CN114081204A - Cinnamyl alcohol microcapsule and preparation method thereof, tobacco granules and preparation method thereof, filter stick or filter tip, tobacco product and application - Google Patents
Cinnamyl alcohol microcapsule and preparation method thereof, tobacco granules and preparation method thereof, filter stick or filter tip, tobacco product and application Download PDFInfo
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- CN114081204A CN114081204A CN202111422168.8A CN202111422168A CN114081204A CN 114081204 A CN114081204 A CN 114081204A CN 202111422168 A CN202111422168 A CN 202111422168A CN 114081204 A CN114081204 A CN 114081204A
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- cinnamyl alcohol
- microcapsule
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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
- A24D3/04—Tobacco smoke filters characterised by their shape or structure
- A24D3/048—Tobacco smoke filters characterised by their shape or structure containing additives
Abstract
The invention belongs to the field of tobacco products, and particularly relates to a method for preparing cinnamyl alcohol microcapsules, which comprises the following steps: mixing a sodium alginate solution, tween 60 and cinnamyl alcohol to obtain a first mixture; slowly adding the gelatin solution into the first mixture, and mixing to obtain a second mixture; spray drying the second mixture to obtain cinnamyl alcohol microcapsules; wherein the mass ratio of the sodium alginate to the gelatin is 1 (1-2.2), the mass of the Tween 60 is 6-30% of the total mass of the sodium alginate and the gelatin, and the mass of the cinnamyl alcohol is 24-210% of the total mass of the sodium alginate and the gelatin. The invention also relates to cinnamyl alcohol microcapsules, granules for cigarettes, a preparation method of the granules, a filter stick or a filter tip, a tobacco product and application of the granules. The cinnamyl alcohol microcapsule has high cinnamyl alcohol content and high embedding rate, and when being added into cigarettes, the cinnamyl alcohol microcapsule can improve the uniformity of fragrance release, improve the fragrance slow-release effect and prolong the fragrance-remaining period of the cigarettes.
Description
Technical Field
The invention belongs to the field of tobacco products, and particularly relates to cinnamyl alcohol microcapsules and a preparation method thereof, a tobacco granule and a preparation method thereof, a filter stick or a filter tip, a tobacco product and application.
Background
Cinnamon is the dry bark of cinnamon (Cinnamomum cassia Presl) belonging to Lauraceae genus, and has effects of inducing sweat, expelling pathogenic cold, relieving pain, warming and dredging channels, supporting yang, regulating qi, and lowering qi. The cortex Cinnamomi has high volatile oil content, and has antiinflammatory, antibacterial, gastric ulcer resisting, antitumor, and cardiovascular system protecting effects, and has cinnamaldehyde, cinnamyl alcohol, cinnamic acid, coumarin, protocatechuic acid, etc. as main effective components. The cinnamyl alcohol has unique fragrance similar to hyacinth, has sweet taste and can be applied to the production of cosmetics, foods, medicaments and other fine chemical products, but has stronger volatility, easy oxidation, unstable light and heat, short fragrance retention period and certain limitation on storage and use.
The microcapsule technology is a technology in which a solid, liquid or gas core material is embedded by using a natural or synthetic polymer material as a wall material to form a microcapsule having a semipermeable membrane or a sealing membrane.
Therefore, there is a need for a technology for preparing cinnamyl alcohol microcapsules.
Disclosure of Invention
The invention provides a method for preparing cinnamyl alcohol microcapsules, wherein the cinnamyl alcohol content in the prepared cinnamyl alcohol microcapsules is improved, the embedding rate is improved, the cinnamyl alcohol microcapsules are added into cigarettes to improve the fragrance release uniformity of the cinnamyl alcohol during smoking of the cigarettes, the slow release effect of the fragrance is improved, and the fragrance retention period of the cigarettes added with the cinnamyl alcohol microcapsules is obviously prolonged. On the basis, the invention also provides a cinnamyl alcohol microcapsule, a granule for cigarettes, a preparation method of the granule, a filter stick or a filter tip, a tobacco product and application.
