JP2003284523A - Processed product of leaf of magnolia obovata thunb. and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a technique of a method for producing a processed product of a leaf of Magnolia obovata Thunb. containing active ingredients from the leaf of the Magnolia obovata Thunb. and, on the other hand, with suppressed bitterness, etc. <P>SOLUTION: The method for producing the processed product of the leaf of the Magnolia obovata Thunb. comprises a step of drying the raw leaf of the Magnolia obovata Thunb., a first roasting step of roasting the leaf after the drying at ≥100 and ≤150°C and a second roasting step of roasting the leaf passing through the first roasting step at ≥180 and ≤250°C. A tea leaf of the Magnolia obovata Thunb. can be obtained by carrying out the steps. The resultant tea leaf has reduced bitterness components and a flavor and the active ingredients. <P>COPYRIGHT: (C)2004,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a technique of using honoki leaves (hereinafter referred to as hoo leaves) as tea leaves or extracts, and in particular, it is provided with an active ingredient and, at the same time, bitterness and taste without losing flavor and umami. The present invention relates to a technique for producing processed tea leaves or foods having taste and utility, which are suitable for eating, drinking, oral administration, external use, nutritional supplementation, etc.

[0002]

2. Description of the Related Art Honoki is also known as the Hohogiwa tree,
The bark of the honoki is mixed with home remedies such as astringent, diuretic, expectorant, etc. It is blended in. In addition, for honoki bark, lignans such as magnolol (1.0 to 2.5%) and honokiol (0.1 to 0.5%), terpene essential oils such as udesmol, and alkaloids such as magnoclaline. Contains the component (0.007%). It is also reported that these various components have sedative, anticonvulsant, and central muscle relaxant effects. The flower contains the flavonol glycoside rutin. Since the long axis of the honoki is 30 cm long and the leaves are large and have a good scent, it has been used as a container for steaming rice balls, miso and living things. Japanese Patent No. 2886523 discloses:
It is disclosed that magnolol, honokiol and the like have a cancer metastasis inhibitory action.

On the other hand, generally, as a technique for processing plant leaves into foods, it is known to use tea leaves and various preparations or foods including extracted extracts. In formulating, it is particularly necessary to consider the stability of the active ingredient, masking of bitter substances and the like. Examples of the technique for such formulation include (inclusion method with cyclodextrin, enzymatic decomposition masking method, etc., Japanese Patent Nos. 2717509-11, 2705787, and Japanese Patent Publication No.
-9335, 6-316537, 7-252150, 8
No. -245350, Tokuyo Hyo 6-501027, Tokuhei 5
There is a technique disclosed in No. 176739.

[0004]

Ingredients such as magnolol and honokiol are also contained in hoo leaves. Wheat leaves have the advantage of being easy to collect. Therefore, it is desired to process the holly leaf so that it can be eaten and drinked. However, since the peduncle and veins of the holly leaf contain alkaloid components such as udesmol and magnoclarine that have paralytic and curare-like toxic effects in the petiole and vein of the bark in a small amount, conventional food packaging containers Although it was used as, it was not used as food. Therefore, when used for food and drink, it is necessary to remove these alkaloid components. In addition, holly leaf has a strong bitterness and astringent taste, and these taste substances generally have physicochemical instability, strong hygroscopicity, strong scattering property, strong adhesiveness, etc. Is becoming a factor that makes it difficult to realize. The phoenix leaf extract obtained by removing the alkaloid substances according to a conventional method has a strong bitterness and contains a large amount of bitterness-tasting substances. For this reason, there are various restrictions on the processing of holly leaf extract into granules and tablets, and bitterness remains even after masking, and it is not possible to obtain favorable palatability. For these reasons, it has heretofore been virtually impossible to produce processed foods such as holly leaf. Furthermore, the holly leaf extract obtained according to the conventional method also contains a large amount of pigment substances, and since such pigment substances have high solubility, even if masked, the oral cavity and the root part are colored when taken orally. There was a problem such as. On the other hand, these bitter substances and pigment-based substances are often active ingredients having some physiological activity, and it is necessary to avoid treatment or operation that excessively removes or decomposes them.

Therefore, it is an object of the present invention to provide a technique for producing a processed holly leaf product containing an active ingredient from holly leaf and having a reduced bitterness component and the like.

[0006]

In order to solve the above-mentioned problems, the inventors of the present invention have investigated various techniques capable of reducing or removing bitterness and astringent taste. It was found that the above-mentioned problems can be solved by carrying out the heating and roasting process described in 1. and completed the present invention. Furthermore, the present inventors have found that the extract can be obtained from the tea leaf material after the heating and roasting step, and by masking the extract with a predetermined composition, it is possible to improve the palatability while securing the elution property, The present invention has been completed. That is, according to the present invention, the following means are provided.

