WO2007102438A1 - Fractionation product of aqueous extract of eucommia ulmoides oliver leaf, and anti-obesity agent comprising the fractionation product - Google Patents
Fractionation product of aqueous extract of eucommia ulmoides oliver leaf, and anti-obesity agent comprising the fractionation product Download PDFInfo
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- WO2007102438A1 WO2007102438A1 PCT/JP2007/054083 JP2007054083W WO2007102438A1 WO 2007102438 A1 WO2007102438 A1 WO 2007102438A1 JP 2007054083 W JP2007054083 W JP 2007054083W WO 2007102438 A1 WO2007102438 A1 WO 2007102438A1
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- leaf
- extract
- fraction
- tochu
- dried
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- 239000005720 sucrose Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 238000012353 t test Methods 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 238000011200 topical administration Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7042—Compounds having saccharide radicals and heterocyclic rings
- A61K31/7048—Compounds having saccharide radicals and heterocyclic rings having oxygen as a ring hetero atom, e.g. leucoglucosan, hesperidin, erythromycin, nystatin, digitoxin or digoxin
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P3/00—Drugs for disorders of the metabolism
- A61P3/04—Anorexiants; Antiobesity agents
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Definitions
- the present invention relates to a water extract fraction of Tochu Nakaba, and an anti-obesity agent, a composition for oral consumption, a pharmaceutical composition, a food composition, a medicine and a food containing the fraction. Furthermore, the present invention relates to a method for producing the fraction.
- Eucommia ulmoides oliver is a deciduous woody plant that is classified as a genus of the genus Eucommia from Central China, and has a height of 20m. Tonaka is different from the camellia plant, generally called tea, in that it contains no caffeine. Tochu Nakaba has been widely used as a beverage since the 1980s. ⁇ Naka scabbard is treated as a pharmaceutical and is used in China as an effective Chinese medicine for “hypertension, low back pain, joint pain, kidney disease, liver disease, stress, loss of energy, diuresis difficulty, and forgetfulness”.
- Patent Document 1 Japanese Patent Laid-Open No. 2005-289950
- Patent Document 2 JP-A-2005-289951
- Patent Document 3 Japanese Patent Laid-Open No. 2003-342185
- Patent Document 4 Japanese Patent Laid-Open No. 2002-179586
- Patent Document 5 Japanese Patent Laid-Open No. 2002-275077
- the present invention provides a fractionation method for efficiently extracting components of Tochu Naka leaf, particularly medicinal components such as iridoidoid compounds, and Tonaka leaf component containing a specific component at a high concentration.
- the purpose is to provide a fraction.
- the present invention relates to an anti-obesity agent, composition for oral intake, pharmaceutical composition, food composition, medicine and food, which is made of natural materials as raw materials and has little side effects and is safe even when ingested over a long period of time.
- the purpose is to provide.
- a foliage extract of Tochu Nakaba water obtained by a production method comprising:
- the methanol aqueous solution may be a methanol aqueous solution of 10% by volume or more and less than 40% by volume, preferably 20 to 35% by volume, more preferably 25 to 35% by volume. For example, a 30% by volume methanol aqueous solution can be used.
- the aqueous methanol solution for example 40 to 60% by volume, preferably using Yogu example 50 volumes 0/0 of methanol aqueous solution be an aqueous methanol solution of 45-55 volume 0/0 be able to.
- the fraction of the Nakanaka leaf water extract already defined as the present invention comprising 10 to 90% by weight of an iridoidic compound as a solid component after distilling off the solvent.
- asperuloside is, for example, 10% by weight or more, preferably 20% or more, more preferably 30% or more, and still more preferably as a solid component after the solvent is distilled off.
- the dried bonito leaves steamed bonito leaves Obtained by a production method comprising the steps of drying and stirring the zhongyou leaves with z or pressure; and irradiating the kungyou leaves with far infrared rays; Leaf water extract fractions are provided.
- an antiobesity agent and antiobesity agent comprising a fraction of a foliage extract already defined as the present invention.
- a medicine and a food containing the anti-obesity agent already defined as the present invention are provided.
- the food is not particularly limited, and may be, for example, a functional food, a health food, a health supplement, a nutritional supplement, an insurance function food, a specific insurance food or a nutrition function food.
- a method for producing a fraction extracted from a dried nakanaka leaf wherein the extracted nakanaka leaf water extract is adsorbed on a synthetic adsorbent in reverse phase. And washing with water followed by elution with a 5-80% by volume aqueous methanol solution.
- the obtained Nakanaka leaf water extract fraction contains a 10 to 90% by weight of an iridoid compound, and is already defined as the present invention.
- a manufacturing method is provided.
- the ispel mouth side is, for example, 10% by weight or more, preferably 20% or more, more preferably 30% or more, and further preferably 40% or more (for example, 10 to 10%).
- the fraction of Tochu Nakaba extract contains an iridoidic compound at a high concentration, and is therefore useful in the manufacture of a medicine or food for ingesting the compound. Furthermore, since the anti-obesity agent according to the present invention is a natural material and can be safely ingested over a long period of time, a stable anti-obesity effect with less burden on the patient can be obtained.
- Examples of the iridoid compound contained in the fraction of the present invention include, for example, those contained in Tochu Nakaba.
- Examples include iridoid compounds that are saccharide components. Specific examples thereof include geposide acid, asperculoside, asperulosidic acid, diacetyl persulfate, scandoside 10-O-acetate, oakbin and the like.
- the chunaka leaf water extract in the present invention is prepared using, for example, dried chunaka leaf.
- the dry licorice leaf is not particularly limited, but can be prepared, for example, by subjecting licorice leaf to a specific process.
- the bamboo shoot leaves mean the bamboo leaves before harvest and before drying, and may be produced by cultivation or collected from nature. For example, fresh leaves before fallen leaves of the current year can be used, and fresh leaves can be used from April to October, preferably from May to August, more preferably from July to August.
- the cocoon leaves of the present invention may be used as they are, or may be cut. Therefore, the present invention may further include a step of cutting the green leaves. ⁇ ⁇ may be cut into a width of, for example, about 5 to 30 mm, preferably about 10 to 20 mm. In the present invention, unbroken cocoon leaves are preferably used. By using the uncut green leaves, it becomes possible to dry gently and gently in the subsequent drying process, and it is possible to suppress the yield drop and the discoloration of the green leaves during the drying. .
- the steaming process of the cocoon leaves in the present invention can be carried out by a method usually performed in the technical field using a commercially available steamer or an autoclave.
- a commercially available steamer or an autoclave For example, it is possible to steam heat-treat cocoon leaves by spreading them on a net conveyor and passing them through a treatment chamber filled with non-pressure steam supplied from a boiler.
- Kashimura Tekko Co., Ltd., leaf feeder, ground type 1500, net conveyor, trolley type 100, etc. can be used.
- the steaming temperature may be appropriately selected within the range of, for example, 90 to 120 ° C., preferably 95 to 110 ° C., more preferably 100 to 110 ° C., depending on the size of Tochu Nakaba.
- the steaming time can also be appropriately selected within the range of 10 to 240 seconds, preferably 20 to 180 seconds, more preferably 20 to 120 seconds.
- the amount of steam used can be appropriately selected within the range of, for example, 200 to 70 LZ, preferably 170 to L00LZ.
- the treatment amount of the steamed leaves can be appropriately selected in the range of, for example, 3 to: LO kgZ, preferably 4 to 8 kgZ, more preferably 5 to 7 kgZ, depending on the moisture content of the fresh leaves.
- This steaming process discolored Tochu Naka to brown Inactivation of the enzyme that makes it easy to maintain the green color of the Nakanaka leaves; and the softness of the Nakanaka leaves makes it easy to perform the process of drying the Nakanaka leaves after the steaming process with stirring and Z or under pressure The effect of becoming.
- the steamed and heat-treated Tochu Nakaba can also be used in the next step as it is. It can also be used in the next step after cooling.
- the cooling here can be performed by removing rough heat by blowing air or the like.
- the step of drying the rice cake with stirring and Z or pressure is, for example, a commercially available continuous leaf cutter, rotary leaf cutter, batch-type leaf cutter or rough rice cutter.
- a commercially available leaf cutter leaf cutters (batch type) 60K, 90 ⁇ , 120K, and 180K manufactured by Kawasaki Kiko Co., Ltd. can be used.
- the crushing pressure in this process is performed by a “more hand” supported by a panel panel having an appropriate elasticity rotating in the leaf cutter and pressing the corrugated leaf against the wall of the processing cylinder.
- the stirring in this step is performed by rotating the “leaf crust” attached to the leaf cutter.
- the rolling pressure in this step is preferably performed gently, for example, by only rotating the leaves.
- the drying method is not particularly limited, but is preferably performed by sending hot air to Tochu Nakaba.
- the temperature of the hot air is not particularly limited, but may be appropriately selected from the range of, for example, 70 to 120 ° C, preferably 75 to 110 ° C.
- the time required for this step can be appropriately selected within the range of 10 to 60 minutes, preferably 15 to 50 minutes, more preferably 20 to 40 minutes. For example, this step can be performed at 100 ° C. for 20-30 minutes.
- the surface of the nakanaka leaf can be maintained, the surface temperature of the nakanaka leaf can be kept within a certain range, and drying can be performed while suppressing discoloration of the nakanaka leaf. It becomes possible.
- This process The surface temperature of Tochu tea leaves during drying is, for example, 30 to 60 ° C, preferably 40 to 50 ° C.
- the water content of Tochu Nakaba obtained through this step is, for example, 30 to 45%, preferably 30 to 40%, more preferably 30 to 35% on a dry basis.
- the present invention includes a step of homogenizing the moisture of the chunaka leaf between "the step of drying the chunaka leaf with stirring and Z or pressure" and "the step of drying the chunaka leaf". It may be.
- the step of homogenizing the water in the bamboo leaf can be carried out by a method usually performed in the technical field using, for example, a commercially available twister, coarser, or intermediater.
- a commercially available twister Terada Seisakusho Co., Ltd.
- a twister 60 kg type can be used as a commercially available twister, Terada Seisakusho Co., Ltd.
- the homogenization of the water in the cocoon leaf in this process is performed, for example, by sandwiching the cocoon leaf between the turret and the rotating drum of the turret and pressurizing with the rotator while rotating the rotator. Is called. Since the Tochu leaves are dried in the order of mesophyll, vein, and leaf shaft, for example, even if the dryness of the leaf meat is sufficient, excess moisture still remains on the leaf shaft. Therefore, according to this step, the moisture in the bamboo leaf is uniformly prepared, and the powdery wrinkles due to partial drying are suppressed, and at the same time, the time required for drying can be shortened. This step can be performed with heating, if necessary, preferably without heating.
- the time required for this step can be appropriately selected within the range of 10 to 80 minutes, preferably 20 to 60 minutes, more preferably 30 to 45 minutes.
- this process can be performed at room temperature for 40 minutes.
- the force applied by the scissors during this process The no-pressing time at the start of the process can be appropriately selected in the range of 0 to 10 minutes, preferably 2 to 8 minutes, more preferably 4 to 5 minutes. .
- the moisture content of the chunaka leaf obtained through this step is, for example, 25 to 40%, preferably 25 to 35% on a dry basis.
- the present invention includes “a step of homogenizing moisture in the chunaka leaf”, an additional “step of drying the chunaka leaf with stirring and Z or under pressure before the step of drying the chunaka leaf. And “the step of homogenizing the water in the Tochu leaf”, or “the step of drying the Tochu leaf with stirring and Z or pressure” may be included. By repeating these steps, it is possible to obtain Tochu tea leaves from which unnecessary lipids have been further removed.
