JPS5941397B2 - Beaded gel containing flavoring and tobacco products containing the same - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a beaded gel containing a flavoring agent and a tobacco product containing the same.

More specifically, a fragrance is encapsulated using a heat-coagulable polysaccharide mainly composed of β-1,3-glycosidic bonds, and bead-shaped gels (sometimes referred to as microcapsules) containing the fragrance as a core material are produced. The present invention relates to tobacco products containing said microcapsules.

Flavoring agents have traditionally been used in the fields of tobacco and food products to improve the flavor and palatability, but the flavoring method, which simply impregnates or mixes flavoring agents into raw materials such as tobacco and food products, is difficult in the manufacturing process of those products. It is impossible to achieve this purpose if the fragrance is lost or altered during the storage of the product.

For this purpose, methods of stabilizing fragrances and adding them to raw materials are widely used.

However, to explain an example in the tobacco field, conventional methods for stabilizing flavorings have not been able to provide sufficient stability, and even if they can be stabilized, the combustion odor of the stabilizer itself is not desirable for tobacco. In addition, since stabilized products are water-soluble, their use has often been limited.

The bead-shaped gel containing the flavoring agent of the present invention is insoluble in water, and the flavoring agent is stably retained at room temperature, so it can be added to tobacco raw materials, processed products thereof, or tobacco products.
When smoking, aroma components are released to give the tobacco its flavor, and the combustion odor of the heat-coagulable polysaccharide itself, which is mainly composed of β-1,3-glycosidic bonds and is used as a stabilizer, is the cigarette odor. It does not impair the aroma and taste of tobacco, harmonizes well with tobacco flavorings, and is effective in improving the aroma and taste of tobacco.

That is, the present invention provides a bead-shaped gel containing a fragrance, which is prepared by mixing an alkaline aqueous solution of a heat-coagulable polysaccharide mainly composed of β-1,3-glycosidic bonds and a fragrance, and bringing the mixture into contact with a gelling agent. The present invention relates to tobacco products containing the same.

The heat-coagulable polysaccharide mainly composed of β-1,3-glycosidic bonds (hereinafter sometimes referred to as "this polysaccharide") used in the present invention includes, for example, alkaline earth metals or Agrobacterium spp. Specifically, polysaccharides produced by Alcaligenes var.
(IFO13140) (Special Publication No. 48-32673) (hereinafter referred to as "Polysaccharide B")
Agrobacterium radiobacter (I FO1'3
127) and its mutant strain u-19 (IF013126
) polysaccharides produced by
(9, hereinafter referred to as "polysaccharide C", etc. can be used.

For preparing an alkaline aqueous solution capable of dissolving these present polysaccharides, for example, sodium hydroxide, potassium hydroxide, ammonia, etc. can be used.

Examples of fragrances that can be stabilized in the present invention include menthol, organic acid esters (e.g., isoamyl acetate, ethyl butyrate, n-butyl acetate, etc.), and essential oils (e.g., geraniol, citronellol, isoeugenol, etc.). It will be done.

Any gelling agent that can quickly gel the present polysaccharide can be used, but it is preferable to use an acid or an inorganic ion.

As the acid, any inorganic acid or organic acid can be used as long as it has a pH value of 6.0 or less.

Examples of inorganic acids that can be used include hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and boric acid, and examples of organic acids that can be used include formic acid, acetic acid, citric acid, lactic acid, and benzoic acid.

Further, as the inorganic ion, it is preferable to use, for example, calcium ion.

Next, a method for producing a bead-shaped gel containing the fragrance of the present invention will be explained.

That is, first, the present polysaccharide is added to distilled water to obtain a suspension.

In this case, oligosaccharides such as sucrose, corn syrup, textulose, maltose solution, ribose, and fructose may be added to the present polysaccharide as necessary.

The addition ratio of these oligosaccharides varies depending on the type of volatile flavor used, but is approximately 01 to 100% relative to the polysaccharide.

A fragrance or an alcohol (eg, ethanol) solution of a fragrance is added to the above suspension, and the mixture is mixed and stirred.

The amount of flavor added varies depending on the purpose of use of the bead-shaped gel produced, but is generally about 01 to 100% based on the polysaccharide.

