CN110982620A - Porous starch-loaded molecular capsule, and preparation method and application thereof - Google Patents
Porous starch-loaded molecular capsule, and preparation method and application thereof Download PDFInfo
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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
- C11B9/0069—Heterocyclic compounds
- C11B9/0092—Heterocyclic compounds containing only N as heteroatom
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- 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
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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
- C11B9/0069—Heterocyclic compounds
- C11B9/0073—Heterocyclic compounds containing only O or S as heteroatoms
- C11B9/0084—Heterocyclic compounds containing only O or S as heteroatoms the hetero rings containing more than six atoms
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/20—Preparation of compounds containing saccharide radicals produced by the action of an exo-1,4 alpha-glucosidase, e.g. dextrose
Abstract
The invention discloses a porous starch-loaded molecular capsule, which is a capsule formed by coating a perfume with cyclodextrin, and is adsorbed on porous starch. The invention also discloses a preparation method of the porous starch-loaded molecular capsule and application of the porous starch-loaded molecular capsule in stability during storage and quick release of fragrance at high temperature.
Description
Technical Field
The invention relates to the technical field of tobacco, in particular to a porous starch-loaded molecular capsule, a preparation method and application thereof.
Background
Many flavor additives are often applied to cigarette flavoring because of rich and strong tar baking aroma, thereby effectively compensating the aroma loss caused by tar reduction of cigarettes. Researches show that the pyrazine substances have extremely high odor intensity and extremely low threshold value, so that the cigarette product has unique style and sufficient fragrance, and meanwhile, part of miscellaneous gases are masked, and the aftertaste is improved.
At present, the main cigarette flavoring agent is a spice monomer or a microcapsule. The published patent CN101129220A provides a tobacco flavor compensating agent applied to cigarette filter sticks, but because the flavor formula does not have a slow release effect, the flavor supplementing effect is not ideal due to the loss of flavor substances in the storage process. At present, the perfuming of the capsule method mainly utilizes an inert polymeric natural or synthetic polymer material to wrap the perfume in a closed capsule and then implant the filter tip. Patent US3550598 discloses a microcapsule perfuming technology, in which certain volatile perfume materials such as menthol, lime, etc. are reacted with gelatin, sodium alginate, gum arabic and cellulose derivatives to form microcapsules, which are placed in a filter, and the change of humidity and pH during smoking causes the rupture of the wall membrane to release the perfume materials. However, capsule filters suffer from a number of problems: the development cost is high, the preparation process is complex, and the capsule wall material can generate miscellaneous gas during burning and sucking; moreover, the perfume microcapsule is greatly influenced by the external environment, and the perfume can escape after long-term storage.
The cyclodextrin inclusion technology is characterized in that a 'molecular capsule' is formed by intermolecular hydrogen bonds and perfume monomers, slow release of perfume is realized (Rongying, Zhangliang, Sun Haifeet et al, preparation of menthol and β -cyclodextrin inclusion compound and thermal decomposition dynamics research [ J ] Chinese food additive, 2019(7) ]. compared with the common microcapsule technology, the cyclodextrin inclusion technology overcomes the problem of capsule wall materials, and has the advantages of mild process conditions and high embedding rate, but like the common microcapsule, the cyclodextrin 'molecular capsule' is easy to rupture to cause burst release of fragrance under the influence of the temperature, pH and humidity of the external environment, and the perfume can escape after long-term storage.
In order to overcome the problem of premature volatilization of traditional flavoring agents for cigarettes before smoking, in recent years, researches on encapsulation and sustained release of tobacco flavors by utilizing high adsorbability of porous materials are more and more, and patent US4729391 adds microporous polymer particles (such as polypropylene or polyethylene particles and the like) impregnated with flavors into a filter, and causes the release of the flavors through aerosol generated in a smoking process, but the used porous materials are not friendly to the environment.
