CN114287664A - Preparation method of granular microcapsule type spice and application of granular microcapsule type spice in cigarettes - Google Patents
Preparation method of granular microcapsule type spice and application of granular microcapsule type spice in cigarettes Download PDFInfo
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- AEMOLEFTQBMNLQ-AZLKCVHYSA-N (2r,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-AZLKCVHYSA-N 0.000 claims description 5
- AEMOLEFTQBMNLQ-SYJWYVCOSA-N (2s,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-SYJWYVCOSA-N 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
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- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a preparation method of granular microcapsule type spice and application of the granular microcapsule type spice in cigarettes, wherein the preparation method comprises the following steps: (1) preparing a wall material A raw material; (2) preparing a curing liquid; (3) preparing a core material; (4) and (4) preparing microcapsules. According to the invention, natural polysaccharide and amylose corn porous starch are selected as wall materials by adopting a coagulation coprecipitation method, a core material is well wrapped in the wall materials, the natural polysaccharide polymer and the furfural polymer are crosslinked, and the structure of the freeze-dried microcapsule is not damaged. The granular capsule type spice prepared by the invention is applied to the field of tobacco, the slow release performance of the embedded spice is improved, the fragrance retention time is prolonged, and sensory evaluation results show that cigarettes added with the capsule type spice are full in fragrance, good in penetrability, fine and soft in smoke, and capable of obviously improving and promoting the quality characteristics of cigarette products.
Description
Technical Field
The invention belongs to the field of application of tobacco industry, and particularly relates to a preparation method of a granular microcapsule type spice and application of the granular microcapsule type spice in cigarettes.
Background
The microcapsule is prepared by coating solid or liquid medicament with natural or synthetic polymer material as capsule wall shell. After microencapsulation, the release time and the release rate of the core material can be controlled, so that the application time is prolonged, the effective period is prolonged, and in addition, the wall material of the microcapsule isolates the core material from the external environment such as temperature, ultraviolet rays, humidity and the like, so that the stability of the microcapsule is better. The microcapsule has the above functions, so that the microcapsule can be widely applied to the fields of medicines, foods, pesticides and the like.
Because of the influence of the difference of raw materials, the cigarette product can have the problems of insufficient aroma, outstanding miscellaneous gas, strong irritation and the like, the quality of the product can be effectively improved by selecting proper spices according to the style characteristics of the product, and the loss of the added spices inevitably occurs in the actual production process at present because the processing temperature and the moisture need to be adjusted in real time in the cigarette production link according to the processing requirements, so that the improvement effect of the traditional spices on the quality of the product is naturally influenced. Some researches are based on methods in other fields, and attempt to combine microcapsules with tobacco essence and flavor, but the requirements and the characteristics of temperature resistance and pressure resistance of the original auxiliary materials in the processing process in the tobacco field are not met, so that the prepared essence microcapsules have the defects of poor rigidity, poor processing resistance, poor stability and poor structure retention capability. Besides, the essence is taken as a microcapsule form, the embedding rate of the essence is also a very important index for the slow release effect and the final sensory evaluation effect, otherwise, if the embedding rate is very low, the essence is made into the microcapsule form and has no significance.
Therefore, people hope to find out a preparation method of microcapsule-type perfume suitable for the tobacco field, so that the prepared microcapsule-type perfume has higher embedding rate and stability, and the advantage of the microcapsule is really exerted.
The present invention has been made to solve the above problems.
Disclosure of Invention
In order to further improve the quality of cigarette products, the invention develops a novel granular microcapsule spice which is applicable to the field of tobacco, can delay the pyrolysis of an embedding substance, has better rigidity, high embedding rate and good stability, and is applied to the field of cigarette production.
The invention provides a preparation method of granular microcapsule type perfume, which comprises the following steps:
(1) preparing a wall material A raw material: preparing a polysaccharide polymer solution from a purified natural polysaccharide polymer, adding a certain amount of gelatin and lactose solution, and stirring and dissolving to obtain a wall material A raw material;
(2) preparing a curing liquid: dissolving a certain amount of linear polymer formed by connecting beta-D-mannuronic acid and alpha-L-guluronic acid according to 1-4 glycosidic bonds, a mixture of branched corn porous starch and plant pectin and anhydrous calcium chloride in water, and adjusting the pH value to 4-6; wherein the wall material B is a linear polymer formed by connecting beta-D-mannuronic acid and alpha-L-guluronic acid according to 1-4 glycosidic bonds; the mixture of the branched corn porous starch and the plant pectin is the wall material C;
(3) preparing a core material: mixing the core material to be embedded with the spice core material according to the core-wall ratio of 2: 1, adding the mixture into the wall material A solution, stirring, and standing to room temperature after complete dissolution to obtain a wall material A and core material mixed solution;
the sample to be embedded here can be a natural plant extract or other desired flavor.
