JP3342235B2 - Production method of water-soluble extract of animals and plants - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION The present invention is excellent in transparency stability which easily dissolves in water and / or ethanol and does not form insoluble matters such as sediments and precipitates for a long time after dissolution. Also, the present invention relates to a method for producing a water-soluble extract of animals and plants, which is excellent in stability and capable of maintaining a favorable balance of aroma and flavor satisfactorily over time. More specifically, the present invention provides an extract or a concentrate obtained by extracting an animal or plant material with an aqueous ethanol solution of 50% by weight or more, adding water to remove water-insoluble substances produced, and concentrating the resulting aqueous solution. A method for producing a water-soluble extract of animals and plants characterized by the fact that, when producing the extract, animal and plant materials, an extract or a concentrate thereof, an aqueous solution or a water-soluble extract of plants and animals, a polyhydric alcohol,
The present invention relates to a method for producing a water-soluble extract of animals and plants, to which at least one selected from a saccharide or a heated reactant thereof and a sugar-amino reactant (hereinafter, these may be referred to as “water-soluble retaining agent”) is added.

[0002]

2. Description of the Related Art As a method of collecting an active ingredient contained in animal and plant materials from the material, there are, for example, a solvent extraction method, a steam distillation method and a pressing method. The solvent extraction method is simple and has good extraction efficiency. Commonly used. For example, an animal or plant material such as amber, musk, vanilla, coffee, oris is brought into contact with an organic solvent such as ethanol to extract an active ingredient in the material. Condensed into a water-soluble resinous material is called a resinoid, oleoresin, or the like, and is often used as a flavor imparting agent for various foods or cosmetics.

However, when water and / or ethanol is added to a resinoid or oleoresin, for example, it initially dissolves and is transparent, but forms insoluble matters such as sediments and precipitates with the passage of time and becomes turbid. It lacks transparency stability, such as in a state, and this has the disadvantage of significantly reducing commercial value.

[0004] On the other hand, when an extract of animal or plant material is mixed with water or ethanol, essential oil, resin, tannin, pectin, viscous polysaccharide, etc., which have been dissolved in the extract, become insoluble and become opaque. It is well known to cause trouble. In order to prevent these troubles,
For example, tea leaves are preliminarily tannase or this and cellulase,
Extraction after treatment with a cell wall digestive enzyme such as pectinase (JP-B-52-42877, JP-B-62-151)
No. 75, JP-A-60-105454) or a method of obtaining a transparent and non-turbid tea by treating the tea extract with a filtration membrane on which tannase is fixed (Japanese Patent Laid-Open No. 2-128650). And the like) have been proposed.

[0005] However, the conventionally proposed method of obtaining a transparent and non-turbid tea by enzymatic treatment of tea leaves and tea extract has a complicated enzymatic treatment operation, and as the time elapses, precipitates and sediments are removed. Occasionally, generation was observed and the transparency stability was not always fully satisfactory.

[0006]

Resinoids and oleoresins can be easily produced by a solvent extraction method and are useful as flavoring agents, but have the disadvantages described above. There are many restrictions in application or utilization. Therefore, there is a strong demand for the development of a water-soluble extract of animals and plants which is completely dissolved in water and / or ethanol and has excellent transparency stability over time.

[0007]

Means for Solving the Problems The present inventors have intensively studied to solve the above-mentioned drawbacks or restrictions. As a result, water is added to an extract or a concentrate thereof, which is obtained by subjecting animal or plant material to extraction with an aqueous solution of 50% by weight or more of ethanol, removes water-insoluble substances generated, and concentrates the obtained aqueous solution. Animal and plant water-soluble extracts
It has been found that it is completely dissolved in water and / or ethanol and has excellent transparency stability over time. Further research has shown that, in the manufacture of the extract, animal and plant materials, extracts or concentrates thereof, aqueous solutions or water-soluble extracts of plants and animals are selected from polyhydric alcohols, saccharides or their heat reactants and sugar / amino reactants. The water-soluble extract of animals and plants produced by adding at least one kind exhibits extremely excellent transparency stability, and stably maintains a preferable balance of aroma and flavor over a long period of time, and solves the conventional problems at once. The present invention was found to be extremely useful as a fragrance and flavor imparting agent that can be used to complete the present invention.