- the step can be performed by the method and conditions described above, and the temperature of the hot air is not particularly limited. 1S For example, a range force of 50 to 110 ° C., preferably 55 to 105 ° C. may be appropriately selected. The time required for this step can be appropriately selected within the range of 5 to 45 minutes, preferably 10 to 40 minutes, more preferably 10 to 35 minutes. For example, it can be performed at 70 ° C for 20 to 30 minutes.
- the step can be performed by the above-mentioned method and conditions, and the time required for this step is 10 to 80 minutes, preferably It can be appropriately selected within a range of 20 to 60 minutes, more preferably 30 to 45 minutes. For example, it can be performed at room temperature for 40 minutes.
- the step of drying the Tochu leaf of the present invention can be carried out, for example, by a method commonly performed in the technical field using a commercially available dryer.
- the drying method in this process is not specifically limited, For example, it can carry out by moving the Tochu Naka leaf on a conveyance conveyor in the high temperature drying chamber filled with the hot air by a hot air generator.
- a hot air generator For example, it can be performed by a dryer ND120 manufactured by Terada Manufacturing Co., Ltd.
- the temperature of the hot air is not particularly limited, but a range force of, for example, 70 to 100 ° C., preferably 85 to 95 ° C. may be appropriately selected.
- the time required for this step can be appropriately selected within the range of 5 to 80 minutes, preferably 10 to 70 minutes, more preferably 20 to 80 minutes.
- the water content of the bamboo leaf obtained through this step is, for example, a water content of 5% or less, preferably a water content of 3% or less, more preferably a water content of 2% or less.
- the present invention may include a step of drying the chunaka leaf by irradiating the chunaka leaf with far infrared rays.
- this process is not specifically limited, For example, it can be performed using the commercially available far-infrared heater.
- it can be performed by a VR type manufactured by Yamamasu Seisakusho Co., Ltd.
- the wavelength of the far infrared rays irradiated here is appropriately selected from the range of, for example, 1 to: LOOO / zm, preferably 2.5 to 50 ⁇ m, more preferably 3 to 30 ⁇ m.
- the irradiation set temperature during drying can be appropriately selected from the range of, for example, 100 to 400 ° C, preferably 150 to 350 ° C, more preferably 200 to 300 ° C.
- the time required for this step can be appropriately selected within the range of 30 to 60 seconds, preferably 40 to 55 seconds, and more preferably 45 to 50 seconds as the infrared lamp passing speed.
- the moisture content of the dried bamboo leaf obtained through this step is, for example, a moisture content of 5% or less, preferably a moisture content of 3% or less, more preferably a moisture content of 2% or less.
- the nakanaka leaf water extract uses, for example, 5 to 50 kg, preferably 10 to 30 kg, more preferably 15 to 20 kg force, of water appropriately selected for 1 kg of dried nakanaka leaf.
- the extraction temperature can be appropriately selected from the range of, for example, 85 to 98 ° C, preferably 90 to 95 ° C.
- the extraction time is not particularly limited, but can be appropriately selected, for example, 10 to 120 minutes, preferably 20 to 90 minutes, more preferably 30 to 60 minutes.
- Filtration of the extract may be performed using, for example, a filter or a 30-200 mesh filter.
- the filtrate may be allowed to stand for a certain period before concentration. Unnecessary substances can be removed by removing precipitates generated by standing.
- the standing time is not particularly limited, but may be appropriately selected from, for example, 1 to 24 hours, preferably 6 to 20 hours, and more preferably 8 to 18 hours.
- the temperature at the time of standing is not particularly limited. For example, a force of 0 to 35 ° C, preferably 0 to 16 ° C, more preferably 2 to 8 ° C can be appropriately selected.
- the soot extract obtained in this way can be used as it is, but the supernatant obtained after removing the precipitate generated by centrifugation can also be used in the next step. Further, the supernatant can be used after being concentrated.
- the "reverse-phase synthetic adsorbent" used in the present invention is not particularly limited as long as it is usually used for separation of natural components, etc., but is not limited to polystyrene gel (polystyrene'divinylbenzene copolymer, etc.). ), For example, MCIGEL CHP10M / CHP2MGM, SEPABE
- the adsorbent can be used as a column carrier, for example.
- the amount of adsorbent used can be selected, for example, from 1000 to 18000 g, preferably ⁇ 15000 to 18000 g, per 110 L of Tochu leaf extract.
- the Tochu leaf extract is injected into a column packed with a reverse-phase adsorbent, and then the eluted components are removed using water as the eluent.
- the fraction of the present invention can be eluted from the column using an aqueous solution of ⁇ 80% by volume of methanol as an eluent.
- the amount of water used as the eluent is not particularly limited. For example, for an adsorbent of 17200 g, a range force of 70 to: L 10 L is selected. Can be used in
- the methanol aqueous solution used as the eluent may be, for example, a methanol aqueous solution of 10% by volume or more and less than 40% by volume, preferably 15-30% by volume of methanol aqueous solution.
- a methanol aqueous solution of 10% by volume or more and less than 40% by volume preferably 15-30% by volume of methanol aqueous solution.
- 40-60 volume% methanol aqueous solution for example, 50 volume% methanol aqueous solution
- each aqueous methanol solution is not particularly limited.
- an amount selected from the range of 70 L can be used for 17200 g of the adsorbent.
- a more preferable fraction containing the target component at a high concentration can be obtained by fractionating the eluate from the aqueous methanol solution.
- the fraction obtained as a water-methanol solution is preferably used after being concentrated.
- the concentration ratio is not particularly limited.
- the volume ratio is 60% or less, preferably 30% or less, and more preferably used as a solid product obtained by drying.
- the concentration can be carried out under normal pressure or under reduced pressure, but is preferably carried out under reduced pressure.
- the concentration method is not particularly limited as long as it is a commonly used method, and for example, it can be concentrated using a rotary evaporator or the like.
- anti-obesity agent used in the present specification is not particularly limited, but means, for example, a drug administered to obtain the effects of hypertension, hyperlipidemia, and diabetes.
- the anti-obesity agent of the present invention is not particularly limited, but other agents that can be used to improve obesity, preventive and therapeutic agents for antilipidemia, preventive and therapeutic agents for diabetes, hypertension, etc. Can be used with therapeutic or prophylactic agents.
- the anti-obesity agent of the present invention can be used as an active ingredient of a pharmaceutical composition.
- the pharmaceutical composition can be used in various dosage forms such as tablets, capsules, powders, granules, pills, solutions, emulsions, suspensions, solutions, spirits, syrups for oral administration.
- a pharmaceutical composition may contain various commonly used ingredients, such as one or more pharmaceutically acceptable excipients, disintegrants, diluents, lubricants, flavoring agents.
- composition of the present invention may be in a sustained or sustained release dosage form!
- the dose of the anti-obesity agent of the present invention can be appropriately selected depending on the patient's body shape, age, physical condition, degree of disease, elapsed time after onset, etc.
- the pharmaceutical composition of the present invention is a therapeutic agent.
- An effective amount and Z or a prophylactically effective amount of an anti-obesity agent can be included.
- it is generally used in the dose of 10 to 50000 mg / day / adult, preferably 100 to 5000 mg Z day Z adult, as the pulverized mash of the present invention or its water extract.
- Administration of the pharmaceutical composition can be single dose or multiple doses, for example, in combination with other drugs such as other anti-obesity agents.
- the food according to the present invention includes a liquid beverage and a solid food.
- the food can be used as quasi-drugs, other food and drink ingredients, food additives, and the like.
- the composition for ingestion in this specification can be used as a functional food as it is, and can be used as a component of a pharmaceutical, a quasi-drug, a food and drink, and a food additive.
- the use enables daily and continuous ingestion of the food or composition for oral consumption having the obesity-improving effect and arteriosclerosis-preventing agent of the present invention, effectively improving obesity, and obesity-related diseases. Effective prevention of (for example, hypertension, hyperlipidemia, diabetes, etc.) becomes possible.
- Examples of foods or beverages containing the anti-obesity agent of the present invention include functional foods having lipase-inhibiting effects or obesity-inhibiting effects, health foods, health supplements, nutritional supplements (nutrient drinks, etc.), insurance This includes functional foods, foods for specified insurance, functional foods for nutrition, general foods (diuse, confectionery, processed foods, etc.).
- the food or beverage in the present specification includes, as optional additives, inorganic components such as iron and calcium, various vitamins, dietary fibers such as oligosaccharides and chitosan, proteins such as soybean extract, lipids such as lecithin, Sugars such as sucrose and lactose, sweeteners such as aspartame, acesulfame potassium, stevia, sumatin, saccharin, sodium saccharin and the like can be included.
- inorganic components such as iron and calcium
- various vitamins such as oligosaccharides and chitosan
- proteins such as soybean extract
- lipids such as lecithin
- Sugars such as sucrose and lactose
- sweeteners such as aspartame, acesulfame potassium, stevia, sumatin, saccharin, sodium saccharin and the like can be included.
- Ion-exchanged water 70 L was added to dried potato Nakaba (10 kg) and heated at 65 ° C for 7 hours. After heating, it was left overnight.
- Use Zaru Tetron No.3 to remove the Tochu Nakaba residue, and then perform continuous centrifugation! (Centrifugal acceleration: 9340xg; (S-type ultra-high-speed centrifuge U-6-H: manufactured by Kansai Centry Separator)), a supernatant (about 55 L) was obtained.
- Another batch was performed in the same manner, and the Tochu leaf extract was combined to obtain a solution of about 110 L.
- mice 4 weeks old, body weight 20-25 g were divided into 5 groups (5 mice in each group) so that the average values of body weight were equal in each group.
- Table 1 shows the composition of the feed.
- the mixing ratio of the feed is shown in Table 1, with the ratio of the water fraction, fraction A, fraction B, fraction C, and methanol fraction being 100% and the ratio based on the weight of each fraction. It was blended as an alternative feed in 10% of the conical starch.
- the first group is 10% of the extract of dried persimmon Nakaba water
- the second group is 0.82% of fraction A
- the third group is 0.41% of fraction B
- the fourth group is fraction C. 0.15%
- group 5 received a high fat diet (control) adjusted with corn starch as a sample for 4 weeks. During the test, food and water were freely consumed.
- each dried extract of Nakabayashi water extract, fraction koji, and fraction koji were weighed and dissolved in 50% methanol solution.
- the components contained in the test solution were aucubin, asperuloside, geniposidic acid and chlorogenic acid as standard substances.
- Analytical method is HPLC (LC-6: manufactured by Shimadzu Corporation), column: YMC— Pack ODS-A A-312 6.
- Omm X l 50mm manufactured by YMC
- detector UV detector (measurement wavelength: 215nm), flow rate: lmlZmin.
- test solution 1.5 g each of dried kashiwa leaf extract, fraction A and fraction B were weighed and added to 500 mL of distilled water and stirred to obtain a test solution.
- the test solution was sealed in a transparent sealed container and stored at 40 ° C for 2 weeks.
- the test solution was evaluated by visual evaluation with the test solution and the absorbance at wavelengths of OD560 and OD720 using a spectrophotometer (UV-1200: manufactured by Shimadzu Corporation).
- a water extract was prepared in the same manner as in Example 1 using 577. 6 g of dried tochu-nakaba, and concentrated to dryness to obtain an aqueous extract (267.4 g) as a solid.
- the water extract was dissolved in water, and fractions eluted first from the column as a 30% aqueous methanol fraction in a column packed with Diaion HP20 by the same method as in Example 1 (Fraction D: 17.28 g ) And the later eluting fraction (fraction E: 3.78 g).