To achieve the above object, the present invention relates in a first aspect to a method for preparing cinnamyl alcohol microcapsules, comprising the steps of:
(1) mixing a sodium alginate solution, tween 60 and cinnamyl alcohol to obtain a first mixture;
(2) slowly adding a gelatin solution into the first mixture, and mixing to obtain a second mixture;
(3) spray drying the second mixture to obtain cinnamyl alcohol microcapsules;
wherein, the mass ratio of the sodium alginate to the gelatin is 1 (1-2.2) (preferably 1 (1.2-1.8), such as 1:1.2, 1:1.4, 1:1.6 and 1:1.8), the mass of the Tween 60 is 6-30% (preferably 6-28%, such as 10%, 14%, 20%, 22% and 24%) of the total mass of the sodium alginate and the gelatin, and the mass of the cinnamyl alcohol is 24-210% (preferably 26-210%, such as 26%, 30%, 32%, 60%, 70%, 74%, 86%, 90%, 100%, 130%, 170% and 180%) of the total mass of the sodium alginate and the gelatin.
In certain embodiments of the first aspect of the present invention, in step (1), tween 60 and cinnamyl alcohol are added to the sodium alginate solution sequentially and mixed.
In certain embodiments of the first aspect of the present invention, in step (2), the mixing is performed by homogenizing and then stirring.
In some embodiments of the first aspect of the present invention, in the step (2), the stirring treatment is performed for 0.5 to 3 hours, such as 1 hour, 1.5 hours, 2 hours, and 2.5 hours.
In some embodiments of the first aspect of the present invention, in step (1), the concentration of the sodium alginate solution is 3-20 g/L, preferably 3-17 g/L, such as 5g/L, 7g/L, 10g/L, 12g/L, 15g/L, 18 g/L.
In some embodiments of the first aspect of the present invention, in step (2), the concentration of the gelatin solution is 8-25 g/L, preferably 8-22 g/L, such as 10g/L, 15g/L, 18g/L, 20g/L, 22 g/L.
In some embodiments of the first aspect of the present invention, in the step (2), the homogenization treatment is performed for 2 to 10 minutes, such as 3, 4, 5, 7, and 8 minutes.
In certain embodiments of the first aspect of the present invention, in step (2), the homogenization treatment is performed using a homogenizer; preferably, the refiner has a rotational speed of 3000 to 4000rpm, such as 3300rpm, 3500rpm, 3800 rpm.
In certain embodiments of the first aspect of the present invention, in step (2), the agitation treatment is performed at normal temperature.
In some embodiments of the first aspect of the present invention, in the step (2), the rotation speed of the stirring treatment is 400 to 1600 rpm, for example 1000 rpm.
In certain embodiments of the first aspect of the present invention, in step (3), the temperature of the inlet air for spray drying is 115 ℃ to 135 ℃, e.g., 120 ℃, 125 ℃, 130 ℃.
In certain embodiments of the first aspect of the present invention, in step (3), the outlet temperature of the spray drying is from 80 ℃ to 100 ℃, e.g., 85 ℃, 90 ℃, 95 ℃.
In certain embodiments of the first aspect of the present invention, in step (3), the feed rate of the spray drying is 5 to 18mL/min, such as 7mL/min, 10mL/min, 13mL/min, 16 mL/min.
In certain embodiments of the first aspect of the present invention, the gelatin solution is formulated at a temperature of 50 ℃ to 70 ℃, e.g., 55 ℃, 60 ℃, 65 ℃.
In certain embodiments of the first aspect of the present invention, the gelatin solution is stored at room temperature.
In a first aspect of the invention, the sodium alginate solution is an aqueous sodium alginate solution.
In a first aspect of the invention, the gelatin solution is an aqueous gelatin solution.
In the first aspect of the present invention, the normal temperature is also called a general temperature or room temperature, and the range is 15 ℃ to 35 ℃.