Porous starch prepared by enzymatic hydrolysis of starch is a natural degradable material that well avoids this problem. The porous starch has the advantages of porous surface, hollow interior, excellent adsorption performance, better mechanical strength and better adsorption and protection of target substances. However, in the application process, the adsorption and slow release effects of the porous starch on the cigarette flavor with low flavor threshold are not ideal, for example, the flavor threshold concentration of pyrazine is only 1198 mug/kg, and the porous starch has high volatility. Because the high-volatility perfume is easy to escape from the cavities of the adsorbate, the simple physical method is not suitable for the slow release of the high-volatility cigarette perfume such as pyrazine and the like.
The prior art proposes the study of embedding high-volatility guest molecules by a double loading method (B.McCormack, G.Gregoriadis. drugs-in-cyclodextrins-in-lipomes: a novel conjugate in drug delivery. int.J.Pharm,1994,112:249-258), which is a cyclodextrin-clathrate-liposome system. Patent CN107960634A discloses a method for temperature-controlled release of perfume by porous starch adsorbed liposome. However, the particle size and entrapment rate of the synthetic liposome are influenced by various factors, and the stability is poor.
The invention can effectively solve the problems of short storage time of the high-volatility spice and burst release in cigarette application by combining cyclodextrin inclusion and porous starch adsorption technologies.
Disclosure of Invention
The invention provides a new technical scheme aiming at the problems of short spice storage time and burst release in cigarette application in the prior art.
The invention provides a porous starch-loaded molecular capsule, which is a capsule formed by coating a perfume with cyclodextrin, and is adsorbed on porous starch.
Preferably, the molecular capsules have an annual flavour release at 50 ℃ of not more than 40%.
Preferably, the spice is one or more of pyrazine, 2-methylpyrazine and 2, 3-dimethylpyrazine, and is pyrazine, the cyclodextrin is preferably one or more of α -cyclodextrin, β -cyclodextrin and gamma-cyclodextrin, and is β cyclodextrin.
The second aspect of the invention discloses a preparation method of the porous starch-loaded molecular capsule, which comprises the following steps:
(1) preparation of cyclodextrin perfume molecule capsules: adding perfume into cyclodextrin saturated water solution, mixing, reacting, cooling the reaction solution, crystallizing, filtering, washing, and vacuum drying to obtain white powder, i.e. cyclodextrin perfume molecular capsule;
(2) preparing porous starch: regulating pH of the starch emulsion to 5.5-6.5 with buffer solution, heating to 50-60 deg.C, adding mixed enzyme solution for reaction, centrifuging, filtering, washing, and vacuum drying to obtain white powder as porous starch;
(3) and (2) dissolving the cyclodextrin perfume molecular capsules obtained in the step (1) in water, adjusting the pH to 1.0-3.0, adding the porous starch obtained in the step (2), mixing, filtering and drying to obtain white solids, namely the porous starch-loaded molecular capsules.
Preferably, in the step (1), the spice is one or more of pyrazine, 2-methylpyrazine and 2, 3-dimethylpyrazine, more preferably pyrazine, the cyclodextrin is one or more of α -cyclodextrin, β -cyclodextrin and gamma-cyclodextrin, more preferably β -cyclodextrin, the molar ratio of the spice to the cyclodextrin is 1: 1-1: 3, the reaction temperature is 30-50 ℃, and the spice is washed by ethanol.
Preferably, the buffer solution of step (2) is disodium hydrogen phosphate-citric acid buffer solution, the mixed enzyme is α -mixture of amylase and saccharifying enzyme, the added amount of the mixed enzyme is 0.1-0.5 wt% of starch, and the washing is washed with distilled water.
Preferably, the reaction time of step (3) is 30-90min, more preferably 60 min; the reaction temperature is 20-40 ℃, and the preferable temperature is 30 ℃; the dosage of the porous starch is 10-30mg/L, and preferably 10 mg/L; the mass fraction of the cyclodextrin perfume molecule capsules is 5.0-7.0mg/g, more preferably 5.0 mg/g.
In a third aspect of the invention, the use of said porous starch-loaded molecular capsules for the storage-stable and rapid release of flavour at elevated temperatures in cigarette paper is disclosed.
Preferably, the porous starch-loaded molecular capsules are directly added during the production of the cigarette paper, or the solution is coated on the inner side of the cigarette paper after the porous starch-loaded molecular capsules are dissolved by a solvent.
Preferably, the solvent is one of ethanol, ethyl acetate and propylene glycol.