(1) A method for producing a processed product of honoki, which comprises the steps of drying fresh leaves of honoki and roasting the dried leaves. (2) The roasting step includes a first roasting step in a first temperature range and a second roasting step in a second temperature range higher than the first temperature range, (1 ) The method described. (3) The method according to (2), wherein the first roasting step is a step of mainly removing body water. (4) The method according to (2) or (3), wherein the first temperature range is 100 ° C. or higher and 150 ° C. or lower, and the second temperature range is 180 ° C. or higher and 250 ° C. or lower. (5) The method according to any one of (2) to (4), wherein the second roasting step is continuously performed after the first roasting step. (6) The method according to any one of (1) to (5), wherein the drying step is performed at 80 ° C. or higher and 110 ° C. or lower. (7) The method according to any one of (2) to (6), wherein the first temperature range is 100 ° C. or higher and 135 ° C. or lower. (8) The method according to any one of (2) to (7), wherein the second temperature range is 180 ° C. or higher and 200 ° C. or lower ₅ . (9) Tea leaves that are honoki tea leaves, which are obtained by roasting dried honoki leaves. (10) The tea leaf according to (9), which is obtained by roasting at a temperature of 100 ° C to 150 ° C and then roasting at a temperature of 180 ° C to 250 ° C. (11) A honoki tea leaf containing magnolol, wherein the alkaloid component content is 0.01 wt% or less. (12) 0.002 wt% or more of magnolol 0.0
The tea leaf according to (11), which contains 90 wt% or less. (13) The honoki tea leaf according to any one of (9) to (12), and green tea leaf, persimmon leaf, peach leaf, ginkgo leaf, shakuchu leaf, dokudami leaf, pigeon wheat, mandarin orange peel, akebi no vine, mulberry Leaves, Jerusalem artichoke, Salacia, taranome, agarix, Phellinus linteus,
A tea leaf composition, comprising one or more teas selected from the group consisting of Ganoderma lucidum, ginseng and its leaves, and field seven carrots and its leaves. (14) A honoki leaf extract, which is (9) to (12)
An extract obtained by extracting the tea leaves of honoki according to any one of 1 to 3 above with water and / or a hydrophilic organic solvent. (15) An extract of honoki, which has a magnolol content of 1 wt% or more and an alkaloid component content of 0.01 wt% or less. (16) A method for producing a honoki leaf extract composition, comprising:
Step of drying fresh leaves of honoki and 10 leaves after drying
The first roasting step of roasting at a temperature of 0 ° C. or higher and 150 ° C. or lower, and the leaves that have undergone the first roasting step are 180 ° C. or higher and 250 ° C.
A second roasting step of roasting at the temperature below, a step of extracting leaves with water and / or a hydrophilic organic solvent after the second roasting step to obtain an extract, and the obtained extract And supplying a masking agent and mixing, and granulating the mixture. (17) The method according to (16), wherein the masking agent is one or more selected from the group consisting of cyclodextrin, dextrin, silicon dioxide, anhydrous saccharides, methylcellulose and shellac. (18) 100 parts by weight of the honoki leaf extract according to (14) or (15), and 200 parts by weight or more of a masking agent 40
A honoki leaf component-containing composition, which comprises 0 part by weight or less. (19) The composition according to (18), wherein the masking agent is one or more selected from the group consisting of cyclodextrin, dextrin, silicon dioxide, anhydrous saccharide, methylcellulose and shellac. (20) The composition according to (18) or (19), which further contains the honoki tea leaf according to any one of (9) to (12).

According to these inventions, by carrying out the above-mentioned roasting step, it is possible to effectively reduce or remove the components exhibiting bitterness or acrid taste. Therefore, it is possible to suppress the inactivation or removal of the active ingredient derived from pea leaf and at the same time to obtain a processed product suitable for eating and drinking or external use.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described in detail below. The method for producing a processed holly leaf product of the present invention includes a step of roasting dried hollyhock leaves. Preferably, the roasting step includes a first roasting step in the first temperature range and a second roasting step in the second temperature range higher than the first temperature range. The primary processed product (roasted holly leaf) obtained by these steps is typically honoki tea leaf. Furthermore, from this tea leaf, it is possible to obtain a hoo leaf extract as a secondary processed product according to a conventional method. Further, the processed hoo leaf product of the present invention is a tea leaf obtained by roasting dried hoo leaves, and preferably 10
Roast at a temperature between 0 ° C and 150 ° C, then 180 ° C
Tea leaves obtained by roasting at a temperature of 250 ° C. or higher, or magnolol, containing alkaloid components,
It contains tea leaves of 0.01 wt% or less. Furthermore, the extract of the present invention is a hoo leaf extract extracted by a conventional method from the processed product (tea leaf as a primary processed product) obtained by these steps. Further, the extract composition of the present invention can take the form of a granular agent containing the extract and a masking agent in a predetermined composition, in addition to the form containing the peach leaf extract. Furthermore, the composition of the present invention can take a form containing tea leaves together with the extract and / or the extract-containing masking granule. Further, the tea leaf composition of the present invention may contain various kinds of tea leaves in addition to hoha leaf tea leaves.

(Phoenix leaf) The phoenix leaf used in the present invention is the leaf of Magnolia obovata, which is a magnolia family plant. Homologs of peach leaves can also be used in the present invention in the same manner as peach leaves. The holly leaf homolog means a leaf containing one or two of magnolol and honokiol. Of the magnoliaceae plants, preferred are plants belonging to the same genus as honoki or leaves of related species. For example, calla hoo (Ma
gnolia officinalis) and its variants (Magnolia
officinalis var. biloba, ibid.).

[0011] Although the whole holly leaf can be used uniformly, it can also be used by separating it into a petiole and a mesophyll and appropriately mixing them. Usually, the petiole contains more components than the mesophyll that exhibit the bitterness and astringency, and the mesophyll contains a sweet scent component. Therefore, it is possible to change the palatability of the tea leaves or the extract by appropriately changing the composition thereof as needed. For example, when the mesophyll: petiole (weight ratio) is in the range of 9: 1 to 5: 5, tea leaves having a well-balanced flavor and sweetness can be obtained. When the weight ratio of petioles exceeds mesophyll, bitterness and astringent taste tend to be stronger. Preferably, the weight ratio of mesophyll: petiole is 9: 1.
~ 6: 4.