Next, an alkaline aqueous solution is added to this for the purpose of dissolving the present polysaccharide.

The amount of alkaline aqueous solution added is generally such that the concentration of this polysaccharide is 0.
01-15%, preferably 1-10%, and the pH
It is desirable to carry out the process so that the value is generally between 9 and 13, preferably between 10 and 12.

A bead-shaped gel can be obtained by dropping the alkaline aqueous solution of the present polysaccharide containing the fragrance thus obtained into a gelling agent, or by adding the gelling agent to the alkaline aqueous solution while stirring.

When an acid is used as a gelling agent, it is sufficient that it is at least the equimolar amount of the alkali used, and when an inorganic ion is used, it is sufficient that it is at least the equimolar amount of the alkali used, but it is not less than 5 mol. By using it, gelation can be carried out quickly.

For dropping the alkaline aqueous solution of the present polysaccharide containing the fragrance into the gelling agent, for example, a pressurized nozzle or a device provided with an orifice can be used.

The size of the beaded gel containing the fragrance obtained in this way varies depending on the manufacturing conditions, but is generally about 5 to 5,000.
It is possible to produce beads with a particle size in the μ range, and generally by lowering the concentration of the alkaline aqueous solution of this polysaccharide, beads with a larger particle size can be obtained, and when adding the gelling agent to the alkaline aqueous solution of this polysaccharide, stirring is required. Increasing the speed generally results in beads with smaller particle sizes.

When the beaded gel containing the flavor obtained as described above is used for flavoring tobacco, it is generally preferable that the particle size is about 50 to 500 microns, although it varies depending on the purpose of use.

The amount of such bead-shaped gel added varies depending on the type of tobacco, use, preference, type of flavor, etc., but in most cases, it is preferably about 0.05 to 3% based on the combustible substrate.

The combustible substrate herein refers to natural leaf tobacco or smokable substitutes used in its place.

There are no particular restrictions on the timing or method of adding the present bead-shaped gel to tobacco, and it is generally added by adhesion to tobacco manufacturing raw materials or processed products thereof, or by the method described in U.S. Pat. No. 3,540,456. Similarly, it can also be kneaded into sheet cigarettes.

In addition, the quantitative analysis of menthol in the following experimental examples and examples was performed using gas chromatography (GC-4BPTF, manufactured by Shimadzu Corporation), and the analysis method was as follows.

Precisely weigh 1 g of microcapsules to 0.01 N-Na.
Dissolved in 30 ml of OH aqueous solution.

Next, 0.5% n-pentanol ethanol solution 1
0 ml was added and left overnight, and 0.6τ of it was injected into Gas Chroma 1-Graphie.

The column used was 9 mmφ x 2 m, 5% polyethylene glycol 20M was used as the liquid phase, and Gaschrome P (manufactured by Applied Science) was used as the trench carrier.

The temperature is raised from ioooC to 1300G'! f
The temperature was increased by 5°C per minute.

Its detection was by hydrogen flame method. Experimental Example 1 Microcapsules and polysaccharide B obtained in the examples below
05g of menthol was added to 5g and simply mixed to obtain [
Figure 1 shows the results of examining the change in menthol retention over time when the mixture was left in the air.

From FIG. 1, it is clear that the retention of the microcapsules of the present invention by number is extremely superior to that of the "mixture."

Experimental Example 2 (Example 7 without using this polysaccharide) 8 g of menthol was added to 120 g of a 10% gelatin aqueous solution consisting of 12.9 gelatin and 108 ml of distilled water, and the mixture was heated at 40°
The mixture was stirred at C.

Next, 120 g of a 10% gum arabic aqueous solution consisting of 12 g of gum arabic and 108 ml of distilled water was added and mixed to the above menthol dispersion at 40° C., and 15 TL of a 10% acetic acid aqueous solution was added to adjust the pH to 4.2.

570 ml of 40°C warm water was added so that the concentration of the gelatin/gum arabic aqueous solution was 1.5% to generate coacervation.

After gradually cooling the system to 5°C over 1 hour, 10ml of 25% glutaraldehyde aqueous solution was added as a hardening agent and stirred at 5°C for 2 hours to form microcapsules with menthol as the core material. did.

They are centrifuged and lyophilized to a menthol content of 1.
3% dried microcapsules13. :l was obtained.