In a second aspect, the present invention relates to a cinnamyl alcohol microcapsule prepared by the process of the first aspect of the invention.
In some embodiments of the second aspect of the present invention, the content of cinnamyl alcohol in the cinnamyl alcohol microcapsules is not less than 20% by mass, preferably 20% to 60%, such as 30%, 40%, 50%.
In some embodiments of the second aspect of the present invention, the encapsulation rate of the cinnamyl alcohol microcapsules is not less than 70%, preferably 70% to 90%, such as 80%, 85%.
The third aspect of the invention relates to a method for preparing granules for cigarettes, which comprises the following steps:
mixing the cinnamyl alcohol microcapsules with alcohol or a solution thereof, granulating, drying, and optionally screening to obtain granules for cigarettes; wherein the cinnamyl alcohol microcapsule is a cinnamyl alcohol microcapsule prepared by the method of the first aspect of the invention or the cinnamyl alcohol microcapsule of the second aspect of the invention.
In some embodiments of the third aspect of the present invention, the alcohol solution has a concentration of 50% to 90%, for example 60%, 70%, 80%, 85% by mass.
In some embodiments of the third aspect of the invention, the drying is carried out at 60 ℃ to 95 ℃, e.g., 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃.
In some embodiments of the third aspect of the present invention, the particles are sieved through a 14-25 mesh screen.
In some embodiments of the third aspect of the present invention, the ratio of the cinnamic alcohol microcapsules to the alcohol or solution thereof is such that the mixture is maintained in a moist state suitable for granulation.
The fourth aspect of the invention relates to a granule for tobacco, which is prepared by the method of the third aspect of the invention.
The fifth aspect of the invention relates to a filter stick or a filter tip, which comprises the cinnamyl alcohol microcapsule of the second aspect of the invention or the granule for cigarettes of the fourth aspect of the invention.
The sixth aspect of the present invention relates to a tobacco product comprising the cinnamyl alcohol microcapsule of the second aspect of the present invention, the granule for cigarettes of the fourth aspect of the present invention or the filter stick or the filter of the fifth aspect of the present invention; preferably, the tobacco product is a cigarette.
A seventh aspect of the invention relates to a use of a cinnamyl alcohol microcapsule according to the second aspect of the invention, a granule for cigarettes according to the fourth aspect of the invention or a filter stick or a filter tip according to the fifth aspect of the invention in a tobacco product; preferably, the tobacco product is a cigarette.
The invention has the following beneficial effects:
1. the cinnamyl alcohol content in the cinnamyl alcohol microcapsule is improved, and the embedding rate is improved;
2. the cinnamyl alcohol microcapsule provided by the invention is added into cigarettes, so that the uniformity of cinnamyl alcohol fragrance release during smoking of the cigarettes can be improved, the slow release effect of the fragrance is improved, and the fragrance retention period of the cigarettes is obviously prolonged.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which:
figure 1 is a graphical representation of the cinnamyl alcohol content of the puff-by-puff smoke of cigarettes 1-3 and control cigarettes.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Adding sodium alginate into 1L of pure water, stirring for dissolving, sequentially adding Tween 60 and cinnamyl alcohol, and fully stirring to form a uniform mixed solution, wherein the mass content of sodium alginate is 10g/L, the mass content of Tween 60 is 2g/L, and the mass content of cinnamyl alcohol is 20 g/L;
(2) adding gelatin into pure water, stirring and dissolving in water bath at 60 ℃, and cooling to room temperature to obtain 15g/L gelatin water solution;
(3) slowly adding gelatin aqueous solution into the mixed solution, homogenizing for 5min at 3500rpm by high-speed dispersion homogenizer, and stirring at normal temperature at 1000 rpm for 1h to obtain uniform emulsion;
(4) and (3) carrying out spray drying on the emulsion under the conditions that the air inlet temperature is 125 ℃, the air outlet temperature is 90 ℃ and the feeding speed is 10mL/min to obtain a microcapsule powder sample 1.