(Drying Step) In the present invention, first, it is preferable to dry the collected raw phoenix leaves. By pre-drying, the roasting step to be performed later can be effectively performed in a short time. The desired dry state in the drying step is, for example, when the water content is 5-10.
% Or less (weight loss on drying (105 ° C., 6 hours)), or as a touch, to the extent that it can be rubbed with a hand in a crispy state or slightly moistened. In addition, as the drying progressed, the peach leaves had green, gray green, greenish brown,
Although the color changes to grayish brown, brown, or dark brown, the desired dry state can be obtained by drying to a coloration state of approximately green brown or more. More preferably, it is gray brown or more. The drying method can be carried out by a conventional method such as drying in the shade, aeration drying, or heat drying, but heat drying is preferable. By heat drying, at the same time,
It can inactivate the enzyme in peach leaves and prevent the subsequent change in the composition of leaves.

In the heating and drying step, it is preferable to dry the peach leaves to a desired dry state in the range of 45 ° C. or higher and 150 ° C. or lower. The time required varies depending on the state of the hoo leaves used for the drying step, but when fresh leaves are dried, at least 2 hours, preferably 4 hours or more and 10 hours or less,
More preferably, it is 4 hours or more and 8 hours or less. Also,
The temperature is preferably 110 ° C. or lower, more preferably 80 ° or higher and 110 ° C. or lower. 80 ° C or higher 110
When the temperature is not higher than 0 ° C, a substantially sufficient dried state can be obtained in 4 to 8 hours. If it is lower than 80 ° C, the drying time tends to be too long, and if it exceeds 110 ° C, the risk of decomposition of the active ingredient increases. In addition, it is preferable that the drying step is performed in a state in which the overall shape of the pea leaves is roughly maintained.

(Roasting Step) The roasting step is a step of roasting dried hoo leaves in a short time. The roasting step preferably includes a roasting step in the first temperature range and a roasting step in the second temperature range. The roasting step is preferably performed on shredded dried hoo leaves. The hoo leaves can be shredded after the drying step by hand or mechanically loosening, or they may be shredded before the drying step. The size of the fine pieces is not particularly limited, but is preferably about 5 mm square.

The roasting step can be carried out continuously after the drying step. For example, the roasting step can be performed while the heat supplied to the peach leaves in the drying step remains. Moreover, the thing after cooling, such as what was once preserve | saved in the humidity-controlled atmosphere, can also be used for a roasting process.

The first temperature range is preferably 100 ° C. or higher and 150 ° C. or lower. In this temperature range, it is possible to effectively evaporate the internal water content (also referred to as body water) remaining in the peach leaves after the drying step. This is because if the temperature is lower than 100 ° C., evaporation of bound water is not promoted.
More preferably, it is 100 ° C. or higher and 135 ° C. or lower. Further, from the viewpoint of quickly evaporating the bound water in a short time, it is preferable that the time is several minutes to a dozen minutes at the longest,
It is more preferably 2 minutes or more and 10 minutes or less, and further preferably 3 minutes or more and 5 minutes or less.

The second temperature range is higher than the first temperature range. By performing the second roasting step after performing the first roasting step, the bitterness component and the alkaloid component can be effectively eliminated. Preferably,
The temperature range is 180 ° C. or higher and 250 ° C. or lower. Within this temperature range, it is possible to effectively obtain tea leaves from which alkaloid components and bitterness components are removed as a result, while maintaining well the magnolol as well as the flavor and aroma. 18
If it is lower than 0 ° C, the removal of bitterness components and the like tends to be insufficient, and if it exceeds 250 ° C, the flavor tends to deteriorate. More preferably, it is 180 ° C. or higher and 200 ° C. or lower. The roasting time is not particularly limited, but heating for a long time leads to the disappearance of the active ingredient and the fragrance, so the time is preferably from a few minutes to a long dozen minutes, and more preferably from 2 minutes to 10 minutes. It is within minutes, and more preferably from 3 minutes to 5 minutes.

It is preferable that the second roasting step is continuously carried out subsequent to the first roasting step. By such continuous implementation, removal of internal water and disappearance of bitterness components and the like can be effectively achieved. It is preferable to immediately carry out the second roasting step on the leaves immediately after carrying out the first roasting step, but to the extent that the heat supplied to the hoo leaves in the first roasting step is roughly maintained. The gap between the first roasting step and the second roasting step is included in the continuous operation.

For example, the first roasting step and the second roasting step in the present invention can be carried out as follows. The fine pieces of peach leaves are passed through the hollow oven heated to the first temperature range for a predetermined time, and then passed through the hollow oven heated to the second temperature range.
In each oven, it is preferable that the linseed leaves move while being stirred and mixed.

The transition from the first temperature range to the second temperature range can be accompanied by a temperature raising step within an allowable time. The temperature raising step is preferably as short as possible.

(Honoki Tea Leaf and Tea Leaf Composition) By carrying out such a roasting step, a primary processed product of hoo leaves of the present invention, that is, honoki tea leaves can be obtained. According to such a tea leaf, the bitterness component and the alkaloid component are effectively eliminated, and the tea leaf has both an active ingredient and a palatability. The obtained tea leaves can be not only conventional tea leaves but also tea beverages. Further, it can be pulverized into powdery tea, or it can be in the form of being left as it is or mixed with confectionery such as rice crackers, steamed buns, yokan, and processed foods such as miso, jam, and sprinkles for edible use. Alternatively, conventionally known various tea leaves, that is, green tea leaves, persimmon leaves, peach leaves, ginkgo leaves, shakachu leaves, dokudami leaves, pigeon barley, mandarin orange peel, akebi no vine, mulberry leaves, kikuimo, salcia, taranome, agarix, Phellinus linteus,
It can also be provided as a tea leaf composition in combination with one or more materials selected from the group consisting of Reishi, ginseng and its leaves, and field seven carrots and its leaves. Also in such a tea leaf composition, the tea leaf may be in the form of a conventional strip, may be in the form of powder, or may be a mixture of various forms. It can also be provided as a beverage.

