JP3400543B2 - Powder fragrance and its manufacturing method - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a powdered perfume in which a base material containing calcium lactate contains a perfume, which can be widely used for the purpose of imparting an aroma to foods, cosmetics and the like, and a method for producing the same.

[0002]

2. Description of the Related Art Many attempts have been made so far to powder liquid perfumes. By pulverizing, it is possible to prevent the aroma component from being oxidized and volatilized to enhance the storability, and to simplify the handling. The conventional powdering methods are roughly classified as follows.

(1) Adsorption method: A method in which an appropriate amount of liquid flavor is added to powder such as lactose powder to adsorb it. (2) Spray drying method: A method in which a flavor is mechanically added to an aqueous solution of a constant concentration such as carbohydrate or protein to mechanically form an O / W type emulsion, and spray drying is performed. (3) Containment method: A method in which a flavor is mechanically contained in an amorphous substance in which sugar is boiled down. (4) Micelle formation method: A method of forming micelles with an aqueous solution of sugar and protein, solubilizing the perfume, and drying this. (5) Inclusion method: Cyclodextrin is dispersed in water,
A method in which a fragrance is added, stirred and included. (6) Others: A method of mixing and stirring a fragrance, a base material for inclusion of a fragrance, and a polyol (use of the method described in JP-A No. 64-27430).

[0004]

As described above, many powdering methods of perfume have been proposed in the past, but each has its advantages and disadvantages. For example, although the adsorption method (1) is a simple method, there is a limit to the ratio of the perfume adsorbed to the base material. Although the method of using the polyol of (6) is a method having a considerably high fragrance content ratio among the above methods,
The long-term storage causes the low boiling point substance to volatilize in the composition over time, and has a drawback that the scent and taste are changed. An object of the present invention is to obtain a powdered fragrance in which the fragrance content ratio is increased and volatile components, particularly low-boiling substances, are less volatile due to aging.

[0005]

In order to solve these problems, the present inventors have noticed that the solubility of calcium lactate in water increases significantly as the water temperature rises, and by utilizing this property, After adding water to the base material containing calcium lactate, heating and dissolving the calcium lactate, cooling to a temperature at which the perfume does not deteriorate, adding the perfume, and further cooling it, the calcium lactate that cannot be dissolved It has been found that the base material containing the perfume is precipitated and dried, and when it is dried, a powdered perfume capable of containing up to about 60% by weight of the base material is obtained. Further, in the case of a fragrance containing a low-boiling substance, this is heated in advance under reduced pressure to adsorb the low-boiling substance in the volatile fragrance to the powdery adsorbent, and the remaining low-boiling substance is removed. It was found that a powdered fragrance in which the volatilization of the low-boiling substance due to aging is further suppressed can be obtained by pulverizing the fragrance by the method described above and mixing it with the powder in which the low-boiling substance is adsorbed. completed.

That is, the present invention is as follows. 1. A powdered fragrance characterized by including 10 to 60% by weight of the total liquid fragrance in a base material containing 30 to 70% by weight of calcium lactate.

2. (1) 30-70 calcium lactate
Water is added to the base material containing 10 wt% and the mixture is heated to obtain a heating liquid in which calcium lactate is dissolved. (2) The heating liquid obtained in (1) is cooled to obtain this liquid. A step of adding 0.5 to 4 times the weight of liquid perfume to the base material to obtain a perfume-containing liquid, (3) further cooling the perfume-containing liquid obtained in (2),
A process for producing a powdered fragrance, comprising the steps of depositing a solid substance and then drying the solid substance without separating the solid substance to obtain a powdered fragrance.

3. (1) heating liquid perfume under reduced pressure,
A step of adsorbing a low-boiling substance in a perfume onto a powdery adsorbent to obtain a low-boiling substance-containing powder and a liquid perfume from which the low-boiling substance is removed, (2) A step of adding water to a base material containing 70% by weight and heating the mixture to obtain a heating liquid in which calcium lactate is dissolved. (3) Cooling the heating liquid obtained in (2), To
A step of adding a liquid perfume obtained by removing the low boiling point substance obtained in (1) in an amount of 0.5 to 4 times the weight of the base material to obtain a perfume-containing liquid, (4) in (3) Further cooling the obtained flavor-containing liquid,
A step of precipitating a solid substance and then drying the solid substance without separating the solid substance to obtain a flavor-containing powder; (5) The low-boiling substance-containing powder obtained in (1) and (4)
A process for producing a powdered fragrance, comprising the step of obtaining the powdered fragrance by mixing with the fragrance-containing powder obtained in (1).