- Fraction E was purified by preparative HPLC (column: Chromatrex ODS; eluent: 15% aqueous methanol solution) to obtain Asperal mouth side (2001. 5 mg).
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Abstract
[PROBLEMS] To provide: a fractionation method for extracting an ingredient, particularly a pharmacologically active ingredient such as an iridoid compound, from an Eucommia ulmoides oliver leaf with good efficiency; a fractionation product of an Eucommia ulmoides oliver leaf, wherein the fractionation product contains a specific component in a large concentration; and an anti-obesity agent, composition for oral ingestion, pharmaceutical composition, food composition, pharmaceutical or food which comprises a natural material as a raw material, produces little adverse side effects, and is safe even when ingested over a long period. [MEANS FOR SOLVING PROBLEMS] Disclosed is a fractionation product of an aqueous extract of an Eucommia ulmoides oliver leaf. The fractionation product can be produced by: adsorbing an aqueous extract of an Eucommia ulmoides oliver leaf onto a reverse-phase synthetic adsorbent, wherein the aqueous extract is prepared from a dried Eucommia ulmoides oliver leaf; washing the adsorbent with water; and eluting the fractionation product with a 5-80 vol% aqueous methanol solution. Also disclosed is a pharmaceutical or food having an anti-obesity activity, which comprises the fractionation product.
Description
明 細 書 Specification
杜仲葉水抽出物の分画物、および当該分画物を含む抗肥満剤 技術分野 The fraction of Tochu Nakaha extract and anti-obesity agent containing the fraction
[0001] 本発明は、杜仲葉の水抽出物分画物、および当該分画物を含む抗肥満剤、経口 摂取用組成物、医薬組成物、食品組成物、医薬および食品に関する。さらに本発明 は、当該分画物の製造方法に関する。 TECHNICAL FIELD [0001] The present invention relates to a water extract fraction of Tochu Nakaba, and an anti-obesity agent, a composition for oral consumption, a pharmaceutical composition, a food composition, a medicine and a food containing the fraction. Furthermore, the present invention relates to a method for producing the fraction.
背景技術 Background art
[0002] 杜仲（Eucommia ulmoides oliver)は、中国中央部起源のトチュウ科トチュウ属のー 科ー属一種に分類される落葉性木本類で、榭高が 20mに達する喬木である。杜仲 は、一般にお茶と称するツバキ科の植物と比較し、カフェインを全く含んでいないほ 力 含有物も異なる。杜仲葉は、 1980年代から飲料としての用途が普及している。杜 仲の榭皮は医薬品として取り扱われており、中国では「高血圧症、腰痛、関節痛、腎 臓病、肝臓病、ストレス、精力減退、利尿困難、物忘れ」に有効な漢方薬として利用さ れている。 [0002] Eucommia ulmoides oliver is a deciduous woody plant that is classified as a genus of the genus Eucommia from Central China, and has a height of 20m. Tonaka is different from the camellia plant, generally called tea, in that it contains no caffeine. Tochu Nakaba has been widely used as a beverage since the 1980s.杜 Naka scabbard is treated as a pharmaceutical and is used in China as an effective Chinese medicine for “hypertension, low back pain, joint pain, kidney disease, liver disease, stress, loss of energy, diuresis difficulty, and forgetfulness”.
[0003] 天然物由来の食品や漢方薬は、一般に副作用が少ないなどの利点を有することか ら、近年において発生が増加している生活習慣病に対してのその有用性が注目され ている。上述の杜仲に関しても、杜仲葉の成分のリパーゼ阻害活性について検討し た例も 、くつかの報告がされて 、る（特許文献 1〜5を参照)。 [0003] Foods derived from natural products and traditional Chinese medicines have advantages such as generally having few side effects, and thus their usefulness against lifestyle-related diseases, which have been increasing in recent years, has attracted attention. As for the above-mentioned Tochu, there have been several reports on the investigation of the lipase inhibitory activity of Tonaka leaf components (see Patent Documents 1 to 5).
[0004] 特許文献 1：特開 2005— 289950号公報 [0004] Patent Document 1: Japanese Patent Laid-Open No. 2005-289950
特許文献 2 :特開 2005— 289951号公報 Patent Document 2: JP-A-2005-289951
特許文献 3 :特開 2003— 342185号公報 Patent Document 3: Japanese Patent Laid-Open No. 2003-342185
特許文献 4 :特開 2002— 179586号公報 Patent Document 4: Japanese Patent Laid-Open No. 2002-179586
特許文献 5：特開 2002— 275077号公報 Patent Document 5: Japanese Patent Laid-Open No. 2002-275077
発明の開示 Disclosure of the invention
発明が解決しょうとする課題 Problems to be solved by the invention
[0005] 杜仲葉に含まれる成分のうちゲ-ポシド酸などのイリドイドィ匕合物と薬効との関連が 指摘されている。したがって、杜仲葉の薬効成分を効率よく摂取するために、杜仲葉
力 効率よくイリドイドィ匕合物を取り出すための方法が求められて 、る。 [0005] Among the components contained in Tochu Naka, the relationship between iridoid compounds such as geposide acid and medicinal effects has been pointed out. Therefore, in order to ingest the medicinal properties of Tochu Nakaba efficiently, Tochu Nakaba There is a need for a method for efficiently removing iridoidic compounds.
[0006] したがって、本発明は、杜仲葉の成分、特にイリドイドィ匕合物などの薬効成分を効 率的に取り出すための分画方法、および特定の成分を高濃度で含有する杜仲葉成 分の分画物を提供することを目的とする。 [0006] Therefore, the present invention provides a fractionation method for efficiently extracting components of Tochu Naka leaf, particularly medicinal components such as iridoidoid compounds, and Tonaka leaf component containing a specific component at a high concentration. The purpose is to provide a fraction.
[0007] さらに本発明は、天然の素材を原料とし、副作用が少なく長期にわたって摂取した 場合でも安全である抗肥満剤、経口摂取用組成物、医薬組成物、食品組成物、医 薬および食品を提供することを目的とする。 [0007] Furthermore, the present invention relates to an anti-obesity agent, composition for oral intake, pharmaceutical composition, food composition, medicine and food, which is made of natural materials as raw materials and has little side effects and is safe even when ingested over a long period of time. The purpose is to provide.
課題を解決するための手段 Means for solving the problem
[0008] 本発明者は、上記の課題解決のために鋭意研究を進めたところ、杜仲葉成分の特 定の分画物に、高度の抗肥満作用を見いだし、本発明を完成させた。 [0008] As a result of diligent research to solve the above-mentioned problems, the present inventor found a high anti-obesity effect in a specific fraction of Tochu Nakaba component and completed the present invention.
すなわち本発明の一つの側面によれば、乾燥杜仲葉から得られる杜仲葉水抽出物 を逆相の合成吸着剤に吸着させ、水で洗浄後、 5〜80容積％メタノール水溶液で溶 離させる工程を含む製造方法により得られる、杜仲葉水抽出物分画物が提供される 。本発明の 1つの態様において、ここで、前記メタノール水溶液は、例えば 10容積％ 以上 40容積％未満、好ましくは 20〜35容積％、より好ましくは 25〜35容積％のメタ ノール水溶液で合ってもよぐ例えば 30容積％のメタノール水溶液を用いることがで きる。本発明の別の態様において、前記メタノール水溶液は、例えば 40〜60容積％ 、好ましくは 45〜55容積0 /0のメタノール水溶液であってもよぐ例えば 50容積0 /0のメ タノール水溶液を用いることができる。 That is, according to one aspect of the present invention, the step of adsorbing an extract of dried Nakanaka water obtained from dried Nakanaka to a reverse-phase synthetic adsorbent, washing with water, and then dissolving with a 5 to 80% by volume aqueous methanol solution. A foliage extract of Tochu Nakaba water obtained by a production method comprising: In one embodiment of the present invention, the methanol aqueous solution may be a methanol aqueous solution of 10% by volume or more and less than 40% by volume, preferably 20 to 35% by volume, more preferably 25 to 35% by volume. For example, a 30% by volume methanol aqueous solution can be used. In another aspect of the present invention, the aqueous methanol solution, for example 40 to 60% by volume, preferably using Yogu example 50 volumes 0/0 of methanol aqueous solution be an aqueous methanol solution of 45-55 volume 0/0 be able to.
[0009] 本発明の別の側面によれば、溶媒を留去した後の固形成分として、イリドイドィ匕合 物を 10〜90重量％含む、本発明として既に定義した杜仲葉水抽出物分画物が提 供される。 [0009] According to another aspect of the present invention, the fraction of the Nakanaka leaf water extract already defined as the present invention, comprising 10 to 90% by weight of an iridoidic compound as a solid component after distilling off the solvent. Is provided.
さらに、本発明の別の態様によれば、溶媒を留去した後の固形成分として、ァスぺ ルロサイドを、例えば 10重量％以上、好ましくは 20%以上、より好ましくは 30%以上 、さらに好ましくは 40%以上（例えば 10〜70重量％、好ましくは 20〜60重量％、より 好ましくは 30〜60重量％)含む、本発明として既に定義した杜仲葉水抽出物分画物 が提供される。 Furthermore, according to another aspect of the present invention, asperuloside is, for example, 10% by weight or more, preferably 20% or more, more preferably 30% or more, and still more preferably as a solid component after the solvent is distilled off. Is provided as a fraction of the extract of Satsunaka leaf water already defined as the present invention containing 40% or more (for example, 10 to 70% by weight, preferably 20 to 60% by weight, more preferably 30 to 60% by weight).
[0010] さらに、本発明の別の側面によれば、前記乾燥杜仲葉が、杜仲生葉を蒸熱するェ
程;杜仲葉を攪拌および zまたは揉圧しながら乾燥する工程;および杜仲葉に対して 遠赤外線を照射することにより杜仲葉を乾燥する工程を含む製造方法により得られる 、本発明として既に定義した杜仲葉水抽出物分画物が提供される。 [0010] Further, according to another aspect of the present invention, the dried bonito leaves steamed bonito leaves. Obtained by a production method comprising the steps of drying and stirring the zhongyou leaves with z or pressure; and irradiating the kungyou leaves with far infrared rays; Leaf water extract fractions are provided.
[0011] さらに、本発明の別の側面によれば、本発明として既に定義した杜仲葉水抽出物 分画物を含む抗肥満剤抗肥満剤が提供される。 [0011] Furthermore, according to another aspect of the present invention, there is provided an antiobesity agent and antiobesity agent comprising a fraction of a foliage extract already defined as the present invention.
さらに、本発明の別の側面によれば、本発明として既に定義した抗肥満剤を含む医 薬および食品が提供される。前記食品は、特に限定はされないが、例えば、機能性 食品、健康食品、健康補助食品、栄養補助食品、保険機能食品、特定保険用食品 または栄養機能食品であってもよ!、。 Furthermore, according to another aspect of the present invention, there are provided a medicine and a food containing the anti-obesity agent already defined as the present invention. The food is not particularly limited, and may be, for example, a functional food, a health food, a health supplement, a nutritional supplement, an insurance function food, a specific insurance food or a nutrition function food.
[0012] さらに、本発明の別の側面によれば、杜仲葉水抽出物分画物の製造方法であって 、乾燥杜仲葉から得られる杜仲葉水抽出物を逆相の合成吸着剤に吸着させ、水で 洗浄後、 5〜80容積％メタノール水溶液で溶離させる工程を含む、前記方法が提供 される。 [0012] Furthermore, according to another aspect of the present invention, there is provided a method for producing a fraction extracted from a dried nakanaka leaf, wherein the extracted nakanaka leaf water extract is adsorbed on a synthetic adsorbent in reverse phase. And washing with water followed by elution with a 5-80% by volume aqueous methanol solution.