In particular, the honoki tea leaves of the present invention contain magnolol. Magnolol is 0.100 wt%
It is preferably contained in the following range. Magnolol is preferably 0.002 wt% or more and 0.090 wt
% Or less. When it is less than 0.002 wt%, the flavor and effectiveness tend to be low, and when it exceeds 0.090 wt%, the bitterness and the like tend to increase. More preferably, the upper limit is 0.080 wt% or less, and further preferably 0.070 wt% or less. On the other hand, alkaloid components (magnoclarin, magnoflorin, saliciphorin, etc.) are contained in a total amount of 0.
It is preferably not more than 01 wt%. More preferably, it is 0.005 wt% or less, and further preferably,
0.001 wt% or less, and most preferably 0.0
It is 005% or less.

Magnolol can be quantified according to the following method, for example. Approximately 50 g of honoki tea leaves are weighed in a 300 mL eggplant-shaped flask, and ether 200 is added.
After attaching a reflux condenser added with mL, heat in a water bath at 50 ° C. or lower for 1 hour. After cooling, the mixture is filtered by filtration (filter paper for quantitative determination), 200 mL of ether is further added to the residue, and the same operation is performed. The ether layers are combined and evaporated under reduced pressure with an evaporator. Add methanol to the residue to dissolve it, and make exactly 20 mL with methanol to make a sample solution. Weigh out 10 mg of magnolol standard product, dissolve in methanol and measure exactly 20 mg.
mL was used as a standard solution. The HPLC conditions are silica gel modified with octadecylsilanol group (particle size 5 μm,
TSKgel Tosoh Co., Ltd.) was packed in a column having a diameter of 4 mm and a length of 15 cm, and a mobile phase was made to flow a water: acetonitrile: acetic acid mixture (40: 60: 1) at 1.0 mL / min, and an ultraviolet absorptiometer ( Magnolol is detected at 294 nm) and the content is calculated. Note that this method can be similarly applied to the honoki leaf extract. In this case, the sampling amount can be about 5 g.

The following detection method (TLC method) can be applied to the detection of alkaloid components. Also, H
Also by the PLC method, the alkaloid component can be confirmed with a detection sensitivity equivalent to that of the TLC method.

(Thin layer chromatographic method: TLC method) About 5 g of honoki tea leaves was placed in a centrifuge tube, 50 mL of 0.1 M hydrochloric acid: methanol (1: 1) solution was added, and the mixture was shaken for 30 minutes. Centrifugation (5 minutes at 3000 rpm)
Then, the supernatant is subjected to qualitative analysis by thin layer chromatography. The thin layer plate was activated by using silica gel (200 μm, F254 + 365 manufactured by Merck & Co., Inc.) containing a fluorescent agent at 110 ° C. for 30 minutes and then allowed to cool with a desiccator (silica gel). About 2 mg of magnoclarin as a standard substance was precisely weighed and the same operation was performed. 10 μL each of sample solution and standard solution
2.5 cm from the right to 2 cm from the bottom edge of the thin plate.
It was applied every cm. About 10c using toluene: ethyl acetate: diethylamine (70:20:10) as a developing solvent.
After being developed, it was air-dried. UV irradiation (UV-
(365 nm) and a Dragendorf reagent solution are sprayed to confirm the spot, and the Rf value is measured. Other alkaloid components can be similarly detected using standard products. Note that this method can be similarly applied to the honoki leaf extract. The collected amount can be about 5 g.

(High Performance Liquid Chromatography: HPLC
Method) Take 50 g of honoki leaf tea in a centrifuge tube, add 20 mL of 10% 0.1 M hydrochloric acid to ethanol, and add 4
After heating at 5 ° C. to dissolve, the mixture was shake-extracted. Centrifuge for 10 minutes with a centrifuge (3000 rpm), transfer the supernatant to a measuring flask to make exactly 50 mL of ethanol, and measure by HPLC method. A standard solution is prepared, and from the peak (height or area) of this standard solution and the retention time,
The presence or absence or content of alkaloid components such as magnoclarin in the sample is measured. The HPLC conditions may be the same as those for magnolol. The sample solution obtained by the sample solution preparation method applied to the above-described magnolol HPLC method can also be adopted. Moreover, this method can be similarly applied to the honoki leaf extract. The collected amount can be about 5 g.

(Phoenix Leaf Extract) The phoenix leaf extract of the present invention can be obtained by extracting the tea leaves obtained in the above step by a conventional method to obtain an extract. There are no particular restrictions on the extract manufacturing process, and various known methods can be used. The honoki tea leaves can be extracted by extracting with water and / or a hydrophilic organic solvent (including alcohols such as methanol and ethanol and ketones such as acetone, preferably ethanol). Usually, hot water or dilute ethanol (ethanol 5
0 wt% aqueous solution). Hereinafter, an example of hot water extraction and an extract production process using dilute ethanol will be described.

(Production example of hot water extract) Roasted tea leaves are pulverized with a mixer or the like, and about 500 g thereof is weighed and placed in a 2 L beaker. 500 mL of distilled water
And soak for about 30 minutes. Furthermore, 500 mL of distilled water
And boil on a hot plate or on a burner for about 3 hours. After cooling, filter with a wide-mouth funnel using gauze as a filter cloth. Add 1 L of distilled water to the residue and boil for about 1 hour. After cooling, it is filtered in the same manner. The filtrates are combined and filtered again using qualitative filter paper. Dispense into a 200 mL beaker and freeze. It is dried using a freeze dryer, and the dry powder is used as a hot water extract.