Thus, the present invention provides an extract or a concentrate thereof obtained by subjecting an animal or plant material to an extraction with an aqueous solution of 50% by weight or more of ethanol, adding water to the resulting extract to remove water-insoluble matters, and removing the resulting aqueous solution. It is intended to provide a method for producing a water-soluble extract of animals and plants characterized by concentration.

[0009] The present invention also relates to a method for producing the extract, wherein an animal or plant material, an extract or a concentrate thereof, an aqueous solution or a water or plant water-soluble extract is added to a polyhydric alcohol, a saccharide or a heat-reacted product or a sugar-amino reactant thereof. It is intended to provide a method for producing a water-soluble extract of animals and plants, characterized by adding at least one selected from the group.

Hereinafter, the present invention will be described in more detail.

The animal material which can be used as a raw material in the present invention includes, for example, marine animals such as livestock meat, eggs, fish, crustaceans, poultry meat, processed foods thereof, and dairy products. Examples of plant materials include vanilla, coffee, cocoa, teas, spices, herbs, vegetables, fruits, seaweeds, nuts, cereals, and tobacco leaves such as yellow seeds.

The concentration of ethanol in an aqueous ethanol solution used as an extraction solvent in the extraction treatment of these animal and plant materials is 50% by weight or more, more preferably 80% by weight.
That is all. When an ethanol aqueous solution having an ethanol content of less than 50% by weight is used, the extract obtained is dissolved only in water or a low-concentration ethanol solution, and a high-concentration ethanol solution has disadvantages such as formation of a precipitate or a precipitate.

The method of preparing the extract by treating the above animal or plant material with an aqueous solution of 50% by weight or more of ethanol is not particularly limited, and any conventionally known extraction method can be employed. For example, about 2 to about 20 parts by weight of an aqueous ethanol solution is added to 1 part by weight of animal and plant material, and about 0 to about 100 parts by weight.
At 30 ° C. for about 30 minutes to about 24 hours under a stirring or standing condition. After the contact treatment is completed, solid-liquid separation is performed by ordinary separation means, for example, decantation, and the separated liquid is filtered, if necessary. The extract can be easily collected by filtration.

Next, water is added to the extract obtained as described above to remove water-insoluble substances formed, so that the extract is soluble in water and / or ethanol and shows a transparent stability for a long period of time. An animal or plant water-soluble extract can be produced.
In this step, water may be added to the extract itself,
Alternatively, the extract may be added to an extract concentrate obtained by partially or completely distilling off ethanol by distillation or distillation under reduced pressure. The method for preparing an extract concentrate by removing ethanol from the extract is preferably carried out under reduced pressure without heat. For example, the degree of reduced pressure is about 50 to about 360.
mmHg and a distillation temperature in the range of about 20 to about 60 ° C. can be exemplified.

In the case where water is added to the extract or its concentrate, if the amount of water is too small, the removal of water-insoluble matter becomes insufficient and causes formation of sediments and precipitates. Alternatively, it is desirable to add water so that the ethanol concentration of the concentrate becomes 40% by weight or less, more preferably 20% by weight or less. As the amount of water satisfying such conditions, for example, when added to the extract, about 0.1 to about 5 parts by weight of water per 1 part by weight of the extract,
More preferably, the amount can be in the range of about 0.3 to about 3 parts by weight. On the other hand, the amount of water to be added to the extract concentrate varies depending on the degree of concentration. The range of about 0.3 to about 4 parts by weight based on parts by weight can be exemplified.