[0013] さらに、本発明の別の側面によれば、得られる杜仲葉水抽出物分画物がイリドイド 化合物を 10〜90重量％含む本発明として既に定義した杜仲葉水抽出物分画物の 製造方法が提供される。 [0013] Further, according to another aspect of the present invention, the obtained Nakanaka leaf water extract fraction contains a 10 to 90% by weight of an iridoid compound, and is already defined as the present invention. A manufacturing method is provided.
[0014] さらに、本発明の別の側面によれば、ァスペル口サイドを、例えば 10重量％以上、 好ましくは 20%以上、より好ましくは 30%以上、さらに好ましくは 40%以上（例えば 1 0〜70重量0 /0、好ましくは 20〜60重量0 /0、より好ましくは 30〜60重量0 /0)含む、固 体の杜仲葉水抽出物分画物が提供される。 [0014] Further, according to another aspect of the present invention, the ispel mouth side is, for example, 10% by weight or more, preferably 20% or more, more preferably 30% or more, and further preferably 40% or more (for example, 10 to 10%). 70 weight 0/0, preferably from 20 to 60 weight 0/0, more preferably 30 to 60 weight 0/0), Eucommia leaf water extract fraction of the solid body is provided.
発明の効果 The invention's effect
[0015] 本発明により、杜仲葉水抽出物の分画物はイリドイドィ匕合物を高濃度に含むため、 当該化合物を摂取するための医薬、食品の製造において有用である。さらに本発明 に係る抗肥満剤は、天然の素材を原料とし、長期にわたって安全に摂取することが できるため患者に負担が少なぐ安定した抗肥満効果を得ることができる。 [0015] According to the present invention, the fraction of Tochu Nakaba extract contains an iridoidic compound at a high concentration, and is therefore useful in the manufacture of a medicine or food for ingesting the compound. Furthermore, since the anti-obesity agent according to the present invention is a natural material and can be safely ingested over a long period of time, a stable anti-obesity effect with less burden on the patient can be obtained.
本発明の具体的な態様 Specific embodiments of the present invention
[0016] 以下、本発明をさらに具体的に説明する。 [0016] Hereinafter, the present invention will be described more specifically.
本発明の分画物に含まれるイリドイド化合物としては、例えば杜仲葉に含まれる配
糖体成分であるイリドイドィ匕合物が挙げられる。その具体例には、例えば、ゲ-ポシド 酸、ァスペル口サイド、ァスペル口サイド酸（asperulosidic acid)、デァセチルァス ペル口サイド酸、スカンドサイド 10— O—アセテート、オークビンなどが含まれる。 Examples of the iridoid compound contained in the fraction of the present invention include, for example, those contained in Tochu Nakaba. Examples include iridoid compounds that are saccharide components. Specific examples thereof include geposide acid, asperculoside, asperulosidic acid, diacetyl persulfate, scandoside 10-O-acetate, oakbin and the like.
[0017] 本発明における杜仲葉水抽出物は、例えば乾燥杜仲葉を使用して調製される。当 該乾燥杜仲葉は、特には限定されないが、例えば杜仲生葉を特定の工程に付すこと により調製されうる。ここで、杜仲生葉は、収穫後乾燥前の杜仲葉を意味するもので あり、栽培により生産されたものであっても天然より採取されたものであってもよい。例 えば、当年葉で落葉前の生葉を用い、採取時期は 4月から 10月、好ましくは 5月から 8月、より好ましくは 7月力 8月までの生葉を用いることができる。 [0017] The chunaka leaf water extract in the present invention is prepared using, for example, dried chunaka leaf. The dry licorice leaf is not particularly limited, but can be prepared, for example, by subjecting licorice leaf to a specific process. Here, the bamboo shoot leaves mean the bamboo leaves before harvest and before drying, and may be produced by cultivation or collected from nature. For example, fresh leaves before fallen leaves of the current year can be used, and fresh leaves can be used from April to October, preferably from May to August, more preferably from July to August.
[0018] 本発明の杜仲生葉は、そのまま用いてもよいが、裁断したものを用いてもよい。従つ て、本願発明は、杜仲生葉を裁断する工程をさらに含んでいてもよい。杜仲生葉は、 例えば 5〜30mm程度、好ましくは 10〜20mm程度の幅に切断して用いてもよい。 好ましくは、本発明においては裁断されていない杜仲生葉が用いられる。裁断されて いない杜仲生葉を利用することにより、その後の乾燥工程において、緩や力な乾燥 が可能となり、乾燥中に葉が崩れることによる歩留まりの低下、および杜仲葉の変色 を抑制することができる。 [0018] The cocoon leaves of the present invention may be used as they are, or may be cut. Therefore, the present invention may further include a step of cutting the green leaves.杜中生 葉 may be cut into a width of, for example, about 5 to 30 mm, preferably about 10 to 20 mm. In the present invention, unbroken cocoon leaves are preferably used. By using the uncut green leaves, it becomes possible to dry gently and gently in the subsequent drying process, and it is possible to suppress the yield drop and the discoloration of the green leaves during the drying. .
[0019] 本発明における杜仲生葉の蒸熱工程は、市販されて!ヽる蒸し機またはオートクレー ブなどを用いて、当該技術分野で通常行われている方法により実施することができる 。例えば、ネットコンベア上に杜仲生葉を広げ、ボイラーから供給される無圧蒸気を 充満させた処理室を通過させることにより、杜仲生葉を蒸熱処理することができる。例 えば、宫村鉄工株式会社製、給葉機、地上型 1500およびネットコンベア、送帯式 10 00などを用いることができる。蒸熱温度は、杜仲葉の大きさに応じて、例えば 90〜1 20°C、好ましくは 95〜110°C、より好ましくは 100〜110°Cの範囲で適宜選択されう る。また蒸熱時間も、 10〜240秒間、好ましくは 20〜180秒間、より好ましくは 20〜1 20秒間の範囲で適宜選択されうる。また、使用する蒸気量は、例えば 200〜70LZ 分、好ましくは 170〜： L00LZ分の範囲で適宜選択されうる。蒸し葉の処理量は、生 葉の水分率に応じて、例えば 3〜： LOkgZ分、好ましくは 4〜8kgZ分、より好ましくは 5〜7kgZ分の範囲で適宜選択されうる。この蒸熱工程は、杜仲葉を褐色に変色さ
せる酵素が失活することにより杜仲葉の緑色が保たれやすくなる；および、杜仲葉が 柔らかくなることで、蒸熱工程の後の杜仲葉を攪拌および Zまたは揉圧しながら乾燥 する工程の実施が容易になる、などの効果をもたらす。 [0019] The steaming process of the cocoon leaves in the present invention can be carried out by a method usually performed in the technical field using a commercially available steamer or an autoclave. For example, it is possible to steam heat-treat cocoon leaves by spreading them on a net conveyor and passing them through a treatment chamber filled with non-pressure steam supplied from a boiler. For example, Kashimura Tekko Co., Ltd., leaf feeder, ground type 1500, net conveyor, trolley type 100, etc. can be used. The steaming temperature may be appropriately selected within the range of, for example, 90 to 120 ° C., preferably 95 to 110 ° C., more preferably 100 to 110 ° C., depending on the size of Tochu Nakaba. The steaming time can also be appropriately selected within the range of 10 to 240 seconds, preferably 20 to 180 seconds, more preferably 20 to 120 seconds. The amount of steam used can be appropriately selected within the range of, for example, 200 to 70 LZ, preferably 170 to L00LZ. The treatment amount of the steamed leaves can be appropriately selected in the range of, for example, 3 to: LO kgZ, preferably 4 to 8 kgZ, more preferably 5 to 7 kgZ, depending on the moisture content of the fresh leaves. This steaming process discolored Tochu Naka to brown Inactivation of the enzyme that makes it easy to maintain the green color of the Nakanaka leaves; and the softness of the Nakanaka leaves makes it easy to perform the process of drying the Nakanaka leaves after the steaming process with stirring and Z or under pressure The effect of becoming.
[0020] 蒸熱処理された杜仲葉は、そのまま次の工程に使用することもできる力 冷却後に 次の工程で使用することもできる。ここでの冷却は、送風などにより荒熱を取り除くこと により行われうる。 [0020] The steamed and heat-treated Tochu Nakaba can also be used in the next step as it is. It can also be used in the next step after cooling. The cooling here can be performed by removing rough heat by blowing air or the like.
[0021] 本発明において、杜仲葉を攪拌および Zまたは揉圧しながら乾燥する工程は、例 えば、市販されている連続式葉打機、回転式葉打機、回分型葉打機または粗揉機な どを用いて、当該技術分野で通常行われている方法により実施することができる。例 えば市販の葉打機としては、カワサキ機工株式会社製、葉打機（回分型) 60K、 90Κ 、 120Kおよび 180Kなどを用いることができる。例えば、本工程における揉圧は、適 当な弾性を有する板パネで支えられた「より手」が葉打機内で回転し、処理胴の壁面 に杜仲葉を押さえつけることにより行われる。また、本工程における攪拌は、葉打機 に取り付けられた「葉ざらい」が回転することにより行われる。本工程おける揉圧は、 緩やかに行うのが好ましぐ例えば葉ざらいの回転のみで行ってもよい。乾燥方法は 特に限定されないが、好ましくは杜仲葉に熱風を送ることにより行われる。ここで熱風 の温度は、特に限定されないが、例えば 70〜120°C、好ましくは 75〜110°Cの範囲 から適宜選択されうる。また本工程に要する時間は、 10〜60分間、好ましくは 15〜5 0分間、より好ましくは 20〜40分間の範囲で適宜選択されうる。例えば本工程は、 10 0°Cで 20〜30分間行うことができる。本工程により、杜仲葉各部分の水分を均一に 保ちつつ効率よく杜仲葉が乾燥される。また本工程における攪拌および Zまたは揉 圧により、杜仲葉に含まれる糖質、脂質などの粘性物質が杜仲葉から分離され、その 結果得られる杜仲茶の「えぐ味」および「青臭さ」が低減される。本工程は、好ましくは 、水分の杜仲葉表面力 の蒸散速度と杜仲葉内部での水分拡散速度が平衡となる ように行われる。また、得られる杜仲茶の「えぐ味」および「青臭さ」を低減するために 、葉打ち機内の密封性が高いほうが好ましい。このような条件を保ちながら行うことに より、杜仲葉表面がしめった状態を保ち、杜仲葉の表面温度を一定範囲内に保つこ とができ、杜仲生葉の変色を抑制しつつ乾燥させることが可能となる。ここで、本工程
における乾燥時の杜仲茶葉表面温度は、例えば 30〜60°C、好ましくは 40〜50°Cで ある。本工程を経て得られる杜仲葉の水分量は、例えば乾量基準で 30〜45%、好 ましくは 30〜40%、より好ましくは 30〜35%である。 [0021] In the present invention, the step of drying the rice cake with stirring and Z or pressure is, for example, a commercially available continuous leaf cutter, rotary leaf cutter, batch-type leaf cutter or rough rice cutter. Can be carried out by a method commonly used in the art. For example, as a commercially available leaf cutter, leaf cutters (batch type) 60K, 90 機, 120K, and 180K manufactured by Kawasaki Kiko Co., Ltd. can be used. For example, the crushing pressure in this process is performed by a “more hand” supported by a panel panel having an appropriate elasticity rotating in the leaf cutter and pressing the corrugated leaf against the wall of the processing cylinder. In addition, the stirring in this step is performed by rotating the “leaf crust” attached to the leaf cutter. The rolling pressure in this step is preferably performed gently, for example, by only rotating the leaves. The drying method is not particularly limited, but is preferably performed by sending hot air to Tochu Nakaba. Here, the temperature of the hot air is not particularly limited, but may be appropriately selected from the range of, for example, 70 to 120 ° C, preferably 75 to 110 ° C. The time required for this step can be appropriately selected within the range of 10 to 60 minutes, preferably 15 to 50 minutes, more preferably 20 to 40 minutes. For example, this step can be performed at 100 ° C. for 20-30 minutes. By this step, the Nakanaka leaves are efficiently dried while keeping the moisture in each part of the Nakanaka leaves uniform. In addition, due to the stirring and Z or pressure in this process, sugars, lipids, and other viscous substances contained in Tochu Naka are separated from Tochu Naka, and the resulting “Egu taste” and “Blue odor” of Tochu tea are reduced. Is done. This step is preferably performed so that the transpiration rate of the surface strength of the water of the Nakanaka leaf and the moisture diffusion rate inside the Nakanaka leaf are in equilibrium. In addition, in order to reduce the “egu taste” and “blue odor” of the resulting Tochu tea, it is preferable that the sealing performance in the leaf cutter is high. By carrying out while maintaining these conditions, the surface of the nakanaka leaf can be maintained, the surface temperature of the nakanaka leaf can be kept within a certain range, and drying can be performed while suppressing discoloration of the nakanaka leaf. It becomes possible. Here, this process The surface temperature of Tochu tea leaves during drying is, for example, 30 to 60 ° C, preferably 40 to 50 ° C. The water content of Tochu Nakaba obtained through this step is, for example, 30 to 45%, preferably 30 to 40%, more preferably 30 to 35% on a dry basis.