(Production Example of Dilute Ethanol Extract) Similar to the production example of the hot water extract, about 500 g of powdered tea leaves are weighed and placed in a 2 L beaker. 500 diluted ethanol
Immerse in mL for about 30 minutes. Further diluted ethanol 500
Add mL, stir well and leave for about 24 hours. Filter the qualitative filter paper through the funnel through the opening. The extract is stored in a refrigerator, and 1 L of dilute ethanol is added to the residue and left for about 24 hours. Similarly, the mixture is filtered, and an appropriate amount is dispensed into an eggplant-shaped flask and distilled off with an evaporator to obtain a diluted ethanol extract.

The peach leaf extract thus obtained is
The extract has the same characteristics because the bitter components and the like are effectively removed from the raw material, tea leaves.
In the extract, magnolol is concentrated. Magnolol is 1wt% in peach leaf extract
% Or more and 5 wt% or less is preferable. More preferably, it is 2 wt% or more and 4 wt% or less. Magnolol can be quantified according to the method for quantifying magnolol in tea leaves.

In the extract, when the alkaloid component is tested by a method similar to the method for detecting magnoclarin in tea leaves, the extract is preferably 0.1 wt% or less, more preferably 0.01 wt%. Or less, more preferably 0.001 wt% or less, and most preferably 0.0005% or less.

(Phoenix Leaf Extract Composition) The phoenix leaf extract composition of the present invention can be made into a pea leaf extract composition by adding various additives and mixing them in order to prepare various foods or preparations. In order to enhance the palatability or usability of the pea leaf extract of the present invention, it is preferable to supply a masking agent to the pea leaf extract to form a granule. As the masking agent, a conventionally known masking agent can be used. Further, these masking agents can be supplied to the present extract by a known method. In addition, the holly leaf extract supplied with the masking agent can be granulated by a known method depending on the type or supply form of the masking agent. Both masking agent delivery and granulation are well known to those skilled in the art.

As the masking agent, cyclodextrin, dextrin (any of α, β and γ),
Silicon dioxide, anhydrous saccharides, methylcellulose, enzymatically decomposed lecithin (the enzyme can be papain, bromelain, lysozyme, etc.), shellac and the like can be used. These may be used alone or in combination of two or more. Preferred is shellac.

The blending amount of the masking agent is not particularly limited, but is preferably 100 parts by weight or more and 800 parts by weight or less with respect to 100 parts by weight of the extract. This is because if it is less than 100 parts by weight, the masking effect is poor, and if it exceeds 800 parts by weight, the dissolution property in artificial gastric juice or artificial intestinal fluid is too low. More preferably, the masking agent is 200
The amount is not less than 400 parts by weight. Particularly with respect to shellac, both masking and elution can be achieved by supplying such a composition.

An example of applying a masking agent to holly leaf extract to form a granular agent will be described. Hoo leaf extract 100
200 to 400 parts by weight of a masking agent such as shellac is added to parts by weight, and dispersed or dissolved and mixed in a solution state. After homogenization, the mixture is coagulated and dried, then crushed, and the pulverized granules are passed through a screen having an appropriate mesh size to obtain a granule having a predetermined particle size. In addition to the above, in the granulation, other methods such as crushing after freeze-drying, granulation at the same time as drying by spray drying, or granulation by granulating while drying can be appropriately adopted. The particle size is
Although not particularly limited, it is preferably 0.5 mm or less. The lower limit is preferably 0.1 mm or more. The particle shape of the obtained granular agent is not particularly limited, and various shapes such as an irregular shape, a spherical shape, and a rod shape can be adopted.

The peach leaf extract composition containing the peach leaf extract and / or the masking granule containing the extract can take various forms. That is, in addition to food forms such as foods and health foods, various formulation forms such as nutrients and drugs can be adopted. Additives and excipients required depending on the form of food or the form of preparation are well known to those skilled in the art. As for the form of food, in addition to food itself, it can be dissolved, dissolved or suspended to give a beverage. Also,
It may be added to other foods, and may be added to other foods for the purpose of flavor, nutritional supplement or health promotion. Examples of other foods to be added include confectioneries such as rice crackers, steamed buns, yokan, and processed foods such as miso, jam, and sprinkles.

Formulation forms of nutritional supplements and drugs include
Although not particularly limited, it is preferably an oral agent or an enteral agent. As oral agents, tablets, capsules, troches, chewable powders, powders, granules, fine granules, syrups, solids such as powders and tablets to be dissolved in water when necessary should be adopted. You can The enteral agent may be a liquid or a solid agent such as a powder or tablet that dissolves during use. In addition, it is also preferable to use an external preparation such as lotion, cream, gel, and bath, or a cosmetic. It can also be used as an additive such as a holly leaf extract and / or an extract-containing masking granule, an excipient applied to foods and pharmaceuticals.

Further, according to the holly leaf extract and / or the extract-containing masking granule, it can be used as an additive for tea leaves. That is, when these are used by adding them to honoki tea leaves, it is possible to provide a tea leaf composition in which the effectiveness of honoki tea leaves is enhanced. Also,
If used by adding to other tea leaves, compared to conventional tea leaves,
It is possible to provide a tea leaf composition provided with an active ingredient and scent derived from honoki. In any case, according to such a tea leaf composition, it is possible to provide a tea leaf composition which particularly contains a large amount of active ingredients such as magnolol and has a preferable flavor and scent.

[0039]

EXAMPLES Hereinafter, specific examples of the present invention will be described.
It is an example for better explaining the present invention and does not limit the present invention.