When water is added to the extract or extract concentrate,
Until then, components that were dissolved in the extract or extract concentrate,
It precipitates as insoluble matter such as a precipitate or a precipitate. These insolubles dissolve in a high-concentration aqueous ethanol solution of about 50% by weight or more, but are insoluble or hardly soluble in a low-concentration aqueous ethanol solution of about 40% by weight or less. These components include, for example, essential oils, resinous materials, tannin materials, pectin materials, and the like contained in various animal and plant materials. As a means for removing these water-insolubles generated by adding water, for example, a commonly used filtration method can be adopted. At this time, in order to improve the efficiency of removing water-insolubles, Diafloc is used. It is preferable to perform filtration by adding a filter aid such as diatomaceous earth.

By recovering ethanol and / or water from the aqueous solution thus obtained, a water-soluble extract of animals and plants having excellent transparency stability can be produced. As the recovery means, for example, a vacuum recovery method which is usually performed can be employed. At this time, the degree of reduced pressure is, for example, about 30 to about 50 mmHg, and the distillation temperature is, for example, about 20 to about 60 ° C. A degree condition can be employed. The concentrate obtained in this manner can be used as it is as the water-soluble extract of the present invention. However, usually, the concentrate is added to a concentration of about 0 to about 5 to promote the formation of a precipitate or a precipitate. C., a membrane filtration method using a microfiltration (MF) membrane, etc., and a treatment with an enzyme such as tannase, pectinase, cellulase, hemicellulase to decompose tannin, pectin and viscous polysaccharide. Is preferred.

In another aspect of the present invention, in any step of producing the above-mentioned water-soluble extract of animals and plants, a water-soluble preservative is added, solubilized in water or ethanol, and preferable for a long period of time. Maintain the balance of aroma and flavor,
Further, it is possible to produce a water-soluble extract of animals and plants excellent in transparency stability, which can impart a mild and excellent fragrance and persistence.

The water-soluble retaining agent used in this embodiment can be directly added to animal and plant materials, and can also be added in any production process. For example, it can be extracted with an aqueous ethanol solution in the presence of a raw material of animal and plant material and a water-soluble preservative, or can be an extract, an extract concentrate, an aqueous solution obtained in the production process, or a water- or animal- or plant- or animal-plant extract finally obtained. A water-soluble retention agent may be added to the mixture.

As the water-soluble retaining agent, polyhydric alcohols,
Saccharides, their heat reactants, and sugar / amino reactants can be mentioned. Examples of the polyhydric alcohol include propylene glycol, glycerin, sorbitol, mannitol and the like. Further, as the saccharide, for example, sugar, glucose, fructose, invert sugar, isomerized sugar, starch syrup, honey, molasses, maple sugar, coconut sugar, and an aqueous solution (liquid sugar) thereof can be used. Examples of the reactant include, for example, the above-mentioned heated reactants of saccharides, which are usually called caramel. Further, examples of the sugar-amino reactant include a heat-reacted product of an amino acid such as glycine, alanine, glutamic acid, arginine, proline, valine, leucine and the above-mentioned saccharide.

The amount of the water-soluble retaining agent to be added depends on the animal and plant material, the extract, the aqueous solution or the concentration of these liquids, and can be selected as appropriate. The amount of the water-soluble retention agent can be exemplified in the range of about 0.01 to about 20 parts by weight, more preferably about 0.1 to about 4 parts by weight .

The water-soluble extract of animals and plants obtained in this manner is completely dissolved in water or ethanol, and even after a long period of time, it does not produce insoluble matters such as sediments and precipitates, and has a transparent stability. It has many excellent features such as being able to maintain an excellent and preferable balance of flavor and flavor over time, and to impart mild and excellent flavor and flavor. The water-soluble extract of animals and plants of the present invention can be used by being added to the flavor-imparting composition of various products, and the amount of addition varies depending on the purpose of use or the type of the flavor-imparting composition. Can be exemplified in the range of about 0.01 to about 80% by weight based on the total amount of the flavor and flavor imparting composition.

Thus, according to the present invention, it is possible to provide a flavor-imparting composition comprising a water-soluble extract of animals and plants as an active ingredient, and to use the composition to produce foods and beverages, cosmetics, and the like.
The aroma and flavor of the water-soluble extract, which is characteristic for health, hygiene, pharmaceuticals, etc., can be imparted.