The invention has the beneficial effects that:
1. after the porous starch is subjected to enzymolysis by mixed enzyme, hydrophilic hydroxyl groups are distributed on the surface of the porous starch. Compared with directly adsorbing lipophilic perfume, the water-soluble cyclodextrin-perfume molecular capsule has higher adsorption rate and stronger adsorption effect. After the high-volatility perfume is sequentially subjected to cyclodextrin inclusion and porous starch adsorption, the escape process must overcome double resistance: the suction force on the surface of the porous starch and the intermolecular hydrogen bond action of the cyclodextrin overcome the defects of the existing high-volatility spice storage and slow release technology, and the temperature-controlled spice which is stable in storage period, can be quickly released at high temperature and can be added to the cigarette paper and the preparation method thereof are provided.
2. The temperature-controlled release spice prepared by the invention has the characteristics of stability in storage period and slow release at high temperature. The fragrance of the invention has the annual fragrance release amount not higher than 40% (namely the residual fragrance release amount is more than 60%) of the initial amount at normal temperature; whereas the prior art fragrances have an annual fragrance release at ambient temperature of more than 80% (i.e. less than 20% remaining) of the initial amount.
3. The invention skillfully solves the problems that the traditional microcapsule method for preparing the flavor additive is greatly influenced by the environment and burst release in specific application by combining cyclodextrin inclusion and porous starch adsorption technologies.
4. The spice of the invention is added into the cigarette paper as a flavor compensation agent, so that the loss of tar-reducing flavor can be effectively compensated, the flavor of the product is sufficient and moderate, and meanwhile, part of miscellaneous gas is covered, and the aftertaste is improved.
5. The invention has the advantages of easily obtained raw materials, environment-friendly added auxiliary materials, simple preparation process, high safety, low cost and easy realization of large-scale production.
Drawings
FIG. 1 is a graph of perfume release during shelf life (at ambient temperature) for porous starch loaded molecular capsules of the present invention and a control.
FIG. 2 is a graph of the thermal weight loss of porous starch loaded molecular capsules of the present invention versus a control.
Detailed Description
The following examples further illustrate the method of making a porous starch-loaded cyclodextrin-flavor molecule capsule disclosed in the present process by reference to the examples, which are provided for illustration only and are not intended to limit the invention.
Example 1
Weighing α -cyclodextrin 11.36g in a 500ml round bottom flask, adding 200ml of distilled water, heating to 40 ℃, magnetically stirring to obtain a cyclodextrin saturated solution, weighing pyrazine 0.4g in the solution, carrying out closed reflux reaction for 5h, standing the reaction solution in a refrigerator at 4 ℃ overnight to separate out crystals, carrying out suction filtration, and carrying out vacuum drying to obtain a solid, namely the cyclodextrin-coated pyrazine molecular capsule.
Weighing 10g of corn starch, adding a disodium hydrogen phosphate-citric acid buffer solution to adjust the pH value to 6.0, preparing 30% starch slurry, preheating for 15min at 55 ℃, adding about 1.2 wt% of α -amylase, saccharifying enzyme (1: 2) and mixed enzyme solution, reacting for 12h, adding 5ml of 4% sodium hydroxide solution to terminate the reaction, and then centrifuging, filtering, washing, drying in vacuum and crushing to obtain the corn porous starch.
Weighing 5g of molecular capsule of cyclodextrin coated pyrazine, dissolving in 100ml of water, adjusting pH to 2.0 with 0.1mol/l HCl, adding 10g of corn porous starch, stirring at constant temperature of 20 ℃ for 1h to fully mix with the porous starch, filtering and drying to obtain the molecular capsule loaded with the porous starch.
Example 2
Weighing β -cyclodextrin 5.68g into a 500ml round bottom flask, adding 200ml distilled water, heating to 40 ℃, magnetically stirring to obtain a cyclodextrin saturated solution, weighing pyrazine 0.4g into the solution, carrying out closed reflux reaction for 5h, standing the reaction solution in a refrigerator at 4 ℃ overnight to separate out crystals, carrying out suction filtration, and carrying out vacuum drying to obtain a solid, namely the cyclodextrin-coated pyrazine molecular capsule.