(4) Preparing microcapsules: slowly adding the mixed solution of the wall material A and the core material prepared in the step (3) into the solidified solution obtained in the step (3) through a peristaltic pump, stirring, standing to obtain microspheres with uniform and round shapes, filtering, separating, vacuum-filtering, and freeze-drying to obtain the granular microcapsule type spice.
Preferably, in step (1), the purity of the purified natural polysaccharide polymer reaches more than 95%, and the natural polysaccharide polymer is selected from but not limited to spirulina polysaccharide, aloe polysaccharide, cactus polysaccharide and ganoderma lucidum polysaccharide; preparing 0.5-1.5% polysaccharide polymer solution; the gelatin and the lactose are added to increase the stability of the granular microcapsule type perfume and improve the embedding rate of the granular microcapsule type perfume, and the mass ratio of the gelatin to the lactose is 2-4; the stirring temperature is 40-45 ℃, the magnetic stirring speed is 400-450rpm, and the stirring time is 30-40 min.
Preferably, in the step (2), the mass fraction of the anhydrous calcium chloride is 1.5-5%; in the step (2), the concentration of the wall material B is 3.5-5.5%, the concentration of the wall material C is 1-3%, and then the pH value is adjusted by sodium bicarbonate.
Preferably, in the step (3), the stirring temperature is 40-45 ℃ and the stirring time is 25-50 min.
Preferably, in the step (4), the stirring time is 20-30min, and the standing time is 20-30 min; in the step (4), the freeze drying temperature is-20 to-30 ℃, and the freeze drying time is 12 to 24 hours.
In a second aspect, the present invention provides a granular microcapsule-type perfume obtained by the method for producing a granular microcapsule-type perfume according to the first aspect of the present invention.
In a third aspect of the present invention, there is provided a use of the particulate microcapsule-type perfume of the second aspect of the present invention in a cigarette, wherein the particulate microcapsule-type perfume is added to tobacco shreds in an amount of 4 to 8mg per cigarette, and the cigarette is prepared. A sensory evaluation group is formed by 10 fixed persons who engage in cigarette blending for a long time and have rich sensory analysis experience, smoking evaluation is carried out on cigarette samples, and the style characteristics and the quality characteristics of the cigarette samples are evaluated respectively.
According to the fourth aspect of the invention, the method for improving the slow release effect of the spice added into the cut tobacco is used for preparing the spice into granular microcapsules and then adding the granular microcapsules into the cut tobacco.
Preferably, the method for improving the stability and encapsulation efficiency of the granular microcapsule-type flavor is to add a certain amount of gelatin and lactose solution during the microcapsule preparation process.
The embedding rate of the obtained granular microcapsule product is measured.
The embedding rate is calculated as follows:
the embedding rate (%) - (sum of peak areas of main components of the core material embedded by the microcapsules/sum of peak areas of main components of the core material multiplied by 100%
The stability of the invention refers to the ability of the microspheres obtained in the step (4) to remain intact after freeze drying without damaging the structure.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention explores a preparation method of the granular capsule type spice suitable for tobacco according to the requirements and characteristics of tobacco application, the capsule type spice prepared by the method has a complete capsule wall structure and better rigidity, microencapsulation delays the pyrolysis of an embedding object, shows that the wall material has a protection effect on a core material, achieves the purpose of embedding, and well meets the special requirements of temperature change caused by tobacco heating combustion and mechanical collision caused in a rolling process on the original auxiliary material. Specifically, a certain amount of gelatin and lactose solution is added in the microcapsule preparation process, the proportion of the gelatin and the lactose is ensured to be 2-4, and the condition can obviously improve the embedding rate of the granular microcapsule type perfume, thereby ensuring the slow release effect and the sensory evaluation effect of the microcapsule type perfume.
2. According to the invention, natural polysaccharide and amylose corn porous starch are selected as wall materials, the perfume material is successfully embedded, the core material is well wrapped in the wall materials, the granular capsule prepared by the method has high perfume embedding rate and good stability, the natural polysaccharide polymer and the furfural polymer are crosslinked, and the structure of the freeze-dried microcapsule is not damaged. The selected wall materials are all nontoxic, good biocompatibility and biodegradable materials.
3. The granular capsule spice prepared by the invention is applied to the field of tobacco, the slow release performance of an embedding substance spice is improved, the fragrance retention time is prolonged, and sensory evaluation results show that cigarettes added with the granular capsule spice are full in fragrance, good in penetrability, fine and soft in smoke, and capable of obviously improving and promoting the quality characteristics of cigarette products. And moreover, the microcapsule not only brings in spice components, but also can bring in partial moisture, and the purpose of keeping moisture and increasing aroma of the cigarette can be achieved.