The present invention will be described in detail below. In the present invention, calcium lactate is used as a base material for containing a perfume in an amount of about 30 to
A base material containing 70% by weight is used. When the content of calcium lactate in the base material is less than 30% by weight, there is a possibility that the solid deposition containing the perfume may not be desirably precipitated when the perfume-containing liquid is cooled. Also, a multi Kunar content of calcium lactate as a perfume inclusion for substrate exceeds 70 wt%,
The content ratio of the fragrance in the obtained powder fragrance is reduced, which is not preferable.

In the present invention, calcium lactate is usually pentahydrate. The component other than calcium lactate constituting the base material may be water-soluble or water-insoluble, but in order to easily confirm that calcium lactate was uniformly dissolved during heating. It is preferably water-soluble or one that dissolves when heated. Specific examples thereof include polysaccharides such as starch, dextrin, water-soluble cellulose, methyl cellulose and carboxymethyl cellulose and hydrolysates thereof, and derivatives thereof, sucrose, lactose, fructose, sugars such as glucose, guar gum and locust bean gum. Gums such as gum arabic, gum karaya, gum tragacanth and agar, mucilage polysaccharides such as carrageenan, alginate, chitin, chitosan, polyols such as glycerin, propylene glycol, pentaerythritol, glues such as gelatin, stearic acid Examples thereof include sodium and fatty acid salts such as sodium palmitate. One or two or more of these may be appropriately selected and used. Of these, polysaccharides and their hydrolyzates and saccharides are preferably used in the present invention. Further, those obtained by mixing agar and gelatin with these polysaccharides and sugars are also preferably used.

The amount of water added to the base material varies depending on the composition of the base material and the properties of the added perfume, but is not particularly limited as long as calcium lactate is uniformly dissolved during heating. However, the preferable amount is about 0.5 to 4 times, and particularly preferably about 1 to 2 times the weight of the substrate. If the amount of water added is too large, the step of drying afterwards becomes undesirably long.

The order of adding water is not particularly limited.
That is, it is possible to add calcium lactate and a base material other than calcium lactate in advance and then add water, or add water to a part of the base material and then add the remaining base material (for example, Alternatively, water may be added to a base material other than calcium lactate in advance, and then this may be heated in advance, and then calcium lactate is added).

The temperature at which the base material to which water is added is heated is not particularly limited as long as it is a temperature at which a heating liquid in which calcium lactate in the base material is uniformly dissolved can be obtained. If the calcium lactate in the base material is uniformly dissolved, no further heating is necessary. In the case where components other than calcium lactate constituting the base material are water-insoluble, or the amount of water is small even if water-soluble, the heating liquid in which calcium lactate is dissolved is an opaque liquid. Becomes

The heated liquid thus obtained is then cooled to a temperature at which the perfume does not deteriorate in order to add a perfume to this liquid to obtain a perfume-containing liquid (perfume-containing solution or perfume dispersion). The cooling temperature varies depending on the fragrance used, but specifically, it may be about 40 to 50 ° C. The amount of the fragrance added is about 0.5 to 4 times the weight of the base material.
If the amount is less than 0.5 times, the amount of the base material is too large, resulting in a bulky powder. Further, if the amount is more than 4 times, the amount of the fragrance not included in the base material increases, which is uneconomical.

As the fragrance used in the present invention, any of a hydrophobic fragrance, a hydrophilic fragrance (essence), a synthetic flavor, a natural extract, or a prepared fragrance in which these fragrances are combined can be used. . Perfumes for use in the present invention, Ru liquid der at room temperature. Further, other additives can be added as needed. As other additives, an emulsifier for uniformly dispersing the perfume in the base material, an antioxidant,
Examples include food dyes, nutritional substances, and the like.

The perfume-containing liquid obtained by adding the perfume is cooled with stirring, whereby the base material containing calcium lactate that cannot be dissolved becomes a solid (wet powder) including the perfume. Will start to precipitate. The cooling temperature is not particularly limited as long as such a perfume-containing base material is deposited as a solid, but in practice, it may be about 0 to 5 ° C. with ice water or the like.

By drying the obtained solid matter (wet powder), the desired fluid powdery fragrance can be obtained.
The drying method is not particularly limited, but it is necessary to avoid the condition that the perfume is deteriorated, and it is preferable to employ reduced pressure drying or air drying.