For example, drinks such as fruit juice drinks, fruit liquors, milk drinks, carbonated drinks; ice creams, sorbets, cold desserts such as popsicles; Japanese / Western sweets, jams, chewing gums, breads Luxury items such as coffee, cocoa, tea, tea, tobacco;
Soups such as Japanese-style soups and Western-style soups; foods and beverages obtained by adding an appropriate amount of an animal or plant water-soluble extract capable of imparting its unique aroma to a flavor seasoning, various instant beverages or foods, various snack foods, etc. Can be provided. Also, for example, shampoos, hair creams, pomades, and other hair cosmetic bases;
Cosmetics can be provided in which an appropriate amount of an animal or plant water-soluble extract capable of imparting its unique fragrance is added to oscilloscope, lipstick, other cosmetic bases, cosmetic detergent bases, and the like. Furthermore, the water-soluble extract of animals and plants of the present invention is added to laundry detergents, disinfectant detergents, room air fresheners and other various health and hygiene materials; flavors and flavoring agents for facilitating the taking of pharmaceuticals. Health, hygiene and medicines can be provided.

Hereinafter, embodiments of the present invention will be described more specifically with reference to Comparative Examples and Examples.

[0026]

【Example】

Example 1 600 g of vanilla beans cut to about 1 cm in a flask, 9
2700 g of 5% ethanol and 300 g of water are charged and extracted while stirring at a temperature of 70 to 75 ° C. for 2 hours in a flask. After completion of the extraction, the mixture is cooled to about 30 ° C. or lower and left overnight. The separated solution obtained by decantation is filtered through a filter paper to obtain 2897 g of a filtrate. 1200 g of propylene glycol (2 times the amount of vanilla beans) is added and dissolved in the obtained filtrate. This solution was subjected to a pressure reduction of 120 mmHg, 65 to 70
The primary concentrate 1362 was distilled under reduced pressure at a temperature of about 2 ° C. for about 2 hours.
g was obtained. To this concentrate, 2724 g of soft water (2 times the amount of the concentrate) was added, and at room temperature, in order to remove the generated water-insoluble matter,
Filter in the presence of a filter aid (diafloc: diatomaceous earth = 1: 1). The obtained filtrate was concentrated under reduced pressure (bath temperature: about 60 ° C., degree of reduced pressure: 40 to 50 mmHg) to obtain 1,198 g of red-brown and transparent final concentrate [sugar content (Bx) 59.2]. The concentrate was filtered through a Saran cloth filter-filler of 80 mesh to obtain 1180 g of the vanilla oleoresin of the present invention.
Was obtained (Product No. 1 of the present invention). Yield: 197% (based on vanilla beans) Specific gravity (20 ° C): 1.0719 Refractive index (20 ° C): 1.4398

Comparative Example 1 A vanilla oleoresin was produced under the same conditions as in Example 1 except that the step of adding and dissolving propylene glycol to the filtrate and the step of adding soft water to the concentrate were omitted. (Comparative product No. 1).

Example 2 300 g of a dried bonito grinder powder (G powder) in a flask, 95 g
Then, 1080 g of ethanol and 120 g of water are charged, and the mixture is extracted with stirring at a temperature of 78 to 82 ° C. for 2 hours in a flask. After completion of the extraction, the mixture was cooled to about 40 ° C. or lower, and 1036 g of the separated solution obtained by centrifugation was filtered through a filter paper to obtain a filtrate 1025 g.
g. The obtained filtrate has a reduced pressure of 170 mmHg to 4 mm.
Concentrate at 0 mmHg, 40-50 ° C. temperature to obtain 150 g concentrate. 600 g of water (4 times the amount of the concentrate) is added to the concentrate, and sterilization and dissolution are performed at 88 ° C to 92 ° C, 15 ° C.
And stir in a refrigerator at 0-5 ° C overnight. In order to remove the generated water-insoluble matter, the mixture was filtered in a refrigerator at the same temperature in the presence of a filter aid (diafloc: diatomaceous earth = 1: 2), and 732 g (refractive index n ²⁰ _D 1.3418) of the filtrate was filtered. obtain. The filtrate was concentrated under reduced pressure (bath temperature about 50 ° C., degree of vacuum 50 mmHg) to give a dark brown, almost transparent final concentrate 49.
g (Bx19.5) was obtained (Product No. 2 of the present invention). Yield: 16% (based on G powder)