(Example 1) Example of extraction of magnolol and the like from hoo leaves The hoo leaves collected were raw leaves, leaves dried in the shade for about 1 month,
The dried leaves were divided into petioles, veins and mesophyll. Each was made into powder with a mixer or the like, and about 50 g of the powder was weighed in a 300 mL eggplant-shaped flask, a reflux condenser added with 200 mL of ether was attached, and then heated in a water bath at 50 ° C. or lower for 1 hour. After cooling, filtration (filter paper for quantification) was performed, and 200 mL of ether was further added to the residue and the same operation was performed. The ether layers were combined and evaporated under reduced pressure with an evaporator. Add methanol to the residue to dissolve it, and add 20
mL was used as the sample solution. In addition, the dilute ethanol extract and hot water extract extracted from these are methanol 50
It was dissolved in mL to obtain a sample solution. 10 mg of each standard product of magnolol and magnoclarin was weighed and dissolved in methanol to make exactly 20 mL to prepare a standard solution. As the HPLC conditions, silica gel (particle size 5 μm, TSKgel Tosoh Co., Ltd.) modified with an octadecylsilanol group was packed in a column having a diameter of 4 mm and a length of 15 cm, and water was used as a mobile phase.
Acetonitrile: acetic acid mixture (40: 60: 1) was flowed at 1.0 mL / min, and magnolol and magnoclarin were detected by an ultraviolet absorptiometer (294 nm). The content was calculated using standard products of both components. The results are shown in Table 1.

[Table 1]

(Example 2) Production Test Example 1 (Pho-cha Production Example) The present invention, which is an example of producing pho-tea, will be specifically described below with respect to the results of drying, roasting and evaluation. It is not limited to these hoo leaf tea production methods.

Drying method 10 sheets each were bundled and stacked by changing the direction of the leaf axis and the front and back.
Drying conditions As shown in Table 2.

[Table 2]

Dry A or B rank hoo leaves under the conditions of the roasting method were kneaded by hand or by a machine or cut into 5 mm square pieces and roasted under the following conditions. The combination of body water removal and roasting was as shown in Table 3.

[Table 3]

3 g of hoo leaf tea roasted under the conditions of taste and fragrance were placed in a teapot and poured into boiling water to evaluate the taste and fragrance. It was cut into about 5 mm square and roasted under the following conditions. The taste and fragrance were evaluated by 5 people, and the taste and fragrance were freely expressed, and 5 people rated it as good (◎) when the taste and fragrance were sufficient and could be continued to be consumed. 3 people rated it as good (○), 1 out of 5 people who can drink but do not like it very much
People rated it as good (△), and when bitterness and astringent taste remained and was not suitable for drinking, none was rated as good (×).
Divided into The results are shown in Table 4.

[Table 4]

According to the evaluation of the main component content, the magnolol content of the main component was measured by the above-mentioned method. The results are shown in Table 5.

[Table 5]

(Example 3) Production test example 2 (manufacture example of hoo tea) Dried hoo leaves were dried by the drying method of manufacture test example 1 and dried A and B rank ones were divided into mesophyll and petioles. Was cut to about 1 mm. The roasting method is shown in Table 3,
An example of roasting under the conditions of 2, 3, 5, 6, 7, and 8 is shown.

Evaluation of Taste and Aroma The roasted mesophyll and petioles were mixed at various ratios, and 3 g each was placed in a tea bag to give hoo leaf tea. The tea bangs were placed in a teacup, and boiling water was poured to evaluate the taste and aroma. The evaluation of taste and aroma was performed by 5 persons as in Production Test Example 1. The results are shown in Table 6.

[Table 6]

According to the evaluation of the main component content, the magnolol content of the main component was measured by the above-mentioned method. The results are shown in Table 7.

[Table 7]

(Example 4) Production Test Example 3 (Production Example of Pho-Leaf Extract) Hereinafter, the present invention will be described in detail with reference to Examples of the preparation method of pea-leaf extract. It is not limited to.

1. Preparation Method of Hot Water Extract The honoki tea leaves of the present invention obtained by roasting were powdered with a mixer or the like, and about 500 g thereof was weighed and placed in a 2 L beaker. Distilled water (500 mL) was added thereto, and the mixture was immersed for about 30 minutes. Furthermore, 500 mL of distilled water was added and the mixture was boiled on a hot plate or on a burner for about 3 hours. After cooling, filter with a wide-mouth funnel using gauze as a filter cloth. 1 L of distilled water for the remainder
Was added and boiled for about 1 hour. After cooling, it was filtered in the same manner. The filtrates are combined and filtered again using qualitative filter paper. 200m
It was dispensed into a L beaker and frozen. It was dried using a freeze dryer, and the dry powder was used as a hot water extract.

2. Preparation method of dilute ethanol extract 1. Approximately 500 g of honoki tea leaves powdered in the same manner as
Was weighed and placed in a 2 L beaker. Dilute ethanol 5
Immerse in 00 mL for about 30 minutes. Further dilute ethanol 5
00 mL was added, and the mixture was stirred well and left for about 24 hours.
The qualitative filter paper was filtered through a funnel with a through hole. The extract is stored in a refrigerator and the residue is diluted with 1 L of dilute ethanol.
It was added and left for about 24 hours. Similarly, the mixture was filtered, and an appropriate amount was dispensed into eggplant-shaped flasks and distilled off with an evaporator to obtain diluted ethanol extract.

3. Main component content The magnole content of the main component was measured by the method described above. The results are shown in Table 8.

[Table 8]

4. Evaluation Method The bitterness of the hoo leaf extract in the preceding paragraph was evaluated, and a sensory test was carried out by allowing 5 expert panelists to include it in their mouths for 10 seconds. First, the standard bitterness solution (quinine sulfate) shown in Table 9 was included in the mouth, and the evaluation scale of each panel was unified. Next, 30 mg of hoo tea extract was dissolved in 20 mL of water, and a sensory test was conducted by including the sample in the mouth. The results are shown in Table 10.