Weighing 10g of corn starch, adding a disodium hydrogen phosphate-citric acid buffer solution to adjust the pH value to 6.0, preparing 30% starch slurry, preheating for 15min at 55 ℃, adding about 1.2 wt% of α -amylase, saccharifying enzyme (1: 2) and mixed enzyme solution, reacting for 12h, adding 5ml of 4% sodium hydroxide solution to terminate the reaction, and then centrifuging, filtering, washing, drying in vacuum and crushing to obtain the corn porous starch.
Weighing 5g of molecular capsule of cyclodextrin coated pyrazine, dissolving in 100ml of water, adjusting pH to 2.0 with 0.1mol/l HCl, adding 10g of corn porous starch, stirring at constant temperature of 30 ℃ for 1h to fully mix with the porous starch, filtering and drying to obtain the molecular capsule loaded with the porous starch.
Example 3
Weighing β -cyclodextrin 5.68g into a 500ml round bottom flask, adding 200ml distilled water, heating to 40 ℃, magnetically stirring to obtain a cyclodextrin saturated solution, weighing pyrazine 0.4g into the solution, carrying out closed reflux reaction for 5h, standing the reaction solution in a refrigerator at 4 ℃ overnight to separate out crystals, carrying out suction filtration, and carrying out vacuum drying to obtain a solid, namely the cyclodextrin-coated pyrazine molecular capsule.
Weighing 10g of corn starch, adding a disodium hydrogen phosphate-citric acid buffer solution to adjust the pH value to 6.0, preparing 30% starch slurry, preheating for 15min at 55 ℃, adding about 1.2 wt% of α -amylase, saccharifying enzyme (1: 2) and mixed enzyme solution, reacting for 12h, adding 5ml of 4% sodium hydroxide solution to terminate the reaction, and then centrifuging, filtering, washing, drying in vacuum and crushing to obtain the corn porous starch.
Weighing 5g of molecular capsule of cyclodextrin coated pyrazine, dissolving in 100ml of water, adjusting pH to 2.0 with 0.1mol/l HCl, adding 10g of corn porous starch, stirring at constant temperature of 20 ℃ for 1h to fully mix with the porous starch, filtering and drying to obtain the molecular capsule loaded with the porous starch.
Example 4
Weighing β -cyclodextrin 5.68g into a 500ml round bottom flask, adding 200ml distilled water, heating to 40 ℃, magnetically stirring to obtain a cyclodextrin saturated solution, weighing pyrazine 0.4g into the solution, carrying out closed reflux reaction for 5h, placing the reaction solution in a refrigerator at 4 ℃ overnight to precipitate crystals, carrying out suction filtration and vacuum drying, and obtaining a solid, namely the cyclodextrin-coated pyrazine molecular capsule.
Weighing 10g of corn starch, adding a disodium hydrogen phosphate-citric acid buffer solution to adjust the pH value to 6.0, preparing 30% starch slurry, preheating for 15min at 55 ℃, adding about 1.2 wt% of α -amylase, saccharifying enzyme (1: 2) and mixed enzyme solution, reacting for 12h, adding 5ml of 4% sodium hydroxide solution to terminate the reaction, and then centrifuging, filtering, washing, drying in vacuum and crushing to obtain the corn porous starch.
Weighing 6g of molecular capsule of cyclodextrin coated pyrazine, dissolving in 100ml of water, adjusting pH to 2.0 with 0.1mol/l HCl, adding 20g of corn porous starch, stirring at constant temperature of 40 ℃ for 1h to fully mix with the porous starch, filtering and drying to obtain the molecular capsule loaded with the porous starch.
Example 5: slow release performance investigation of cigarette sample storage period
The sample prepared in example 2 was coated on the inner side of cigarette paper to prepare a cigarette, a cigarette smoking test was performed on an RM200 smoking machine according to standard smoking conditions, and the pyrazine content in the smoke of the cigarette was measured by gas chromatography, comparing the cigarette sample with the monthly pyrazine smoking release amount during the 12-month storage period. The result shows that after the cigarette sample added with the porous starch loaded molecular capsule is stored for 12 months, the residual pyrazine content is more than 80% of the initial amount, and the pyrazine in the cigarette sample added with only pyrazine is extracted to only leave 19% of the initial content. The technology of the invention obviously improves the stability of the pyrazine, prolongs the aroma-keeping period and improves the product quality. See the control curve of figure 1.
