio to obtain a color-changeable bougainvillea spectabilis spice coating liquid; the color-changeable bougainvillea spectabilis spice coating liquid is coated on the cigarette paper in a spraying, roller shaft embossing or fixed-point spraying mode to obtain color cigarette paper containing the color-changeable bougainvillea spectabilis spice;
(2) In tipping paper: diluting the color-changeable triangle Mei Xiangliao 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 0.1-1 wt% of the mass of the mixed solution to obtain an ink matrix; mixing the diluted color-changeable bougainvillea spectabilis spice with an ink matrix according to a proportion of 1: mixing uniformly in a mass ratio to obtain color ink with color changeable bougainvillea spectabilis 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 color-changeable bougainvillea spectabilis spice;
(3) In the cigarette filter particles: freeze-drying the color-changeable bougainvillea spectabilis flavor to obtain color-changeable bougainvillea spectabilis Mei Xiangliao freeze-dried powder; mixing the obtained spice freeze-dried powder with a granule excipient according to a mass ratio of 1:1 to 1:10, after uniformly mixing, placing the mixture in a fluidized bed for spray granulation, and spraying an adhesive solution with the concentration of 4-10wt% in the granulation process to obtain color-changeable bougainvillea spectabilis spice particles; adding the obtained color-changeable bougainvillea spectabilis spice particles into a transparent cavity of a multi-element composite filter rod or a filter rod silk bundle gap;
(4) In cigarette tows: freeze-drying the color-changeable bougainvillea spectabilis flavor to obtain color-changeable bougainvillea spectabilis Mei Xiangliao 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 bouquet spice through a tow production process and a filter tip forming process; or diluting the color-changeable triangle Mei Xiangliao freeze-dried powder 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 the color filter tip containing the color-changeable triangle plum flavor.
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