[0022] 本発明にお 、ては、「杜仲葉を攪拌および Zまたは揉圧しながら乾燥する工程」と「 杜仲葉を乾燥する工程」の間に、杜仲葉の水分を均一化する工程が含まれていても よい。本発明において、杜仲葉中の水分を均一化する工程は、例えば市販されてい る揉捻機、粗揉機または中揉機を用いて、当該技術分野で通常行われている方法 により実施することができる。例えば市販の揉捻機としては、株式会社寺田製作所製 、揉捻機 60Kg型などを用いることができる。本工程における杜仲葉中の水分の均一 化は、例えば、揉捻機の揉捻盤と回転胴の間に杜仲葉が挟まれ、かつ揉捻盤により 加圧されると同時に回転胴が回転することにより行われる。杜仲葉は葉肉、葉脈、葉 軸の順に乾燥するので、例えば葉肉の乾燥度が十分な場合でも葉軸にはまだ余分 な水分が残っている。従って、本工程により、杜仲葉中の水分が均一に整えられ、部 分乾燥による粉体ィ匕が抑制されるのと同時に、乾燥に要する時間を短縮することが できる。本工程は、必要の応じて加熱下で行うこともできる力 好ましくは加熱せずに 行われる。また本工程に要する時間は、 10〜80分間、好ましくは 20〜60分間、より 好ましくは 30〜45分間の範囲で適宜選択されうる。例えば本工程は、常温で 40分 間行うことができる。本工程中に揉捻盤による加圧がなされる力 工程開始時の無加 圧時間は、 0〜10分間、好ましくは 2〜8分間、より好ましくは 4〜5分間の範囲で適 宜選択されうる。本工程を経て得られる杜仲葉の水分量は、例えば乾量基準で 25〜 40%、好ましくは 25〜35%である。 [0022] The present invention includes a step of homogenizing the moisture of the chunaka leaf between "the step of drying the chunaka leaf with stirring and Z or pressure" and "the step of drying the chunaka leaf". It may be. In the present invention, the step of homogenizing the water in the bamboo leaf can be carried out by a method usually performed in the technical field using, for example, a commercially available twister, coarser, or intermediater. For example, as a commercially available twister, Terada Seisakusho Co., Ltd., a twister 60 kg type can be used. The homogenization of the water in the cocoon leaf in this process is performed, for example, by sandwiching the cocoon leaf between the turret and the rotating drum of the turret and pressurizing with the rotator while rotating the rotator. Is called. Since the Tochu leaves are dried in the order of mesophyll, vein, and leaf shaft, for example, even if the dryness of the leaf meat is sufficient, excess moisture still remains on the leaf shaft. Therefore, according to this step, the moisture in the bamboo leaf is uniformly prepared, and the powdery wrinkles due to partial drying are suppressed, and at the same time, the time required for drying can be shortened. This step can be performed with heating, if necessary, preferably without heating. The time required for this step can be appropriately selected within the range of 10 to 80 minutes, preferably 20 to 60 minutes, more preferably 30 to 45 minutes. For example, this process can be performed at room temperature for 40 minutes. The force applied by the scissors during this process The no-pressing time at the start of the process can be appropriately selected in the range of 0 to 10 minutes, preferably 2 to 8 minutes, more preferably 4 to 5 minutes. . The moisture content of the chunaka leaf obtained through this step is, for example, 25 to 40%, preferably 25 to 35% on a dry basis.
[0023] 本発明に「杜仲葉中の水分を均一化する工程」が含まれる場合、杜仲葉を乾燥す る工程の前に、追加の「杜仲葉を攪拌および Zまたは揉圧しながら乾燥する工程」お よび「杜仲葉中の水分を均一化する工程」、または「杜仲葉を攪拌および Zまたは揉 圧しながら乾燥する工程」が含まれて 、てもよ 、。これらの工程を繰り返すことにより、 不要な脂質などがさらに取り除かれた杜仲茶葉を得ることができる。 [0023] When the present invention includes "a step of homogenizing moisture in the chunaka leaf", an additional "step of drying the chunaka leaf with stirring and Z or under pressure before the step of drying the chunaka leaf. And “the step of homogenizing the water in the Tochu leaf”, or “the step of drying the Tochu leaf with stirring and Z or pressure” may be included. By repeating these steps, it is possible to obtain Tochu tea leaves from which unnecessary lipids have been further removed.
[0024] 「杜仲葉を攪拌および Zまたは揉圧しながら乾燥する工程」を追加する場合、当該 工程は上述の方法および条件で行うことができ、熱風の温度は、特に限定されない
1S 例えば 50〜110°C、好ましくは 55〜105°Cの範囲力も適宜選択されうる。また本 工程に要する時間は、 5〜45分間、好ましくは 10〜40分間、より好ましくは 10〜35 分間の範囲で適宜選択されうる。例えば 70°Cで 20〜30分間行うことができる。 [0024] In the case of adding a "step of drying and stirring and stirring Z or under pressure", the step can be performed by the method and conditions described above, and the temperature of the hot air is not particularly limited. 1S For example, a range force of 50 to 110 ° C., preferably 55 to 105 ° C. may be appropriately selected. The time required for this step can be appropriately selected within the range of 5 to 45 minutes, preferably 10 to 40 minutes, more preferably 10 to 35 minutes. For example, it can be performed at 70 ° C for 20 to 30 minutes.
[0025] 「杜仲葉中の水分を均一化する工程」を追加する場合、当該工程は上述の方法お よび条件で行うことができ、また本工程に要する時間は、 10〜80分間、好ましくは 20 〜60分間、より好ましくは 30〜45分間の範囲で適宜選択されうる。例えば常温で 40 分間行うことができる。 [0025] In the case of adding "a step of homogenizing moisture in Tochu-nakaba", the step can be performed by the above-mentioned method and conditions, and the time required for this step is 10 to 80 minutes, preferably It can be appropriately selected within a range of 20 to 60 minutes, more preferably 30 to 45 minutes. For example, it can be performed at room temperature for 40 minutes.
[0026] 本発明の杜仲葉を乾燥する工程は、例えば、市販されている乾燥機を用いて当該 技術分野で通常行われている方法により実施することができる。本工程における乾燥 方法は、特に限定はされないが、例えば、搬送コンベア上の杜仲葉を、熱風発生器 による熱風で満たされた高温の乾燥室内を移動させることにより行うことができる。例 えば、株式会社寺田製作所製、乾燥機 ND120型により行われうる。ここで熱風の温 度は、特に限定されないが、例えば 70〜100°C、好ましくは 85〜95°Cの範囲力も適 宜選択されうる。また本工程に要する時間は、 5〜80分間、好ましくは 10〜70分間、 より好ましくは 20〜80分間の範囲で適宜選択されうる。本工程を経て得られる杜仲 葉の水分量は、例えば水分率 5%以下、好ましくは水分率 3%以下、より好ましくは水 分率 2%以下である。 [0026] The step of drying the Tochu leaf of the present invention can be carried out, for example, by a method commonly performed in the technical field using a commercially available dryer. Although the drying method in this process is not specifically limited, For example, it can carry out by moving the Tochu Naka leaf on a conveyance conveyor in the high temperature drying chamber filled with the hot air by a hot air generator. For example, it can be performed by a dryer ND120 manufactured by Terada Manufacturing Co., Ltd. Here, the temperature of the hot air is not particularly limited, but a range force of, for example, 70 to 100 ° C., preferably 85 to 95 ° C. may be appropriately selected. The time required for this step can be appropriately selected within the range of 5 to 80 minutes, preferably 10 to 70 minutes, more preferably 20 to 80 minutes. The water content of the bamboo leaf obtained through this step is, for example, a water content of 5% or less, preferably a water content of 3% or less, more preferably a water content of 2% or less.
[0027] 本発明においては、杜仲葉に対して遠赤外線を照射することにより杜仲葉を乾燥 する工程を含んでいてもよい。当該工程は、特に限定はされないが、例えば市販され ている遠赤外線ヒーターを用いて行うことができる。例えば、山益製作所株式会社製 、 VR型により行われうる。ここで照射される遠赤外線の波長は、例えば 1〜： LOOO /z m、好ましくは 2. 5〜50 μ m、より好ましくは 3〜30 μ mの範囲から適宜選択される。 乾燥中の照射設定温度は、例えば 100〜400°C、好ましくは 150〜350°C、より好ま しくは 200〜300°Cの範囲の範囲より適宜選択されうる。また本工程に要する時間は 、赤外線ランプ通過速度として 30〜60秒間、好ましくは 40〜55秒間、より好ましくは 45〜50秒間の範囲で適宜選択されうる。本工程を経て得られる乾燥杜仲葉の水分 量は、例えば水分率 5%以下、好ましくは水分率 3%以下、より好ましくは水分率 2% 以下である。
[0028] 本明細書において杜仲葉水抽出物は、乾燥杜仲葉 lkgに対して、例えば 5〜50k g、好ましくは 10〜30kg、より好ましくは 15〜20kg力 適宜選択される量の水が用 いることができる。抽出温度は、例えば 85〜98°C、好ましくは 90〜95°Cの範囲から 適宜選択されうる。抽出時間は、特に限定はされないが、例えば 10〜120分、好まし くは 20〜90分、より好ましくは 30〜60分力 適宜選択されうる。 [0027] The present invention may include a step of drying the chunaka leaf by irradiating the chunaka leaf with far infrared rays. Although this process is not specifically limited, For example, it can be performed using the commercially available far-infrared heater. For example, it can be performed by a VR type manufactured by Yamamasu Seisakusho Co., Ltd. The wavelength of the far infrared rays irradiated here is appropriately selected from the range of, for example, 1 to: LOOO / zm, preferably 2.5 to 50 μm, more preferably 3 to 30 μm. The irradiation set temperature during drying can be appropriately selected from the range of, for example, 100 to 400 ° C, preferably 150 to 350 ° C, more preferably 200 to 300 ° C. The time required for this step can be appropriately selected within the range of 30 to 60 seconds, preferably 40 to 55 seconds, and more preferably 45 to 50 seconds as the infrared lamp passing speed. The moisture content of the dried bamboo leaf obtained through this step is, for example, a moisture content of 5% or less, preferably a moisture content of 3% or less, more preferably a moisture content of 2% or less. [0028] In the present specification, the nakanaka leaf water extract uses, for example, 5 to 50 kg, preferably 10 to 30 kg, more preferably 15 to 20 kg force, of water appropriately selected for 1 kg of dried nakanaka leaf. Can be. The extraction temperature can be appropriately selected from the range of, for example, 85 to 98 ° C, preferably 90 to 95 ° C. The extraction time is not particularly limited, but can be appropriately selected, for example, 10 to 120 minutes, preferably 20 to 90 minutes, more preferably 30 to 60 minutes.