[Table 9]

[Table 10]

(Example 5) Production test example 4 (extract-containing masking granule) 1. Raw materials used a) 2.5% magnolol holly leaf extract of the present invention b) shellac solution White shellac E (manufactured by Gifu shellac) 32% shellac c) β-cyclodextrin celltex B-100 (Japanese food processing) d ) Oxygen-decomposed lecithin Benecoat BMI-40 (Kao)

2. Formulation method a) Shellac-coated holly leaf extract and shellac solution were mixed in the ratios shown in Table 11 below, mixed with a stirrer for 10 minutes, and then dried under reduced pressure at 50 ° C to obtain a dried product. The dried product was crushed and sieved with a 0.5 mm screen to give a coating composition.

[Table 11]

B) Cyclodextrin clathrate holly leaf extract 10 parts and purified water 60 parts were mixed, and after mixing with a stirrer for 10 minutes, 40 parts of β-cyclodextrin was gradually added and stirring was continued for 90 minutes. This was freeze-dried, then crushed and sieved with a 0.5 mm screen to obtain a clathrate. α-Cyclodextrin or γ-cyclodextrin may be used.

C) Masking with enzyme-decomposed lecithin 10 parts of peach leaf extract and 40 parts of enzyme-decomposed lecithin were mixed, an appropriate amount of purified water was added, and the mixture was stirred in a mortar and granulated. After drying at 50 ° C. for 3 hours, it was crushed and sieved with a 0.5 mm screen to obtain a composition. Papain, bromelain-in, lysozyme and the like may be used as the enzyme.

3. Evaluation method With respect to the samples of the formulation methods a) and b), a sensory test was conducted by allowing 5 professional panelists to put the samples in their mouths for 10 seconds. A proficiency test was conducted with reference to the previous section.

4. Results The bitterness test results are shown in Table 12. The bitterness of peach leaf extract is
It was significantly improved by shellac coating. The result is 40
It is remarkable at 0% or more, and when compared with 400% coating, β-
It was more prominent than cyclodextrin and enzymatically degraded lecithin.

[Table 12]

(Example 6) Dissolution test in the body As a model experiment of the dissolution property of the pea leaf extract in the body, a dissolution test was conducted using artificial gastric juice and artificial intestinal fluid. Since the amount of the active ingredient of holly leaf extract is usually defined by the content of magnolol, magnolol was quantified as an index of its elution property.

1. Dissolution test 30 for samples containing 20 mg equivalent as peach leaf extract
After adding mL of artificial gastric juice and shaking at 37 ° C for 1 hour,
It was filtered with a 0.45 μm membrane filter. The filtrate was evaporated to dryness using an evaporator and used for the determination of magnolol. After collecting the residue, wash it with water to 30 mL.
After adding the artificial intestinal fluid of 1 above and shaking at 37 ° C. for 1 hour,
It was filtered with a 45 μm membrane filter. The filtrate was evaporated to dryness using an evaporator and used for quantification of macnolol. The quantification was according to the above-mentioned HPLC method.

2. Dissolution rate Dissolution rate is based on the magnolol content of the used hoo leaf extract.
It was set to 00, and it calculated | required from the sum total of the magnolol content eluted in the artificial gastric juice and the artificial intestinal fluid. The elution results are shown in Table 13. It was considered that the elution property of holly leaf extract in the body was good when it was 400% or less even if it was coated with a ceramic, and poor when it was 800% or more.

[Table 13]

3. Consideration and comprehensive evaluation When the above results are comprehensively evaluated, the shellac 10% coating has good in-body dissolution but little bitterness masking effect. Similarly, 100-200% coating has good in-body dissolution but slightly poor bitterness masking. It was found that at 800% or more, the bitterness masking effect was exhibited, but the in-body dissolution property was deteriorated. For this reason, the most desirable is 200-400%
It was found that a shellac coating composition having a good feeling in use and a good elution property in the body can be obtained by coating the shellac of the above.

(Example 7) Alkaloid removal test example Although the content of toxic alkaids (magnoclarine, magnoflorin, saliciphorin, etc.) is scarcely present in pea leaves, it can be removed by roasting by comparing wood and leaves. Indicates.

1. Qualitative properties of magnoclarin (thin layer chromatographic method: TLC method) About 5 g of honoki bark and hoo leaf tea or about 0.5 g of hoo leaf extract were placed in a centrifuge tube, and a 0.1 M hydrochloric acid: methanol (1: 1) solution was added. 50 mL was added and shaken for 30 minutes. After centrifugation (3000 rpm for 5 minutes), the supernatant is qualitatively analyzed by thin layer chromatography.
The thin layer plate was activated by using silica gel (200 μm, F254 + 365 manufactured by Merck & Co., Inc.) containing a fluorescent agent at 110 ° C. for 30 minutes and then allowed to cool with a desiccator (silica gel). About 2 mg of magnoclarin as a standard substance was precisely weighed and the same operation was performed. 10 μL of each of the sample solution and the standard solution was applied at a distance of 2 cm from the lower end of the thin layer plate in order from the right at 2.5 cm intervals. After developing with toluene: ethyl acetate: diethylamine (70:20:10) for about 10 cm as a developing solvent, the mixture was air-dried. UV irradiation of thin layer plate (UV-365
nm) and the Dragendorff reagent solution were sprayed to confirm spots, and Rf values were measured.