Example 2
(1) Adding sodium alginate into 1L of pure water, stirring for dissolving, sequentially adding Tween 60 and cinnamyl alcohol, and fully stirring to form a uniform mixed solution, wherein the mass content of sodium alginate is 5g/L, the mass content of Tween 60 is 4g/L, and the mass content of cinnamyl alcohol is 30 g/L;
(2) adding gelatin into pure water, stirring and dissolving in water bath at 60 ℃, and cooling to room temperature to obtain 10g/L gelatin water solution;
(3) slowly adding gelatin aqueous solution into the mixed solution, homogenizing for 5min at 3500rpm by high-speed dispersion homogenizer, and stirring at 1000 rpm for 2 hr at normal temperature to obtain uniform emulsion;
(4) and (3) carrying out spray drying on the emulsion under the conditions that the air inlet temperature is 125 ℃, the air outlet temperature is 90 ℃ and the feeding speed is 10mL/min to obtain a microcapsule powder sample 2.
Example 3
(1) Adding sodium alginate into 1L of pure water, stirring for dissolving, sequentially adding Tween 60 and cinnamyl alcohol, and fully stirring to form a uniform mixed solution, wherein the mass content of sodium alginate is 15g/L, the mass content of Tween 60 is 6g/L, and the mass content of cinnamyl alcohol is 10 g/L;
(2) adding gelatin into pure water, stirring and dissolving in water bath at 60 ℃, and cooling to room temperature to obtain 20g/L gelatin water solution;
(3) slowly adding gelatin aqueous solution into the mixed solution, homogenizing for 5min at 3500rpm by high-speed dispersion homogenizer, and stirring at normal temperature at 1000 rpm for 1.5 hr to obtain uniform emulsion;
(4) and (3) carrying out spray drying on the emulsion under the conditions that the air inlet temperature is 125 ℃, the air outlet temperature is 90 ℃ and the feeding speed is 10mL/min to obtain a microcapsule powder sample 3.
Example 4
The microcapsule powder samples of examples 1-3 were each mixed with 75% W/W alcohol, kept in a wet state suitable for granulation, granulated by a granulator, dried at 80 ℃, and sieved through a 14-25 mesh screen to obtain composite microcapsule particles 1-3.
Comparative example 1
The gelatin in example 1 was replaced with pectin of equal mass, and the rest was the same as in example 1, to obtain microcapsule powder sample a 1;
the same procedure as in example 1 was repeated except for replacing the gelatin in example 1 with the gum arabic of equal mass, to obtain microcapsule powder sample a 2.
Comparative example 2
The mass content of sodium alginate in example 1 was adjusted to 5g/L, and the rest was the same as in example 1, whereby microcapsule powder sample B1 was obtained;
a microcapsule powder sample B2 was obtained in the same manner as in example 1 except that the mass content of sodium alginate in example 1 was adjusted to 20 g/L.
Comparative example 3
The mass content of the gelatin aqueous solution in example 1 was adjusted to 5g/L, and the rest was the same as in example 1, to obtain microcapsule powder sample C1;
a microcapsule powder sample C2 was obtained in the same manner as in example 1 except that the mass content of the aqueous gelatin solution in example 1 was adjusted to 25 g/L.
Comparative example 4
The same procedures as in example 1 were repeated except for adjusting the mass content of tween 60 in example 1 to 1g/L to obtain a microcapsule powder sample D1;
the same procedure as in example 1 was repeated except for adjusting the mass content of Tween 60 in example 1 to 8g/L to obtain microcapsule powder sample D2.
Comparative example 5
The same procedure as in example 1 was repeated except for adjusting the cinnamyl alcohol mass content to 5g/L in example 1 to obtain microcapsule powder sample E1;
the same procedure as in example 1 was repeated except that the amount of cinnamyl alcohol in example 1 was adjusted to 60g/L to obtain microcapsule powder sample E2.