Example 6: thermogravimetric (TG) technology for investigating thermal decomposition performance of perfume sample
The method has the advantages that the temperature rise process of the sample in the cigarette smoking process is simulated, and the mass change of the sample is measured by means of the thermobalance, so that the thermal stability and the degradation process of the sample are accurately analyzed.
The test procedure was as follows: 10mg of the perfume sample prepared in example 2 (to the nearest 0.1mg) are weighed into a model 209F1 thermal analysis system under the following test conditions: n is a radical of2The flow rate is 30mL/min, and the heating rate is 10 ℃/min.
The characteristics of the TG curves are compared as follows:
(1) the pyrazine monomer is continuously weightless in the range from the initial temperature to 150 ℃, the maximum endothermic peak is 125 ℃, and the weightless curve tends to be stable after 150 ℃, which indicates that pyrazine is completely volatilized;
(2) the sample of the invention has slow weight loss between room temperature and 325 ℃, the weight loss is only 3 percent, and when the temperature is continuously increased, obvious weight loss occurs, and the weight loss exceeds 70 percent.
The thermogravimetric analysis results show that: pyrazine monomers are rapidly volatilized at a lower temperature; the spice sample (the porous starch loaded molecular capsule cigarette sample) prepared by the invention hardly releases under the storage condition of less than 300 ℃ and obviously releases under the high-temperature condition of more than 300 ℃, thus being an ideal cigarette flavoring agent. See the control curve of figure 2.
Example 7: simulating the release of spice in the cigarette smoking process by a thermal cracking gas chromatography (PY-GC) technology
The thermal cracking experiment procedure was as follows: weighing 0.1g of the spice sample prepared in example 2 (accurate to 0.1mg), preparing a suspension with the concentration of about 10mg/mL by using absolute ethyl alcohol, filling 1mg-2mg of quartz wool in the central position of a cracking tube, placing 2 mu L of sample solution on the quartz wool, then placing the cracking tube into a cracking instrument for cracking, and separating and identifying volatile substances released after cracking in a GC (gas chromatography) by using carrier gas.
(1) Thermal cracking conditions are as follows: pyrolysis atmosphere: 276mL/min of nitrogen-oxygen mixed gas; temperature programming: 30 ℃ (5s) → 900 ℃ (5 s); the initial temperature of a cracking instrument interface is 50 ℃, and the working temperature is 250 ℃; the temperature of the valve box is 280 ℃; the transfer line temperature was 280 ℃.
(2) Chromatographic conditions are as follows: HP-5MS capillary column [30m X250 μm (inside diameter) X0.25 μm (liquid film thickness)](ii) a Carrier gas: he (purity 99.999%); the flow rate was 1.5mL/min (column head pressure of gas chromatography: 1.80X 104 Pa); temperature programming:
the split ratio is as follows: 100:1.
The relative release amounts of pyrazine at different temperatures (50 ℃, 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃) were calculated by dividing the corrected peak areas obtained at different temperatures and the peak areas obtained at 50 ℃, and the ratio of the relative release amounts of pyrazine with temperature increase is shown in table 1 below.
TABLE 1 relative release of pyrazine with increasing temperature for the inventive and comparative samples
As can be seen from the data in the table: the high-volatility pyrazine perfume monomer is released at 50-150 ℃ in an accelerated mode, and is basically and completely released at 150 ℃. The release amount of the spice sample prepared by the invention is less than 10% of the original content before 250 ℃, and the spice sample can be rapidly released at a high temperature of 250-300 ℃, and the release amount reaches 50% of the original content.