Comparative Example 2 In Example 2, the extraction solvent was 95% ethanol 720
gatsuobushi extract was produced under the same conditions as in Example 2 except that g and water were replaced by 1680 g (Comparative Product No. 2).

Example 3 3.0 k of cocoa powder (10-12% fat) was added to an extraction kettle.
g, 15.75 kg of 95% ethanol and 6.75 k of water
g, and extraction is performed while stirring at an internal temperature of 50 to 55 ° C. for 1 hour. After completion of the extraction, the mixture is cooled to about 30 ° C. or lower, and subjected to suction filtration in the presence of a filter aid (Diafloc) to give a filtrate.
43 kg were obtained. The filtrate has a reduced pressure of 170 mmHg or more.
40 mmHg, concentrated at a temperature of 45 to 55 ° C.,
g of concentrate are obtained. An equal amount of water was added to the concentrate, and the mixture was stirred and dissolved at room temperature for 60 minutes.
Min.) To obtain 2.6 kg of supernatant (Bx13.1). The supernatant is a rotary evaporator (bath temperature about 6
The mixture was concentrated at 0 ° C. under a reduced pressure of 45 mmHg to obtain 440 g of a concentrate (Bx70). 704 g of glycerin in this concentrate
(1.4 times the amount of the concentrate), 264 g of molasses (0% of the concentrate.
6 times) and stirred and mixed at room temperature for 30 minutes.
After sterilizing at 15 ° C. for 15 minutes, the mixture was cooled to 70 ° C., and hot-filled while filtering through a 60-mesh wire mesh (Product No. 3 of the present invention). Yield: 46% (based on cocoa powder) Moisture (K · F method): 19.4% Specific gravity (20 ° C.): 1.2833 Refractive index (20 ° C.): 1.4698

Comparative Example 3 In Example 3, the extraction solvent was 9 kg of 95% ethanol.
A cocoa oleoresin was produced under the same conditions as in Example 3 except that glycerin and molasses were not used in place of water and 21 kg of water (comparative product No. 3).

Example 4 Chamomile (German) Fine Cut 1 was added to a flask.
Then, 00 g, 825 g of 95% ethanol and 675 g of water are charged, and the mixture is extracted with stirring at a temperature of 34 to 36 ° C. for 2 hours in a flask. After completion of the extraction, the mixture was subjected to suction filtration in the presence of a filter aid (diafloc) to obtain 1323 g of a filtrate.
2646 g of water (twice the amount of the filtrate) was added to the filtrate, and the mixture was stirred and dissolved at room temperature for 60 minutes. This was subjected to suction filtration in the presence of a filter aid (diafloc: diatomaceous earth = 1: 1) to obtain 3770 g of a filtrate. This is rotary evaporator (bath temperature 50-60 ° C), decompression degree 40-4
The mixture was concentrated at 5 mmHg to obtain 22 g of a concentrate (Bx70). Further, after sterilization at 90 to 95 ° C. for 15 minutes, the mixture was cooled to 70 ° C., and hot-filled (filling amount: 17 g) at the same temperature while filtering through a 60-mesh wire mesh (product No. 4 of the present invention). Yield: 17% (vs. chamomile) Bx (20 ° C.): 70.1

Comparative Example 4 In Example 4, the extraction solvent was 95% ethanol 540.
A chamomile extract was produced under the same conditions as in Example 4 except that g and water were replaced by 1260 g (Comparative Product No. 4).