Comparative example 6
After homogenization in step (3) of example 1, stirring was continued at normal temperature for 0.5h, the same as in example 1 was repeated, to obtain microcapsule powder sample F1;
after homogenization in step (3) of example 1, stirring was continued at room temperature for 4 hours, and the same procedure as in example 1 was repeated to obtain microcapsule powder sample F2.
Test example 1 determination of the Total cinnamyl alcohol content and the embedding Rate of microcapsules
(1) Determination of the total content of cinnamyl alcohol in the microcapsules:
the total cinnamyl alcohol content in the microcapsule powder samples of examples 1-3 and comparative examples 1-6 was determined.
The determination method comprises the following steps: accurately weighing 10mg of cinnamyl alcohol, fully dissolving the cinnamyl alcohol by absolute ethyl alcohol, then fixing the volume to 10mL to obtain a cinnamyl alcohol ethanol solution with the concentration of 1mg/mL, then diluting the cinnamyl alcohol ethanol solution with 100 times to 0.01mg/mL by using ethanol as a stock solution, diluting the stock solution, respectively preparing the cinnamyl alcohol ethanol solution with the concentration of 1.5, 3.0, 4.5, 6.0, 7.5 and 9.0 mu g/mL, and measuring the absorbance at 250nm to obtain a standard working curve y of the absorbance to the cinnamyl alcohol concentration of 0.1103x +0.0162, wherein R2 is 0.9989 (y: absorbance; x: cinnamyl alcohol concentration). Weighing 0.1g of microcapsule powder sample, adding 10mL of absolute ethyl alcohol, performing vortex oscillation for 1min, then performing ultrasonic treatment for 10min, after complete dispersion, centrifuging at 6000rpm for 5min, absorbing and diluting the supernatant, measuring the absorbance of the supernatant at the wavelength of 250nm, calculating the cinnamyl alcohol concentration in the supernatant according to a standard working curve, and further calculating the total cinnamyl alcohol content in the microcapsule powder sample.
(2) Determination of the encapsulation efficiency of the microcapsules:
the embedding rate of the microcapsule powder samples of examples 1 to 3 and comparative examples 1 to 6 was measured.
The determination method comprises the following steps: a0.1 g sample of the microcapsule powder was weighed into a beaker and washed with 10ml of absolute ethanol and filtered. Measuring the light absorption value at 250nm after the filtrate is diluted, calculating the weight content of the cinnamyl alcohol residual on the surface of the microcapsule powder sample according to a standard working curve, and recording as m0. The total cinnamyl alcohol content in the microcapsule powder sample determined above was recorded as m1The microcapsule embedding rate Y is calculated according to the following formula.
The above results are shown in Table 1.
TABLE 1 Total cinnamyl alcohol content and encapsulation efficiency results in microcapsule powder samples
As can be seen from table 1, the microcapsule powder samples prepared by the method of the present invention have a higher total cinnamyl alcohol content and a higher entrapment rate than the microcapsule powder samples prepared by comparative examples 1 to 6.
Test example 2 Release uniformity and Slow Release Effect
Composite microcapsule particles made from the microcapsule powder samples of examples 1-3 (see example 4 for method) were added into a filter rod with a ternary cavity and rolled into cigarettes 1-3; the control cigarette is prepared by adding equivalent cinnamyl alcohol into a filter stick.
(1) And (3) measuring the cinnamyl alcohol content of the smoke of the cigarettes 1-3 and the control cigarettes in the smoking process.
a. Materials, reagents and instruments:
phenethyl acetate (standard), ethyl acetate (HPLC) (lark corporation); anhydrous sodium sulfate, sodium chloride (AR, national drug stock limited); pure water (self-made, meeting the requirements of first-grade water in GB/T6682-2008 [1 ]); TRACE1310 gas chromatography + ISQ LT quadrupole mass spectrometry (Thermo corporation, USA); 7890A gas chromatograph (Agilent, USA); RM20H carousel-type smoking machines; ML204 electronic balance (sensory 0.0001 g, Toledo company, Metler, Switzerland); elmasonic S300 ultrasonic extractor (Elma, germany); Milli-Q ultra pure water machine (Millipore, USA).