[0029] 抽出液の濾過は、例えば、ざる、または 30〜200メッシュのフィルターなどを用いて 行われうる。濾液は濃縮を行う前に一定時間静置してもよい。静置することにより発生 する沈殿物を除去することにより、不要物を取り除くことができる。静置する時間は、 特に限定はされないが、例えば 1〜24時間、好ましくは 6〜20時間、より好ましくは 8 〜18時間から適宜選択されうる。静置する際の温度は、特に限定はされないが、例 えば 0〜35°C、好ましくは 0〜16°C、より好ましくは 2〜8°C力も適宜選択されうる。 [0029] Filtration of the extract may be performed using, for example, a filter or a 30-200 mesh filter. The filtrate may be allowed to stand for a certain period before concentration. Unnecessary substances can be removed by removing precipitates generated by standing. The standing time is not particularly limited, but may be appropriately selected from, for example, 1 to 24 hours, preferably 6 to 20 hours, and more preferably 8 to 18 hours. The temperature at the time of standing is not particularly limited. For example, a force of 0 to 35 ° C, preferably 0 to 16 ° C, more preferably 2 to 8 ° C can be appropriately selected.
[0030] こうして得られる杜仲葉抽出液をそのまま使用することもできるが、遠心分離に付し て生じる沈殿を除去した後に得られる上澄みを次の工程に使用することもできる。さ らに、当該上澄み液を濃縮して使用することもできる。 [0030] The soot extract obtained in this way can be used as it is, but the supernatant obtained after removing the precipitate generated by centrifugation can also be used in the next step. Further, the supernatant can be used after being concentrated.
[0031] 本発明で使用される「逆相の合成吸着剤」は、天然成分の分離などに通常使用さ れるものであれば特に限定されないが、ポリスチレンゲル（ポリスチレン'ジビニルべ ンゼン共重合体など）、例えば、 MCIGEL CHP10M/CHP2MGM, SEPABE [0031] The "reverse-phase synthetic adsorbent" used in the present invention is not particularly limited as long as it is usually used for separation of natural components, etc., but is not limited to polystyrene gel (polystyrene'divinylbenzene copolymer, etc.). ), For example, MCIGEL CHP10M / CHP2MGM, SEPABE
HP2MGY/SP207/SP825/SP850/SP70/SP700, Diaion HP20/H P21ZHP2MGなどが挙げられ、工業的スケールにおける製造の観点力 好ましく は Diaion HP20が使用される。当該吸着剤は、例えばカラムの担体として使用する ことができる。使用される吸着剤の量は、杜仲葉抽出液 110Lに対して、例えば 1000 0〜 18000g、好まし <は 15000〜 18000gの範囲力も選択されうる。 HP2MGY / SP207 / SP825 / SP850 / SP70 / SP700, Diaion HP20 / H P21ZHP2MG, and the like. Manufacturing viewpoints on an industrial scale Preferably Diaion HP20 is used. The adsorbent can be used as a column carrier, for example. The amount of adsorbent used can be selected, for example, from 1000 to 18000 g, preferably <15000 to 18000 g, per 110 L of Tochu leaf extract.
[0032] 本発明の 1つの態様において、逆相の吸着剤を充填させたカラムに杜仲葉抽出液 を注入し、その後水を溶出液として使用して溶出する成分を除去し、さらにその後に 5〜80容積％のメタノール水溶液を溶離液として使用して、当該カラムより本発明の 分画物を溶離させることができる。ここで、溶出液として使用する水の量は特には限 定されないが、例えば、吸着剤 17200g対して、 70〜： L 10Lの範囲力 選択される量
で使用することができる。 [0032] In one embodiment of the present invention, the Tochu leaf extract is injected into a column packed with a reverse-phase adsorbent, and then the eluted components are removed using water as the eluent. The fraction of the present invention can be eluted from the column using an aqueous solution of ˜80% by volume of methanol as an eluent. Here, the amount of water used as the eluent is not particularly limited. For example, for an adsorbent of 17200 g, a range force of 70 to: L 10 L is selected. Can be used in
[0033] 上記態様にぉ ヽて、溶離液として使用するメタノール水溶液は、例えば 10容積％ 以上 40容積％未満のメタノール水溶液、好ましくは 15〜30容積％のメタノール水溶 液を使用することができる。また、 15〜30容積％のメタノール水溶液 (例えば 30容積 %のメタノール水溶液）を使用した後に、 40〜60容積％のメタノール水溶液 (例えば 50容積％のメタノール水溶液)を使用することもできる。この態様において、各々のメ タノール水溶液は、特には限定されないが、例えば、吸着剤 17200g対して、 70Lの 範囲から選択される量を使用することができる。さらに、当該メタノール水溶液による 溶離物を分取することにより、目的の成分を高濃度で含むより好ましい分画物を得る ことができる。 [0033] In the above embodiment, the methanol aqueous solution used as the eluent may be, for example, a methanol aqueous solution of 10% by volume or more and less than 40% by volume, preferably 15-30% by volume of methanol aqueous solution. Moreover, after using 15-30 volume% methanol aqueous solution (for example, 30 volume% methanol aqueous solution), 40-60 volume% methanol aqueous solution (for example, 50 volume% methanol aqueous solution) can also be used. In this embodiment, each aqueous methanol solution is not particularly limited. For example, an amount selected from the range of 70 L can be used for 17200 g of the adsorbent. Furthermore, a more preferable fraction containing the target component at a high concentration can be obtained by fractionating the eluate from the aqueous methanol solution.
[0034] 水—メタノール溶液として得られる分画物は、好ましくは、濃縮して使用される。濃 縮率は特に限定されないが、例えば容積比で 60%以下であってよぐ好ましくは 30 %以下であり、さらに好ましくは乾固して得られる固体物として使用される。また当該 濃縮は常圧下または減圧下の 、ずれにぉ ヽても行われうるが、好ましくは減圧下で 行われる。濃縮方法は、通常使用される方法であれば特に限定されず、例えばロー タリーエバポレーターなどを使用して濃縮することができる。 [0034] The fraction obtained as a water-methanol solution is preferably used after being concentrated. The concentration ratio is not particularly limited. For example, the volume ratio is 60% or less, preferably 30% or less, and more preferably used as a solid product obtained by drying. Further, the concentration can be carried out under normal pressure or under reduced pressure, but is preferably carried out under reduced pressure. The concentration method is not particularly limited as long as it is a commonly used method, and for example, it can be concentrated using a rotary evaporator or the like.
[0035] 本明細書で用いられる用語「抗肥満剤」とは、特に限定はされないが、例えば、高 血圧症、高脂血症、糖尿病の効果を得るために投与される薬剤を意味する。 [0035] The term "anti-obesity agent" used in the present specification is not particularly limited, but means, for example, a drug administered to obtain the effects of hypertension, hyperlipidemia, and diabetes.
本発明の抗肥満剤は、特に限定はされないが、肥満の改善のために使用されうる 他の薬剤、抗脂血症の予防剤および治療剤、糖尿病の予防剤および治療剤、なら びに高血圧など治療剤または予防剤とともに使用されうる。 The anti-obesity agent of the present invention is not particularly limited, but other agents that can be used to improve obesity, preventive and therapeutic agents for antilipidemia, preventive and therapeutic agents for diabetes, hypertension, etc. Can be used with therapeutic or prophylactic agents.
[0036] 本発明の抗肥満剤は、医薬組成物の有効成分として使用することができる。当該 医薬組成物は、種々の剤形、例えば、経口投与のためには、錠剤、カプセル剤、散 剤、顆粒剤、丸剤、液剤、乳剤、懸濁液、溶液剤、酒精剤、シロップ剤、エキス剤、ェ リキシル剤などとすることができ、例えば、局所投与のためにはクリーム、ゼリー、ゲル 、ペースト、軟膏などとすることができるが、これらには限定されない。当該医薬組成 物は、一般に用いられる各種成分を含みうるものであり、例えば、 1種もしくはそれ以 上の薬学的に許容され得る賦形剤、崩壊剤、希釈剤、滑沢剤、着香剤、着色剤、甘
味剤、矯味剤、懸濁化剤、湿潤剤、乳化剤、分散剤、補助剤、防腐剤、緩衝剤、結 合剤、安定剤、コーティング剤等を含みうる。また本発明の医薬組成物は、持続性ま たは徐放性剤形であってもよ!/ヽ。 [0036] The anti-obesity agent of the present invention can be used as an active ingredient of a pharmaceutical composition. The pharmaceutical composition can be used in various dosage forms such as tablets, capsules, powders, granules, pills, solutions, emulsions, suspensions, solutions, spirits, syrups for oral administration. For example, cream, jelly, gel, paste, ointment and the like can be used for topical administration, but not limited thereto. The pharmaceutical composition may contain various commonly used ingredients, such as one or more pharmaceutically acceptable excipients, disintegrants, diluents, lubricants, flavoring agents. , Colorant, sweet Flavoring agents, flavoring agents, suspending agents, wetting agents, emulsifying agents, dispersing agents, adjuvants, preservatives, buffering agents, binders, stabilizers, coating agents and the like can be included. The pharmaceutical composition of the present invention may be in a sustained or sustained release dosage form!
[0037] 本発明の抗肥満剤の投与量は、患者の体型、年齢、体調、疾患の度合い、発症後 の経過時間等により、適宜選択することができ、本発明の医薬組成物は、治療有効 量および Zまたは予防有効量の抗肥満剤を含むことができる。例えば本発明の杜仲 葉粉砕物またはその水抽出物として、一般に 10〜50000mg/日/成人、好ましく は 100〜5000mgZ日 Z成人の用量で使用される。当該医薬組成物の投与は、単 回投与または複数回投与であってもよぐたとえば他の抗肥満剤などの他の薬剤と組 み合わせて使用することもできる。 [0037] The dose of the anti-obesity agent of the present invention can be appropriately selected depending on the patient's body shape, age, physical condition, degree of disease, elapsed time after onset, etc. The pharmaceutical composition of the present invention is a therapeutic agent. An effective amount and Z or a prophylactically effective amount of an anti-obesity agent can be included. For example, it is generally used in the dose of 10 to 50000 mg / day / adult, preferably 100 to 5000 mg Z day Z adult, as the pulverized mash of the present invention or its water extract. Administration of the pharmaceutical composition can be single dose or multiple doses, for example, in combination with other drugs such as other anti-obesity agents.