Commercially available: 100 g of illite ■ 5 m of glycerin
1, and then 2 g of the dried microcapsules obtained in the above manner were sprinkled and mixed.

Next, it was dried for 5 minutes at 50°C in a dryer, and after being left to cool, it was heated using a test hoist to a length of 701nrft and a circumference of 257mm.
I obtained rolled-up menthol-containing tobacco products according to my friend's specifications.

This tobacco product had a protein smell produced when gelatin was burned, and the flavor was not at all pleasant.

Example 1 A processing suspension of 5 g of polysaccharide B (see text) in 90 ml of distilled water was obtained.

Dissolve 0.5.9 menthol in 30 ml of ethanol,
This solution was added to the suspension and stirred and mixed for about 15 minutes.

10 ml of IN-KOH aqueous solution was added to this to dissolve polysaccharide B.

When the obtained menthol dispersion was dropped into a stirred solution of 100 d of a 20% calcium chloride aqueous solution through an orifice with an inner diameter of 1 mm, it immediately gelled to form capsules.

The product was filtered through a nylon cloth, washed with water, and freeze-dried.

7 g of microcapsules were obtained, the menthol content of which was 4.3%, and 61% of the added menthol was encapsulated.

Example 2 In the same manner as in Example 1, 20 nl of IN-HC was used instead of calcium chloride as a gelling agent.

Freeze-drying yielded 4.2 g of solid microcapsules,5 with a menthol content of 3.6% and 30% of the added menthol being encapsulated.

Example 3 In the same manner as in Example 1, 5 g of sucrose was added to 5 g of polysaccharide B, and the menthol content was 2.2%.
microcapsules were obtained.

52% of the added menthol was encapsulated.

Example 4 In the same manner as in Example 1, 5 g of glucose was further added to 5 g of polysaccharide B, and the menthol content was reduced to 1.
．． 8% microcapsules were obtained.

48% of the added menthol was encapsulated.

Example 5 In the same manner as in Example 1, 2.5 g of sucrose was added to 5 g of polysaccharide B.
microcapsules were obtained by adding 2.5 g of glucose and 2.5 g of glucose.

Its menthol content was 2.1% and 56% of the added menthol was encapsulated.

Example 6 In the same manner as in Example 2, sucrose 2.
Microcapsules were obtained by adding 5 g of glucose and 2.5 g of glucose.

Its menthol content was 1.5% and 21% of the added menthol was encapsulated.

Example 7 In the same manner as in Example 1, microcapsules were obtained by adding menthol as a powder without using ethanol to dissolve it.

The menthol content was 1.9%, and 48% of the added menthol was encapsulated.

Example 8 Commercially available...100 g of illite ■ 5 m of glycerin
1, and then 2 g of the microcapsules obtained in Example 1 were sprinkled thereon and mixed.

Next, dry at 50°C for 5 minutes in a dryer, and after cooling, test 1
Using a trial hoist, the length is 70 mm and the circumference is 25.7 m.
A rolled-up menthol-containing tobacco product was obtained with the specifications of M.

This tobacco product had good aroma and menthol odor.

Example 9 Commercially available... Glycerin 5m in increments 10.1 for illite ■
1 g of microcapsules obtained in Example 7 after spraying
was sprinkled and mixed.

The obtained mixture was dried in a dryer at 50°C for 5 minutes, and after being left to cool, it was rolled up using a winding machine for test 1 to a length of 70711 rIL and a circumference of 25.7 mm to obtain a menthol-containing tobacco product. .

This tobacco product had good flavor and menthol odor.

[Brief explanation of the drawing]

FIG. 1 shows oral changes in menthol retention of microcapsules.

Claims (1)

[Scope of Claims] 1. A bead-shaped bead containing a fragrance, which is prepared by mixing an alkaline aqueous solution of a heat-coagulable polysaccharide mainly composed of β-1,3-glycosidic bonds and a fragrance, and bringing the mixture into contact with a gelling agent. gel. 2 Contains a bead-shaped gel containing a fragrance obtained by mixing an alkaline aqueous solution of a heat-coagulable polysaccharide mainly composed of β-1,3-glycosidic bonds and a fragrance, and contacting the mixture with a gelling agent. Tobacco products consisting of