Example 5 600 g of vanilla beans cut into columns of about 1 cm, 95 g
5100 g of ethanol and 900 g of water were charged, and extraction was continued for 6 hours while circulating the extract at a temperature of 28 to 30 ° C. in the column at a flow rate of 50 ml / min. After the extraction,
Liquid separation (seed extraction residue is separated by filtration with bleached cloth)
8 g were obtained. The separated liquid was concentrated at a bath temperature of 58 to 62 ° C and a degree of reduced pressure of 120 to 140 mmHg to obtain 375 g of a concentrate. To this concentrate, 1425 g of water (adjusted water so that the total amount of the concentrate and water to be added becomes 1800 g) was added, and the mixture was stirred at room temperature for 30 minutes and allowed to stand for 60 minutes to sufficiently perform separation. . Filter aid (diafloc: diatomaceous earth =
Suction filtration was performed in the presence of 1: 1), and 1725 g (Bx
6.9) was obtained. Using a rotary evaporator, the bath temperature is 55 to 60 ° C, the pressure is reduced from normal pressure to 30 mmHg.
Under the conditions described above, until the solvent is no longer distilled off,
36 g of viscous vanilla oleoresin was obtained (Product No. of the present invention)
5). Yield: 6.0% (based on vanilla beans)

Example 6 Example 1 (product No. 1 of the present invention) to Example 5 (product No. 5 of the present invention) and Comparative Example 1 (comparative product No. 1) to Comparative Example 4
A perfume-transparency stability test was performed on various water-soluble extracts of animals and plants obtained in (Comparative Product No. 4), and the results are shown in Table 1. In addition, the fragrance transparency stability test was Brix1
No. 1 of the present invention to No. 1 of the present invention N in sugar solution of 2 ゜, pH 3.0
o5 and comparative product No1 to comparative product No4 are each 0.1
%, And stored at room temperature after sterilization.

Table 1: Perfume Transparency Stability Test Storage days 1 month 3 months 6 months 1 year Invention product No1----Invention product No2-± ± ± Invention product No3--± ± Invention product No4 − − − ± Product of the present invention No. 5 − − ± ± Comparative product No. 1 + + + + + + + + Comparative product No. 2 + + + + + + + + + + + + Comparative product No. 3 + + + + + + + + + + + Comparative product No. 4 + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + Meaningful. -No formation of insolubles (sediments, precipitates). ± Slight formation of insolubles (sediment, precipitate) was observed. + Insoluble matter (sediment, precipitate) is observed. ++ A lot of insoluble matter (sediment, precipitate) is observed. +++ The formation of insolubles (sediment, precipitate) is remarkably observed.

As is evident from the results in Table 1, no insoluble matter was found even after one year, and all of the products of the present invention showed extremely excellent transparency stability. On the other hand, many of the comparative products do not dissolve transparently when prepared for the dissolution test, and also generate many insolubles over time, resulting in extremely poor transparency stability.

[0038]

According to the present invention, water is added to an extract or a concentrate obtained by extracting animal and plant materials with an aqueous ethanol solution of 50% by weight or more to remove water-insoluble substances produced. It is easily dissolved in water and / or ethanol by a simple means of concentrating the resulting aqueous solution, and has excellent transparency stability without producing insoluble matter such as sediments and precipitates for a long time after dissolution. And water-soluble extracts of animals and plants.

────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tsutomu Saga 335 Kariyuku, Nakahara-ku, Kawasaki-shi, Kanagawa Hasegawa Perfume Co., Ltd. (56) References JP-A-3-98566 (JP, A) JP-A-5-98 95764 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) A23L 1/221 A23G 1/00

Claims (1)

(57) [Claims] 1. A water was added to the extract or concentrate thereof vanilla beans were harvested by extraction with 50% or more by weight of ethanol aqueous solution to remove the resulting water insoluble material and concentration of the resulting aqueous solution A method for producing a water-soluble extract of vanilla beans.
The extract or concentrate, aqueous solution or vanilla bean water
Soluble extract, polyhydric alcohol, sugar or its heat reaction
Or at least one selected from sugar and amino reactants
A method for producing a water-soluble vanilla bean extract, comprising adding water.