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Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental methods not specified in the examples are generally commercially available according to the conventional conditions and the conditions described in the manual, or according to the general-purpose equipment, materials, reagents and the like used under the conditions recommended by the manufacturer, unless otherwise specified. The starting materials required in the following examples and comparative examples are all commercially available.
Example 1
(1) Preparing a wall material A raw material: taking purified spirulina polysaccharide (purity is 95%), preparing 1.0% polysaccharide solution, adding a certain amount of gelatin and lactose solution, stirring under magnetic force at a rotation speed of 450rpm for 30min, wherein the ratio of gelatin to lactose is 3:1, and stirring at 42 deg.C for completely dissolving.
(2) Preparation of curing liquid (wall material B and wall material C): dissolving a certain amount of wall material B (a linear polymer formed by connecting beta-D-mannuronic acid and alpha-L-guluronic acid by 1-4 glycosidic bonds) and wall material C (a mixture of amylopectin corn porous starch and plant pectin) with a certain amount of anhydrous calcium chloride in water, wherein the concentration of the wall material B is 4 percent, the concentration of the wall material C is 1.5 percent, and adjusting the pH value to 5 by using sodium bicarbonate.
(3) Preparing a core material: mixing the notoginseng extract according to the ratio of core to wall of 2: 1, adding the mixture into the wall material A solution, stirring in a water bath at 42 ℃ for 30min, and standing to room temperature after complete dissolution.
(4) Preparing microcapsules: slowly adding the mixed solution of the wall material A and the core material into the curing solution through a peristaltic pump, stirring for 30min, standing for 30min to obtain microspheres with uniform and round shapes, filtering and separating, performing vacuum filtration, and performing freeze drying to obtain the microcapsule product. The embedding rate was measured. The freeze drying temperature is-25 deg.C, and the freeze drying time is 15 h.
The application of the granular microcapsule type spice in cigarettes comprises the following steps: the granular microcapsule type perfume prepared by the invention is added into tobacco shreds according to the addition of 6 mg/cigarette, and cigarettes are prepared. And the cigarette sample is evaluated.
Comparative example 1
For comparison, the same brand of cigarette without added microcapsule flavor was used as a control.
Example 2
The perfume was also prepared in the form of microcapsules, and the preparation method of the microcapsule perfume was substantially identical to that of example 1 except that gelatin and lactose were not added during the preparation in step (1).
Example 3
The flavor was also prepared in the form of microcapsules, which were prepared in substantially the same manner as in example 1 except that gelatin was not added during the preparation in step (1) and only 2% lactose was added.
Example 4
The flavor was also prepared in the form of microcapsules, which were prepared in substantially the same manner as in example 1 except that lactose was not added during the preparation in step (1) and only 3% gelatin was added.
Example 5
The perfume was also prepared in the form of microcapsules, which were prepared in substantially the same manner as in example 1 except that the gelatin and lactose were added in a ratio of 1:1 during the preparation in step (1).
Example 6
The perfume was also prepared in the form of microcapsules, the process for preparing the microencapsulated perfume being substantially identical to that of example 1 except that the gelatin and lactose were added in a ratio of 5:1 during the preparation in step (1).
Example 7
The perfume was also prepared in the form of microcapsules, and the preparation method of the microcapsule perfume was substantially the same as that of example 1 except that ethylcellulose was selected as the wall materials B and C in step (2).
TABLE 1 comparison of embedding rates and sensory test results
As can be seen from Table 1, the embedding rate of the granular microcapsule spice prepared by the invention is obviously higher than that of the comparative example, and when the granular microcapsule spice is applied to tobacco, the cigarette product has the advantages of full aroma, enough quantity, good hair penetration, fine and smooth smoke, softness, good smoothness, appropriate aftertaste and obvious improvement and promotion effect on the quality characteristics of the cigarette product. The particle type capsule spice prepared by the invention delays the pyrolysis of an embedding substance due to microencapsulation, and the wall material has a protection effect on the core material, thereby achieving the purpose of embedding, well meeting the special requirement of temperature change caused by heating and burning tobacco on the original auxiliary material, having good slow release performance and prolonged aroma retention time.
In addition, in comparative example 7 and example 1, the prepared granular capsule perfume has high embedding rate and good stability by using the selected natural polysaccharide and the amylose porous starch as wall materials, the natural polysaccharide polymer and the furfural polymer are crosslinked, and the structure of the freeze-dried microcapsule is not damaged. In example 7, ethyl cellulose is selected as a wall material, and the structure of the prepared granular capsule flavor is obviously damaged in the freeze-drying process, which is also the reason that the embedding rate of the sample in example 7 is far lower than that in other examples.