2. Quantification of magnoclarin (high-performance liquid chromatography method: HPLC method) 50 g of hoo leaf tea or 5 g of hoo leaf extract was placed in a centrifuge tube, and a solution 2 was prepared by adding 10% of 0.1 M hydrochloric acid to ethanol.
After adding 0 mL and heating at 45 degreeC and melt | dissolving, it shake-extracted. Centrifugation was carried out for 10 minutes with a centrifuge (3000 rpm), the supernatant was transferred to a measuring flask to make exactly 50 mL of ethanol, and measured by HPLC method. The detected peak is indicated by the retention time (retention time RT).

3. Table 14 shows the detection of alkaloid components by evaluation roasting. H
PLC R.M. T. Although it could not be identified as magnoclarin, alkaloids were not detected in holly leaf tea and holly leaf extract by both TLC method and HPLC method.

[Table 14]

[0068]

EFFECTS OF THE INVENTION According to the present invention, it is possible to provide a processed holly leaf product containing an active ingredient from holly leaf and having a reduced bitterness component and the like.

─────────────────────────────────────────────────── ───

[Procedure amendment]

[Submission date] April 11, 2002 (2002.4.1)
1)

[Procedure Amendment 1]

[Document name to be amended] Statement

[Name of item to be corrected] Claim 16

[Correction method] Change

[Correction content]

   ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Satoshi Sakai             1-18-2, Hayadahonmachi, Gifu City, Gifu Prefecture             Gifu Prefectural Forest Research Institute (72) Inventor Hisamitsu Nagase             2 Gifu medicine at 353 Kitanohigashi, Gifu City, Gifu Prefecture             Department of Hygiene (72) Inventor Masanori Mizuno             8-2-2, Izumi 2-chome, Higashi-ku, Nagoya-shi, Aichi             Asgen Pharmaceutical Co., Ltd. (72) Inventor Kazuo Mochizuki             3 370, Ikeda, Shizuoka City, Shizuoka Prefecture             Shizuoka tea garden F-term (reference) 4B017 LC03 LE01 LE10 LG14 LG15                       LG19 LK01 LK11 LK13 LP01                       LP03 LP04                 4B018 LB08 LE03 LE05 MD01 MD27                       MD35 MD36 MD61 ME14 MF01                       MF04 MF06

Claims (20)

[Claims] 1. A method for producing a processed product of honoki, which comprises the steps of drying fresh leaves of honoki and roasting the dried leaves. 2. The roasting step comprises a first roasting step in a first temperature range and a second roasting step in a second temperature range higher than the first temperature range. The method of claim 1. 3. The method according to claim 2, wherein the first roasting step is a step of mainly removing body water. 4. The first temperature range is 100 ° C. or higher and 150 ° C.
And the second temperature range is 180 ° C. or higher and 250
The method according to claim 2 or 3, which is at most ° C. 5. The method according to claim 2, wherein the second roasting step is continuously performed after the first roasting step. 6. The method according to claim 1, wherein the drying step is performed at 80 ° C. or higher and 110 ° C. or lower. 7. The first temperature range is 100 ° C. or higher and 135 ° C.
The method according to claim 2, wherein: 8. The second temperature range is 180 ° C. or higher and 200 ° C.
The method according to claim 2, wherein: 9. A honoki tea leaf, which is obtained by roasting a dried honoki leaf. 10. The tea leaf according to claim 9, which is obtained by roasting at a temperature of 100 ° C. to 150 ° C. and then roasting at a temperature of 180 ° C. to 250 ° C. 11. A honoki tea leaf containing magnolol, wherein the alkaloid component content is 0.01 wt% or less.
tea leaf. 12. The tea leaf according to claim 11, which contains 0.002 wt% or more and 0.090 wt% or less of magnolol. 13. The honoki tea leaves according to any one of claims 9 to 12, and green tea leaves, persimmon leaves, peach leaves, ginkgo leaves, shakuchu leaves, dokudami leaves, doves, citrus peels, akebi no vines, and mulberry leaves. Leaf, Jerusalem artichoke,
Salacia, Taranome, Agaricus, Phellinus linteus, Reishi,
A tea leaf composition, which comprises one or more teas selected from the group consisting of ginseng carrots and leaves thereof, and field seven carrots and leaves thereof. 14. A honoki leaf extract, which is obtained by extracting the tea leaves of the honoki according to any one of claims 9 to 12 with water and / or a hydrophilic organic solvent. 15. A honoki leaf extract having a magnolol content of 1 wt% or more and an alkaloid component content of 0.01 wt% or less.
extract. 16. A method for producing a honoki leaf extract composition, which comprises a step of drying fresh leaves of honoki, and a first roasting step in which the dried leaves are roasted at a temperature of 100 ° C. or higher and 150 ° C. or lower. Step, a second roasting step of roasting the leaves that have undergone the first roasting step at a temperature of 180 ° C. or higher and 250 ° C. or lower, and the leaves after the second roasting step are water and / or hydrophilic. A method comprising: a step of extracting with a volatile organic solvent to obtain an extract; a step of supplying a masking agent to the obtained extract to mix them; and a step of granulating the mixture. 17. The method according to claim 16, wherein the masking agent is one or more selected from the group consisting of cyclodextrin, dextrin, silicon dioxide, anhydrous saccharides, methylcellulose and shellac. 18. A honoki leaf component-containing composition comprising 100 parts by weight of the honoki leaf extract according to claim 14 or 15 and 200 parts by weight or more and 400 parts by weight or less of a masking agent. 19. The composition according to claim 18, wherein the masking agent is one or more selected from the group consisting of cyclodextrin, dextrin, silicon dioxide, anhydrous saccharides, methylcellulose and shellac. 20. The composition according to claim 18 or 19, further comprising the honoki tea leaf according to any one of claims 9 to 12.