b. The method comprises the following steps:
accurately transferring a certain volume of standard stock solution (cinnamyl alcohol) and internal standard (phenethylacetate) stock solution into a 50mL volumetric flask, and performing constant volume by using ethyl acetate to obtain a series of standard solutions with the concentration range of 5.0-250 mu g/mL, wherein the internal standard concentration is 2.0 mu g/mL. Smoking 20 blank cigarettes by using a rotary disc type smoking machine, and collecting total particulate matters by using a Cambridge filter disc; the filter disc was extracted with 10mL of ethyl acetate, and the extract was washed with 10mL of saturated brine and 0.5mL of 5% hydrochloric acid, dried over anhydrous sodium sulfate, and then filtered through a 0.45 μm Polytetrafluoroethylene (PTFE) filter to obtain a smoke matrix solution. Respectively transferring 2.0mL of smoke matrix solution, adding the smoke matrix solution into the series of standard solutions, shaking up, and standing to obtain a smoke matrix matching standard solution.
By using
Cambridge filter piece mouth-by-mouth trappingExtracting each filter disc with 10mL of ethyl acetate containing an internal standard (the content of phenethyl acetate of the internal standard is the same as that in the smoke matrix matching standard solution), performing ultrasonic extraction for 30min, and filtering the extract through a 0.45-micron filter membrane to obtain a sample solution.
Detecting the matching of the flue gas matrix with the standard solution and the sample solution by adopting GC/MS, wherein the operation conditions are as follows: a chromatographic column: DB-5 capillary column (60m 0.25mm 0.25 μm); sample inlet temperature: 250 ℃; sample introduction amount: 1.0 μ L; the pulse is not shunted; carrier gas: he, 1.5 mL/min; temperature programming: maintaining at 50 deg.C for 2min, increasing to 220 deg.C at 8 deg.C/min, maintaining at 220 deg.C for 23.25min, increasing to 300 deg.C at 20 deg.C/min, and maintaining at 300 deg.C for 27.25 min; an ion source: EI; electron energy: 70 eV; transmission line temperature: 250 ℃; ion source temperature: 250 ℃; solvent retardation: 8 min; mass scan range: 45-300 amu; SCAN and SIM are used simultaneously.
Performing qualitative search with NIST standard library, wherein the retention time of cinnamyl alcohol is 18.35min, the qualitative ion is 92, 115, 134(m/z), and the quantitative ion is 92 (m/z). Establishing an internal standard method standard working curve according to the content of cinnamyl alcohol and an internal standard in the smoke matrix matching standard solution and the measured intensity value, substituting the intensity value detected by the sample solution into the internal standard method standard working curve to calculate the content of cinnamyl alcohol in the sample solution, further calculating the content of cinnamyl alcohol in the cigarette-by-cigarette, and taking the average value of 20 cigarettes, wherein the result is shown in figure 1.
(2) And (3) measuring the cinnamyl alcohol content of the total smoke in the smoking process of the cigarettes 1-3 and the control cigarettes after being placed for a period of time.
After 20 cigarettes are left for a period of time, use
The Cambridge filter disc captures total particulate matters in the mainstream smoke of each cigarette in the whole smoking process, each filter disc is extracted by 10mL of ethyl acetate containing an internal standard (the content of the phenethyl acetate of the internal standard is the same as that in the smoke matrix matching standard solution), ultrasonic extraction is carried out for 30min, and the extract is filtered by a 0.45 mu m filter membrane to obtain a sample solution; the rest are the same as in the above item (1); calculating the standing timeTaking the average value of 20 cigarettes according to the cinnamyl alcohol content of the total smoke in the smoking process of the later cigarettes.