[0038] 本発明に係る食品は、液体飲料および固形の食品を含む。当該食品は、医薬部外 品、他の飲食物などの成分、食品添加物などとして使用することができる。また本明 細書における経口摂取用組成物は、そのまま機能性食品として使用できるほか、医 薬品、医薬部外品、飲食物等の成分、食品添加物などとして使用することができる。 当該使用により、本発明の肥満改善効果および動脈硬化予防剤を有する当該食品 または経口摂取用組成物の日常的および継続的な摂取が可能となり、肥満の効果 的な改善、および肥満に関連する疾患 (例えば、高血圧症、高脂血症、糖尿病など） の効果的な予防が可能となる。 [0038] The food according to the present invention includes a liquid beverage and a solid food. The food can be used as quasi-drugs, other food and drink ingredients, food additives, and the like. In addition, the composition for ingestion in this specification can be used as a functional food as it is, and can be used as a component of a pharmaceutical, a quasi-drug, a food and drink, and a food additive. The use enables daily and continuous ingestion of the food or composition for oral consumption having the obesity-improving effect and arteriosclerosis-preventing agent of the present invention, effectively improving obesity, and obesity-related diseases. Effective prevention of (for example, hypertension, hyperlipidemia, diabetes, etc.) becomes possible.
[0039] 本発明の抗肥満剤を含む食品または飲料の例としては、リパーゼ阻害効果もしくは 肥満抑制効果を有する機能性食品、健康食品、健康補助食品、栄養補助食品 (栄 養ドリンク等)、保険機能食品、特定保険用食品、栄養機能食品、一般食品 (ジユー ス、菓子、加工食品等)などが含まれる。本明細書における食品または飲料は、任意 の添加物として、鉄およびカルシウムなどの無機成分、種々のビタミン類、オリゴ糖お よびキトサンなどの食物繊維、大豆抽出物などのタンパク質、レシチンなどの脂質、 ショ糖および乳糖などの糖類、アスパルテーム、アセスルファムカリウム、ステビア、ソ ゥマチン、サッカリン、サッカリンナトリウムなどの甘味料 '矯味料を含むことができる。 実施例 [0039] Examples of foods or beverages containing the anti-obesity agent of the present invention include functional foods having lipase-inhibiting effects or obesity-inhibiting effects, health foods, health supplements, nutritional supplements (nutrient drinks, etc.), insurance This includes functional foods, foods for specified insurance, functional foods for nutrition, general foods (diuse, confectionery, processed foods, etc.). The food or beverage in the present specification includes, as optional additives, inorganic components such as iron and calcium, various vitamins, dietary fibers such as oligosaccharides and chitosan, proteins such as soybean extract, lipids such as lecithin, Sugars such as sucrose and lactose, sweeteners such as aspartame, acesulfame potassium, stevia, sumatin, saccharin, sodium saccharin and the like can be included. Example
[0040] 以下、本発明の好適な実施例についてさらに詳細に説明する力 本発明はこれら
の実施例に限定されるものではない。 [0040] In the following, the power to explain the preferred embodiments of the present invention in more detail. However, the present invention is not limited to these examples.
[0041] [実施例 1] 合成吸着剤による乾燥杜仲葉水抽出物分画物の調製 [0041] [Example 1] Preparation of a dried koji-nakaba water extract fraction using a synthetic adsorbent
乾燥杜仲葉は、特開 2005— 1287469号公報の実施例 4の記載に基づいて製造 される乾燥杜仲葉を使用した。 As dried dried Nakanaka, dried dried Nakanaka manufactured according to the description in Example 4 of JP-A-2005-1287469 was used.
[0042] 乾燥杜仲葉（10kg)にイオン交換水 (70L)を加え、 65°Cで 7時間加熱した。加熱 後、一晩放置した。ざる (テトロン 3号)を使用して杜仲葉残渣を除去した後に、連続 遠心分離を行！、 (遠心加速度： 9340xg； (S型超高速遠心分離機 U— 6— H：関西遠 心分離機製作所社製)）、上澄み液 (約 55L)を得た。同様の手法でもう 1バッチ行い 、杜仲葉抽出物を合わせて約 110Lの溶液として得た。 [0042] Ion-exchanged water (70 L) was added to dried potato Nakaba (10 kg) and heated at 65 ° C for 7 hours. After heating, it was left overnight. Use Zaru (Tetron No.3) to remove the Tochu Nakaba residue, and then perform continuous centrifugation! (Centrifugal acceleration: 9340xg; (S-type ultra-high-speed centrifuge U-6-H: manufactured by Kansai Centenary Separator)), a supernatant (about 55 L) was obtained. Another batch was performed in the same manner, and the Tochu leaf extract was combined to obtain a solution of about 110 L.
[0043] 得られた溶液を、 Diaion HP20を充填したカラム (^ l35xJ^1200mm)に注 入し、その後さらに 70Lの水を使用して、水により溶出される成分を除去し、水画分を 得た。その後、 30容積％メタノール水溶液 (70L)を使用して溶離した画分 (以下、画 分 Aとも称する）、 50容積％メタノール水溶液 (70L)を使用して溶離した画分 (以下、 画分 Bとも称する）、 80容積％メタノール水溶液 (70L)を使用して溶離した画分 (以 下、画分 Cとも称する）および 100容積％メタノール（70L)を使用して溶離したメタノ 一ル画分を得た。いずれも画分も減圧下 (0. 5kPa)、 65°Cで乾固するまで濃縮し、 水画分(4520§)、画分八(432. Og)、画分 B (215. 4g)、画分 C (76. 7g)およびメ タノール画分（2. 4g)を 、ずれも固体物として得た。 [0043] The obtained solution was poured into a column (^ l35xJ ^ 1200mm) packed with Diaion HP20, and then 70L of water was used to remove the components eluted by water, and the water fraction was separated. Obtained. Then, the fraction eluted using 30% by volume methanol aqueous solution (70L) (hereinafter also referred to as fraction A) and the fraction eluted using 50% by volume methanol aqueous solution (70L) (hereinafter fraction B) The fraction eluted with 80% by volume aqueous methanol (70L) (hereinafter also referred to as fraction C) and the methanol fraction eluted with 100% by volume methanol (70L). Obtained. All fractions were concentrated to dryness under reduced pressure (0.5 kPa) at 65 ° C, water fraction (4520 § ), fraction eight (432.Og), fraction B (215.4g), Fraction C (76.7 g) and methanol fraction (2.4 g) were also obtained as solids.
[0044] [実施例 2] 乾燥杜仲葉水抽出エキスの調製 [0044] [Example 2] Preparation of extract of dried bamboo leaf extract
乾燥杜仲葉は、特開 2005— 1287469号公報の実施例 4の記載に基づいて製造 される乾燥杜仲葉を使用した。乾燥杜仲葉 (2. 3kg)にイオン交換水（16L)を加え、 65°Cで 7時間加熱した。加熱後、一晩放置した。ざる (テトロン 3号)を使用して杜仲 葉残渣を除去した後に、連続遠心分離を行!ヽ (遠心加速度： 9340xg； S型超高速遠 心分離機 U -6-H :関西遠心分離機製作所社製)、上澄み液 (約 12L)を得た。 As dried dried Nakanaka, dried dried Nakanaka manufactured according to the description in Example 4 of JP-A-2005-1287469 was used. Ion-exchanged water (16 L) was added to dried potato Nakaba (2.3 kg) and heated at 65 ° C for 7 hours. After heating, it was left overnight. Use Zaru (Tetron No. 3) to remove Tonaka leaf residue, and then perform continuous centrifugation! ヽ (centrifugal acceleration: 9340xg; S-type ultra-high speed centrifuge U-6-H: Kansai centrifuge ), And a supernatant (about 12 L) was obtained.
[0045] 得られた溶液を、減圧下 (0. 5kPa)、 65°Cで乾固するまで濃縮し、乾燥杜仲葉水 抽出エキス (652g)を固体として得た。 [0045] The obtained solution was concentrated under reduced pressure (0.5 kPa) to 65 ° C to dryness to obtain a dried persimmon Nakaba water extract (652 g) as a solid.
[0046] [実施例 3]杜仲葉水抽出分画物の抗肥満効果試験 [0046] [Example 3] Anti-obesity effect test of Tochu leaf extract
(1)実験材料および飼料の調製
ICR系雌性マウスに、牛脂と杜仲葉水抽出分画物を配合した高脂肪食を摂取させ 、体重、内臓脂肪重量、血液中の中性脂肪及び総コレステロールに対する影響を調 ベた。 (1) Preparation of experimental materials and feed An ICR female mouse was ingested with a high-fat diet containing beef tallow and persimmon leaf extract, and the effects on body weight, visceral fat weight, neutral fat in blood and total cholesterol were examined.
[0047] 具体的には、 ICR系雌性マウス (4週齢、体重 20〜25g)を体重の平均値が各群等 しくなるように 5群に分けた (各群 5匹)。 [0047] Specifically, ICR female mice (4 weeks old, body weight 20-25 g) were divided into 5 groups (5 mice in each group) so that the average values of body weight were equal in each group.
実施例 1と同様の方法により各種画分を調製した。飼料の組成を表 1に示す。飼料 の配合割合は、水画分、画分 A、画分 B、画分 Cおよびメタノール画分の重量の合計 を 100%として各画分の重量をもとに比率を求め、表 1に示す飼料組成物であるコ一 ンスターチ 10%に代替飼料として配合した。 Various fractions were prepared in the same manner as in Example 1. Table 1 shows the composition of the feed. The mixing ratio of the feed is shown in Table 1, with the ratio of the water fraction, fraction A, fraction B, fraction C, and methanol fraction being 100% and the ratio based on the weight of each fraction. It was blended as an alternative feed in 10% of the conical starch.
[0048] 第 1群は乾燥杜仲葉水抽出エキスが 10%、第 2群は画分 Aが 0. 82%、第 3群は画 分 Bが 0. 41%、第 4群は画分 Cが 0. 15%、第 5群はサンプルとしてコーンスターチ で調整した高脂肪食 (コントロール)を 4週間投与した。なお試験中は、餌及び水は自 由摂取とした。 [0048] The first group is 10% of the extract of dried persimmon Nakaba water, the second group is 0.82% of fraction A, the third group is 0.41% of fraction B, and the fourth group is fraction C. 0.15%, group 5 received a high fat diet (control) adjusted with corn starch as a sample for 4 weeks. During the test, food and water were freely consumed.
[0049] 上記飼料を投与して力も 4週間後、体重を測定した後に、マウスをエーテル麻酔に より屠殺し、心臓より採血を行って、血清中の中性脂肪、総コレステロールを酵素法 を用いて測定した。また開腹後、内臓脂肪重量を秤量により測定した。全ての測定値 は、平均士標準偏差で示した。摂取期間における体重及び摂餌量の変動、摂取 4週 間目における群間での体重、内臓脂肪重量及び血中脂質については対応のない t 検定を行った。 [0049] Four weeks after the administration of the above-mentioned feed, the body weight was measured, the mice were sacrificed by ether anesthesia, blood was collected from the heart, and neutral fat and total cholesterol in the serum were measured using an enzymatic method. Measured. After laparotomy, the visceral fat weight was measured by weighing. All measured values are shown in average standard deviation. Uncorresponding t-tests were conducted for changes in body weight and food intake during the intake period, body weight between groups, visceral fat weight, and blood lipids during the fourth week of intake.