After drying, if necessary, sieving is performed. The average particle size of the powdered fragrance obtained by the present invention is about 0.1 to 5 mm. The proportion of the fragrance contained in the powder fragrance thus obtained can be freely changed depending on the amount of the fragrance to be added and the kind of the base material. Can be included.

Further, the powdered fragrance thus obtained was excellent in endurance for long-term storage because the fragrance component was less volatile due to aging. Furthermore, it was confirmed that when the obtained powdery flavor was added to warm water or hot water, it was quickly dissolved and the original flavor and taste were reproduced. Such properties are effectively utilized when added to foods and cosmetics.

When powdering a perfume having a low boiling point of about 40 ° C. or less, for example, a low-boiling substance such as dimethyl sulfide (boiling point, about 37 ° C.) and acetaldehyde (boiling point, about 20 ° C.), Is heated under reduced pressure, the volatile low-boiling substance is adsorbed on the powdery adsorbent to obtain a low-boiling substance-containing powder, while the remaining low-boiling substance-free perfume is pulverized by the method described above, This is achieved by mixing the two powders thus obtained. According to such a method, the original scent and taste without volatilization of the low-boiling point substance in the middle of the process, and further, the powdered fragrance in which the volatilization of the low-boiling point substance in the composition due to long-term storage is further suppressed. Obtainable.

The term "under reduced pressure" as used herein is preferably about 0.1.
-100 Torr, particularly preferably about 1-30 Torr
It is good to The heating temperature is not particularly limited as long as it is a temperature at which the low-boiling substance volatilizes under reduced pressure, but is preferably about 30 to 100 ° C, particularly about 30 to 60 ° C.

In order to adsorb the low-boiling substance to the powdery adsorbent, it is preferable to fill the container with the powdery adsorbent in advance and collect it in this container. The container is preferably cooled with a cryogen such as dry ice-acetone. As the powdery adsorbent, it is preferable to use a powder having a property of including or adsorbing organic compounds such as porous processed starch (crystal dextrin etc.), cyclodextrin and its derivatives, anhydrous calcium lactate etc. The amount used is not particularly limited, but is preferably the smallest amount capable of completely adsorbing the low boiling point substance, and it is uneconomical to use it in an excessively large amount, which is not preferable.

The powdered flavoring agent of the present invention thus obtained can be widely used for the purpose of imparting aroma to foods, cosmetics and the like.

[0024]

EXAMPLES Next, the present invention will be specifically described by way of examples, but the present invention is not limited to these.

[0025]

[0026]

[0027]

Example 1 To 2 g of calcium lactate pentahydrate (content of calcium lactate in base material 41.2% by weight) and 2 g of gum arabic, 8 g of water was added, and this mixture was heated to obtain a heating liquid. It was After cooling this liquid to 50 ° C., 4 g of steak flavor (Takasago Aroma Chemical Co., Ltd., hydrophobic liquid compounding aroma) was added (1.2 times the amount of the base material), and ice water was added with vigorous stirring. Was further cooled to 5 ° C. As it cooled, the mixture gradually thickened and a wet powder was obtained. This powder was air-dried overnight to obtain 7.0 g of the target powdery flavor.

The particle size of the obtained powdery fragrance is about 0.1.
It was 2 mm. Grind this powdered fragrance in a mortar and add diethyl
After extracting with ether, the content of steak flavor in the powdered flavor was measured by gas chromatography.
It was 5.8% by weight, and the yield based on the added steak flavor was 97.7%. 70% of this powdered fragrance
When poured into warm water at ℃, all dissolved within 3 minutes, releasing the aroma and taste of the original steak flavor. Further, the powdered flavor was stored in a closed container at 25 ° C. for 1 month, and no change in aroma and taste was observed.

[0029]

Comparative Example 1 An attempt was made to obtain a powdered fragrance from the method of the present invention by removing water and heating. That is, to a mixture of 2 g of calcium lactate pentahydrate and 2 g of lactose was added 4 g of ramen flavor (Takasago International Kogyo Co., Ltd., a hydrophobic liquid compounding fragrance) and stirred vigorously.
A slurry-like liquid was obtained, and no powder could be obtained.

[0030]

Comparative Example 2 An attempt was made to obtain a powdered flavor by the method of the present invention except that calcium lactate was not added. That is, 6 g of water was added to 4 g of lactose, dissolved by heating, cooled to 50 ° C., and then 4 g of the same ramen flavor as used in Comparative Example 1 was added, and ice water was used with vigorous stirring. And cooled to 5 ° C. As it cools,
The mixture gradually increased in viscosity and became a slurry-like liquid, but when stirring was further continued, the mixture separated into an oil layer and an aqueous layer, and powder could not be obtained.