The cinnamyl alcohol content of the total smoke during smoking of cigarettes 1-3 and control cigarettes after standing for 1 day, 15 days, 30 days and 60 days was determined according to the above method, and the results are shown in table 2.
TABLE 2
As can be seen from fig. 1, compared with the control cigarette, the content of cinnamyl alcohol in the smoke of the cigarette of the invention is more uniform during smoking, which indicates that the fragrance of cinnamyl alcohol in the cigarette of the invention is more uniform;
as can be seen from Table 2, compared with the control cigarette, the cigarette of the present invention can release cinnamyl alcohol substantially stably for a long time, and has a good cinnamyl alcohol fragrance slow-release effect and a long-lasting fragrance-maintaining ability, thereby prolonging the shelf life of the product.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for preparing cinnamyl alcohol microcapsules, comprising the steps of:
(1) mixing a sodium alginate solution, tween 60 and cinnamyl alcohol to obtain a first mixture;
(2) slowly adding a gelatin solution into the first mixture, and mixing to obtain a second mixture;
(3) spray drying the second mixture to obtain cinnamyl alcohol microcapsules;
wherein the mass ratio of the sodium alginate to the gelatin is 1 (1-2.2), the mass of the Tween 60 is 6-30% of the total mass of the sodium alginate and the gelatin, and the mass of the cinnamyl alcohol is 24-210% of the total mass of the sodium alginate and the gelatin.
2. The method according to claim 1, wherein in the step (2), the mixing is performed by homogenizing and then stirring;
preferably, the stirring treatment is carried out for 0.5 to 3 hours.
3. The method as claimed in claim 1 or 2, wherein in the step (1), the concentration of the sodium alginate solution is 3-20 g/L.
4. The method according to any one of claims 1 to 3, characterized by one or more of the following:
1) in the step (2), the concentration of the gelatin solution is 8-25 g/L;
2) in the step (2), homogenizing for 2-10 minutes;
3) in the step (2), homogenizing treatment is carried out by adopting a homogenizer; preferably, the rotating speed of the refiner is 3000-4000 rpm;
4) in the step (2), stirring treatment is carried out at normal temperature;
5) in the step (2), the rotating speed of stirring treatment is 400-1600 rpm;
6) in the step (3), the air inlet temperature of spray drying is 115-135 ℃;
7) in the step (3), the air outlet temperature of spray drying is 80-100 ℃;
8) in the step (3), the feeding speed of spray drying is 5-18 mL/min.
5. A cinnamyl alcohol microcapsule prepared by the process of any one of claims 1 to 4; preferably, the mass content of cinnamyl alcohol in the cinnamyl alcohol microcapsule is not less than 20%; preferably, the encapsulation rate of the cinnamyl alcohol microcapsules is not less than 70%.
6. A method for preparing granules for cigarettes comprises the following steps:
mixing the cinnamyl alcohol microcapsules with alcohol or a solution thereof, granulating, drying, and optionally screening to obtain granules for cigarettes; wherein the cinnamyl alcohol microcapsule is a cinnamyl alcohol microcapsule prepared by the method of any one of claims 1 to 4 or the cinnamyl alcohol microcapsule of claim 5.
7. A granule for tobacco, which is obtained by the method of claim 6.
8. A filter plug or filter comprising the cinnamyl alcohol microcapsule of claim 5 or the tobacco granule of claim 7.
9. A tobacco product comprising the cinnamyl alcohol microcapsule of claim 5, the tobacco granule of claim 7 or the filter plug or filter of claim 8; preferably, the tobacco product is a cigarette.
10. Use of the cinnamyl alcohol microcapsule of claim 5, the granule for cigarettes of claim 7 or the filter rod or filter of claim 8 in a tobacco product; preferably, the tobacco product is a cigarette.
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| CN116236983A (en) * | 2023-03-14 | 2023-06-09 | 福建中烟工业有限责任公司 | Fat-soluble essence slow-release double-layer microcapsule for cigarettes and preparation method thereof |
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