Claims (9)
1. A method for preparing a granular microcapsule-type perfume, comprising the steps of:
(1) preparing a wall material A raw material: preparing a polysaccharide polymer solution from a purified natural polysaccharide polymer, adding a certain amount of gelatin and lactose solution, and stirring and dissolving to obtain a wall material A raw material;
(2) preparing a curing liquid: dissolving a certain amount of linear polymer formed by connecting beta-D-mannuronic acid and alpha-L-guluronic acid according to 1-4 glycosidic bonds, a mixture of branched corn porous starch and plant pectin and anhydrous calcium chloride in water, and adjusting the pH value to 4-6; wherein the wall material B is a linear polymer formed by connecting beta-D-mannuronic acid and alpha-L-guluronic acid according to 1-4 glycosidic bonds; the mixture of the branched corn porous starch and the plant pectin is the wall material C;
(3) preparing a core material: mixing the core material to be embedded with the spice core material according to the core-wall ratio of 2: 1, adding the mixture into the wall material A solution, stirring, dissolving, and standing to room temperature to obtain a wall material A and core material mixed solution;
(4) preparing microcapsules: and (4) slowly adding the mixed solution of the wall material A and the core material prepared in the step (3) into the solidified solution obtained in the step (3) through a peristaltic pump, stirring, standing to obtain microspheres, filtering, separating, performing vacuum filtration, and freeze-drying to obtain the granular microcapsule type spice.
2. The method for preparing a perfume of a granular microcapsule type according to claim 1, wherein in the step (1), the purity of the purified natural polysaccharide polymer is up to 95% or more, and the natural polysaccharide polymer is selected from spirulina polysaccharide, aloe polysaccharide, cactus polysaccharide, ganoderma lucidum polysaccharide; preparing 0.5-1.5% polysaccharide polymer solution; the gelatin and the lactose are added to increase the stability of the granular microcapsule type perfume and improve the embedding rate of the granular microcapsule type perfume, and the mass ratio of the gelatin to the lactose is 2-4; the stirring temperature is 40-45 ℃, the magnetic stirring speed is 400-450rpm, and the stirring time is 30-40 min.
3. The method for producing a granular microcapsule-type perfume according to claim 1, wherein in the step (2), the mass fraction of anhydrous calcium chloride is 1.5 to 5%; in the step (2), the concentration of the wall material B is 3.5-5.5%, the concentration of the wall material C is 1-3%, and then the pH value is adjusted by sodium bicarbonate.
4. The method for preparing a perfume of a microcapsule type in a particle form according to claim 1, wherein the stirring temperature in the step (3) is 40 to 45 ℃ and the stirring time is 25 to 50 min.
5. The method for producing a granular microcapsule-type perfume according to claim 1, wherein in the step (4), the stirring time is 20 to 30min, and the standing time is 20 to 30 min; in the step (4), the freeze drying temperature is-20 to-30 ℃, and the freeze drying time is 12 to 24 hours.
6. A granular microcapsule-type perfume obtained by the method for producing a granular microcapsule-type perfume according to any one of claims 1 to 5.
7. The use of the particulate microcapsule-type flavor of claim 6 in cigarettes, wherein the particulate microcapsule-type flavor is added to tobacco shreds in an amount of 4-8 mg/cigarette and made into cigarettes.
8. A method for improving the slow release effect of a flavor added to cut tobacco, characterized in that the flavor is made into a granular microcapsule form by the preparation method of any one of claims 1 to 5 and then added to the cut tobacco.
9. The method of claim 8, wherein the particulate microcapsule flavor is stabilized and encapsulated by adding a quantity of gelatin and lactose solution during the microcapsule preparation.
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|---|---|---|---|---|
| GB1284151A (en) * | 1969-08-18 | 1972-08-02 | Int Flavors & Fragrances Inc | Tobacco containing encapsulated flavor |
| CN102763684A (en) * | 2011-05-01 | 2012-11-07 | 华中农业大学 | Microcapsule preparation, preparation method and application |
| CN111013505A (en) * | 2019-12-25 | 2020-04-17 | 郑州轻工业大学 | Sustained-release essence microcapsule for cigarettes and preparation method thereof |
| CN112716029A (en) * | 2020-12-21 | 2021-04-30 | 安徽中烟工业有限责任公司 | Granular nano-microcapsule for heating cigarettes and preparation method thereof |
-
2021
- 2021-12-08 CN CN202111493293.8A patent/CN114287664A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1284151A (en) * | 1969-08-18 | 1972-08-02 | Int Flavors & Fragrances Inc | Tobacco containing encapsulated flavor |
| CN102763684A (en) * | 2011-05-01 | 2012-11-07 | 华中农业大学 | Microcapsule preparation, preparation method and application |
| CN111013505A (en) * | 2019-12-25 | 2020-04-17 | 郑州轻工业大学 | Sustained-release essence microcapsule for cigarettes and preparation method thereof |
| CN112716029A (en) * | 2020-12-21 | 2021-04-30 | 安徽中烟工业有限责任公司 | Granular nano-microcapsule for heating cigarettes and preparation method thereof |
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