[0031]

[Example 2] 4 g of ramen flavor (hydrophobic liquid fragrance manufactured by Takasago International Corporation) was heated under reduced pressure of 2 Torr at 50 ° C for 2 hours to volatilize low-boiling substances to give 2-hydroxy. 2 g of propyl-β-cyclodextrin (Nippon Shokuhin Kako Co., Ltd.) was filled and collected in a container cooled with dry ice-acetone to obtain a low boiling point substance-containing powder.

Separately, 6 g of water was added to a mixture of 2 g of calcium lactate pentahydrate (content of calcium lactate in the base material 41.2% by weight) and 2 g of lactose, and the mixture was heated to 60 ° C. to 70 ° C. The mixture was dissolved. After cooling this to 40 ° C., 3.8 g of ramen flavor (1.1 times the amount of the base material) from which the low-boiling substance remaining in the pretreatment was removed was added,
It was further cooled to 5 ° C. with vigorous stirring. As it cools, it becomes a damp mass, which becomes 2 Torr.
The mixture was dried under reduced pressure at 30 ° C. for 16 hours, and the solid obtained was lightly loosened to obtain 6.81 g of a free-flowing powder. To the powder, the low-boiling-point substance-containing powder obtained in the pretreatment was added to obtain 8.31 g of the target powder flavor.

The particle size of the obtained powdery fragrance is about 0.1.
It was 2 mm. Grind this powdered fragrance in a mortar and add diethyl
After extraction with ether, fragrance by gas chromatography
When the content rate was measured, the fragrance content rate was 39.3% by weight.
And the yield based on the ramen flavor used was 8
It was 1.5%. This powdered fragrance had the scent and taste of the original liquid ramen flavor, and when it was added to hot water at 70 ° C., it completely dissolved within 3 minutes and released the scent and taste of ramen flavor. In addition, this powdered fragrance,
No change in aroma and taste was observed by storing in a closed container at 25 ° C. for 1 month.

[0034]

According to the present invention, the fragrance content is high,
In addition, it is possible to provide a novel powdered fragrance in which the volatile components are less volatile, especially the low-boiling substances are less volatile.
Further, the ratio of the fragrance contained in the powder fragrance can be freely changed depending on the amount of the fragrance added and the type of the base material, and the fragrance can be contained in the base material at a maximum of about 60% by weight. Is.

─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP 42-5187 (JP, B1) JP 44-16358 (JP, B1) JP 44-30583 (JP, B1) JP 35- 2041 (JP, B1) (58) Fields surveyed (Int.Cl. ⁷ , DB name) A23L 1/22 A61K 7/46 A23F 3/40 A23F 5/46 JISST file (JOIS)

Claims (3)

(57) [Claims] 1. A powdered fragrance comprising a substrate containing 30 to 70% by weight of calcium lactate and 10 to 60% by weight of the total amount of liquid fragrance. 2. (1) Water is added to a base material containing 30 to 70% by weight of calcium lactate, and the mixture is heated,
A step of obtaining a heating liquid in which calcium lactate is dissolved, (2) cooling the heating liquid obtained in (1), and adding 0.5 to 4 times the liquid perfume to the base material in terms of weight. To obtain a fragrance-containing liquid, (3) further cool the fragrance-containing liquid obtained in (2),
A process for producing a powdered fragrance, comprising the steps of: depositing a solid product, and then drying the solid product without separating the solid product to obtain a powdered fragrance product. Wherein (1) the liquid perfume was heated under reduced pressure, the low boiling substance in the perfume adsorbed on powdered adsorbent, a liquid perfume low boiling substance-containing powder and the low-boiling materials is removed,
(2) a step of adding water to a base material containing 30 to 70% by weight of calcium lactate and heating this mixture to obtain a heating liquid in which calcium lactate is dissolved, (3) (2) Cool the heated liquid obtained in, and in this liquid,
A step of adding a liquid perfume obtained by removing the low boiling point substance obtained in (1) in an amount of 0.5 to 4 times the weight of the base material to obtain a perfume-containing liquid, (4) in (3) Further cooling the obtained flavor-containing liquid,
A step of precipitating a solid substance and then drying the solid substance without separating the solid substance to obtain a flavor-containing powder; (5) The low-boiling substance-containing powder obtained in (1) and (4)
A method for producing a powdered fragrance, comprising the step of mixing the powder containing the fragrance obtained in step 1 to obtain a powdered fragrance.