Example 8: investigation of cigarette perfuming Effect
0.01g of each sample prepared in the above examples 1, 2, 3 and 4 is taken and dissolved in 5mL of absolute ethyl alcohol, a plurality of portions of cigarette paper are taken, a sample ethanol solution is sprayed on each portion of cigarette paper by a micro-spraying device and is uniformly coated (the addition amount is 30mg/cig), and a control sample is directly sprayed with the same amount of ethanol. The cigarette paper samples (the side which has been coated with flavour is the inside) are then rolled into cigarettes, each containing 0.8g of tobacco. Before the test, the cigarette paper samples with or without fragrance are placed in a constant temperature and humidity box to be balanced for 48 hours (the temperature is 22 +/-2 ℃, and the relative humidity is 60 +/-5 percent) for professional staff to smoke. The sensory quality of the samples was evaluated according to the national standard GB/T5606.4-2005 cigarette sensory technical requirement, and the evaluation results are shown in Table 2.
TABLE 2 sensory quality of the inventive and control cigarette samples
As can be seen from Table 2, indexes such as aroma quality, irritation, offensive odor, comfort, uniform release and the like show that the prepared spice (porous starch loaded molecular capsule) can stably release harmonious aroma and harmonize cigarette flavor without irritation when being used in cigarettes and smoked by professionals; is superior to the control.
Claims (10)
1. A porous starch-loaded molecular capsule, wherein the molecular capsule is a cyclodextrin-coated flavor capsule, and wherein the molecular capsule is adsorbed onto porous starch.
2. The porous starch-loaded molecular capsules according to claim 1, wherein the molecular capsules have an annual flavour release at 50 ℃ of not more than 40% of the initial amount.
3. The porous starch-loaded molecular capsule of claim 1, wherein the flavorant is one or more of pyrazine, 2-methylpyrazine, 2, 3-dimethylpyrazine and the cyclodextrin is one or more of α -cyclodextrin, β -cyclodextrin, γ -cyclodextrin.
4. A method of preparing a porous starch-loaded molecular capsule according to claims 1-3, comprising the steps of:
(1) preparation of cyclodextrin perfume molecule capsules: adding perfume into cyclodextrin saturated water solution, mixing, reacting, cooling the reaction solution, crystallizing, filtering, washing, and vacuum drying to obtain white powder, i.e. cyclodextrin perfume molecular capsule;
(2) preparing porous starch: regulating pH of the starch emulsion to 5.5-6.5 with buffer solution, heating to 50-60 deg.C, adding mixed enzyme solution for reaction, centrifuging, filtering, washing, and vacuum drying to obtain white powder as porous starch;
(3) and (2) dissolving the cyclodextrin perfume molecular capsules obtained in the step (1) in water, adjusting the pH to 1.0-3.0, adding the porous starch obtained in the step (2), mixing, filtering and drying to obtain white solids, namely the porous starch-loaded molecular capsules.
5. The process according to claim 4, wherein the flavor in the step (1) is one or more selected from pyrazine, 2-methylpyrazine and 2, 3-dimethylpyrazine, the cyclodextrin is one or more selected from α -cyclodextrin, β -cyclodextrin and γ -cyclodextrin, the molar ratio of flavor to cyclodextrin is 1: 1 to 1: 3, the reaction temperature is 30 to 50 ℃, and the reaction mixture is washed with ethanol.
6. The process according to claim 4, wherein the buffer in the step (2) is disodium hydrogen phosphate-citric acid buffer, the enzyme mixture is α -amylase and saccharifying enzyme mixture, the amount of the enzyme mixture added is 0.1-0.5 wt% of starch, and the mixture is washed with distilled water.
7. The preparation method according to claim 4, wherein the reaction time of the step (3) is 30-90min, the reaction temperature is 20-40 ℃, the dosage of the porous starch is 10-30mg/L, and the mass fraction of the cyclodextrin flavor molecule capsule is 5.0-7.0 mg/g.
8. Use of porous starch-loaded molecular capsules according to claims 1-3 for rapid flavour release in cigarette paper stable during storage and at elevated temperatures.
9. Use according to claim 8, the porous starch-loaded molecular capsules being added directly at the time of production of the cigarette paper; or dissolving the porous starch-loaded molecular capsule with a solvent, and then coating the solution on the inner side of the cigarette paper.
10. The use according to claim 9, wherein the solvent is one of ethanol, ethyl acetate and propylene glycol.
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