[0050] [表 1] [0050] [Table 1]
表 1 . 飼料の組成 （単位： g ) Table 1. Composition of feed (unit: g)
[0051] (2)結果
結果を表 2に示す。乾燥杜仲葉水抽出エキス、画分 A及び画分 Bを添加した群は、 コントロールと比べ体重、内臓脂肪重量、中性脂肪、総コレステロールが低値を示し た。画分 Cにおいては、コントロールに比べ内臓脂肪重量、中性脂肪及び総コレステ ロールが低値を示すことが確認された。乾燥杜仲葉水抽出エキスと各画分を比較し たところ、画分 A及び画分 Bは乾燥杜仲葉水抽出エキスとほぼ同様の挙動を示した。 [0051] (2) Results The results are shown in Table 2. The group to which the dried kashiwa leaf extract, fraction A and fraction B were added showed lower body weight, visceral fat weight, neutral fat and total cholesterol than the control. In fraction C, it was confirmed that the visceral fat weight, neutral fat and total cholesterol were lower than those in the control. Comparing each fraction with the dried bamboo shoot extract, fraction A and fraction B showed almost the same behavior as the dried nakanaka extract.
[0052] [表 2] [0052] [Table 2]
表 2 . 摂取 4週間目における群間での体重、 内臓脂肪重量、 中性脂肪、 総コレステロール Table 2. Body weight between groups, visceral fat weight, neutral fat, total cholesterol at 4 weeks of intake
[0053] [実施例 4] 杜仲葉水抽出物分画物の含有成分 [0053] [Example 4] Constituents in the fraction of Tochu Nakaha extract
(1)試験方法 (1) Test method
試験は、乾燥杜仲葉水抽出エキス、画分 Αおよび画分 Βを各 lOOmg秤量し、 50% メタノール液に溶かし供試した。試験液の含有成分は、ァゥクビン (aucubin)、ァス ぺノレ口サイド (asperuloside)、ゲ-ポシド酸 (geniposidic acid)およびクロロゲン酸 (chlorogenic acid)を標準物質として用いた。分析方法は、 HPLC (LC— 6 :島津 製作所社製）を用いて、カラム： YMC— Pack ODS-A A— 312 6. Omm X l 50mm (YMC社製）、移動層：水ZメタノールZリン酸=870Zl30Zl、カラム温度 :40°C、検出器: UV検出器 (測定波長： 215nm)、流速： lmlZmin. として、試料溶 液を注入し、クロマトグラムを得て、各指標成分のピーク面積から含量を求めた。 In the test, each dried extract of Nakabayashi water extract, fraction koji, and fraction koji were weighed and dissolved in 50% methanol solution. The components contained in the test solution were aucubin, asperuloside, geniposidic acid and chlorogenic acid as standard substances. Analytical method is HPLC (LC-6: manufactured by Shimadzu Corporation), column: YMC— Pack ODS-A A-312 6. Omm X l 50mm (manufactured by YMC), moving bed: water Z methanol Z phosphorus Acid = 870Zl30Zl, column temperature: 40 ° C, detector: UV detector (measurement wavelength: 215nm), flow rate: lmlZmin. Inject sample solution, obtain chromatograms, and obtain peak area of each indicator component The content was determined.
[0054] (2)結果 [0054] (2) Results
結果を表 3に示す。 The results are shown in Table 3.
[0055] [表 3] [0055] [Table 3]
表 3 試験液の含有成分の定量 Table 3 Determination of components in test solution
定量物質 （mg g) Quantitative substance (mg g)
ァゥクビン ゲェポシド酸 ァスペル口サイド クロロゲン酸 乾燥杜仲葉水抽出エキス 148. 9 65. 2 44. 6 58.8 面分 A 12. 9 16. 9 445. 9 32. 0 画分 B 検出せず 検出せず 12. 0 3. 4 画分 C 検出せず 検出せず 検出せず 検出せず
[0056] [実施例 5] 杜仲葉水抽出物分画物の色調変化試験 Wakbin Geeposidic acid Asper mouth side Chlorogenic acid Extracted extract of dried nakanaka water 148. 9 65. 2 44. 6 58.8 Area A 12. 9 16. 9 445. 9 32. 0 Fraction B Not detected Not detected 12. 0 3.4 Fraction C Not detected Not detected Not detected Not detected [0056] [Example 5] Color tone change test of fraction extracted from Tochu Nakaha extract
(1)試験方法 (1) Test method
試験溶液は、乾燥杜仲葉水抽出エキス、画分 Aおよび画分 Bをそれぞれ 1. 5g秤 取り、 500mLの蒸留水に加え攪拌し試験液とした。試験溶液は、透明の密封容器に 封入し 40°C下の環境下で 2週間保管した。試験液の評価は、試験溶液での目視評 価と分光高度計 (UV— 1200 :島津製作所社製）により吸光度を OD560および OD7 20の波長で測定を行った。 For the test solution, 1.5 g each of dried kashiwa leaf extract, fraction A and fraction B were weighed and added to 500 mL of distilled water and stirred to obtain a test solution. The test solution was sealed in a transparent sealed container and stored at 40 ° C for 2 weeks. The test solution was evaluated by visual evaluation with the test solution and the absorbance at wavelengths of OD560 and OD720 using a spectrophotometer (UV-1200: manufactured by Shimadzu Corporation).
[0057] (2)結果 [0057] (2) Results
結果を表 4に示す。 The results are shown in Table 4.
[0058] [表 4] [0058] [Table 4]
試験液の絰時変化 Change in test solution over time
[0059] [実施例 6] 杜仲葉水抽出物分画物のからのァスペル口サイドの単離 [0059] [Example 6] Isolation of asperal mouth side from fraction of Tochu Nakaha extract
乾燥杜仲葉 577. 6gを使用して、実施例 1と同様の手法により水抽出液を調製し、 乾固するまで濃縮して、水抽出物（267. 4g)を固体として得た。当該水抽出物を水 に溶解し、実施例 1と同様の手法により Diaion HP20を充填したカラムで 30%メタ ノール水溶液画分として、カラムから先に溶離した画分 (画分 D : 17. 28g)および後 に溶離した画分 (画分 E： 3. 78g)の 2種類の分画物を得た。 A water extract was prepared in the same manner as in Example 1 using 577. 6 g of dried tochu-nakaba, and concentrated to dryness to obtain an aqueous extract (267.4 g) as a solid. The water extract was dissolved in water, and fractions eluted first from the column as a 30% aqueous methanol fraction in a column packed with Diaion HP20 by the same method as in Example 1 (Fraction D: 17.28 g ) And the later eluting fraction (fraction E: 3.78 g).
[0060] 画分 Dをシリカゲルカラムクロマトグラフィー（溶離液 CHC13 : MeOH = 20 : l→9 [0060] Fraction D was subjected to silica gel column chromatography (eluent CHC13: MeOH = 20: l → 9
: 1)で精製し、ァスペル口サイド（275. 3mg)を得た。 : Purified in 1) to obtain the Aspel mouth side (275. 3 mg).
画分 Eを分取 HPLC (カラム： Chromatrex ODS；溶離液： 15%メタノール水溶液 )により精製し、ァスペル口サイド（2001. 5mg)を得た。
Fraction E was purified by preparative HPLC (column: Chromatrex ODS; eluent: 15% aqueous methanol solution) to obtain Asperal mouth side (2001. 5 mg).
Claims
請求の範囲 The scope of the claims
[I] 乾燥杜仲葉から得られる杜仲葉水抽出物を逆相の合成吸着剤に吸着させ、水で 洗浄後、 5〜80容積％メタノール水溶液で溶離させる工程を含む製造方法により得 られる、杜仲葉水抽出物分画物。 [I] Tochu, which is obtained by a production method comprising a step of adsorbing a Tochu Nakaba extract obtained from dried Tochu leaves on a synthetic adsorbent in reverse phase, washing with water and eluting with a 5 to 80% by volume aqueous methanol solution. Leaf water extract fraction.
[2] 溶媒を留去した後の固形成分として、イリドイドィ匕合物を 10〜90重量％含む、請求 項 1に記載の杜仲葉水抽出物分画物。 [2] The nakanaka leaf water extract fraction according to claim 1, comprising 10 to 90% by weight of an iridoid compound as a solid component after the solvent has been distilled off.
[3] 溶媒を留去した後の固形成分として、ァスペル口サイドを 10〜70重量％含む、請 求項 1に記載の杜仲葉水抽出物分画物。 [3] The foliage extract of Tochu-naka water according to claim 1, comprising 10 to 70% by weight of Asper mouth side as a solid component after the solvent is distilled off.
[4] 前記乾燥杜仲葉が、杜仲生葉を蒸熱する工程;杜仲葉を攪拌および Zまたは揉圧 しながら乾燥する工程;および杜仲葉に対して遠赤外線を照射することにより杜仲葉 を乾燥する工程を含む製造方法により得られる、請求項 1〜3のいずれか 1項に記載 の杜仲葉水抽出物分画物。 [4] A process in which the dried dried leaves are steamed with dried leaves; dried dried with stirring and Z or under pressure; and dried dried leaves by irradiating the dried leaves with far infrared rays. A foliage extract of Tochu leaf extract according to any one of claims 1 to 3, obtained by a production method comprising:
[5] 前記メタノール水溶液力 10容積％以上 40容積％未満のメタノール水溶液である[5] Methanol aqueous solution power 10% by volume or more and less than 40% by volume of methanol aqueous solution
、請求項 1に記載の杜仲葉水抽出物分画物。 2. A fraction extracted from the Tochu leaf extract according to claim 1.
[6] 前記メタノール水溶液力 40〜60容積％メタノール水溶液である、請求項 1に記載 の杜仲葉水抽出物分画物。 [6] The foliage extract of Tochu leaf extract according to claim 1, wherein the methanol aqueous solution power is 40 to 60 vol% methanol aqueous solution.
[7] 請求項 1〜6のいずれか 1項に記載の杜仲葉水抽出物分画物を含む、抗肥満剤。 [7] An anti-obesity agent comprising the fraction of the Nakanaka leaf water extract according to any one of claims 1 to 6.
[8] 請求項 7に記載の抗肥満剤を含む医薬。 [8] A medicament comprising the anti-obesity agent according to claim 7.
[9] 請求項 7に記載の抗肥満剤を含む食品。 [9] A food comprising the anti-obesity agent according to claim 7.
[10] 機能性食品、健康食品、健康補助食品、栄養補助食品、保険機能食品、特定保 険用食品または栄養機能食品である、請求項 9に記載の食品。 [10] The food according to claim 9, which is a functional food, a health food, a health supplement, a nutritional supplement, an insurance functional food, a specified insurance food or a functional nutrition food.
[II] 杜仲葉水抽出物分画物の製造方法であって、 [II] A method for producing a fraction of Tochu Nakaha water extract,
乾燥杜仲葉から得られる杜仲葉水抽出物を逆相の合成吸着剤に吸着させ、水で 洗浄後、 5〜80容積％メタノール水溶液で溶離させる工程を含む、前記方法。 The method comprising the steps of: adsorbing an extract of chunaka leaf water obtained from dried chunaka leaf on a reverse-phase synthetic adsorbent, washing with water, and eluting with 5 to 80% by volume methanol aqueous solution.
[12] 得られる杜仲葉水抽出物分画物力イリドイドィ匕合物を 10〜90重量％含む、請求項 11に記載の方法。 [12] The method according to claim 11, comprising 10 to 90% by weight of the resulting licorice leaf extract fraction strength iridoid compound.
[13] ァスペル口サイドを 10〜70重量％含む、固体の杜仲葉水抽出物分画物。
[13] A solid fraction of extract of Nakanaka leaf water containing 10 to 70% by weight of Asper mouth side.
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| JP2006-058657 | 2006-03-03 | ||
| JP2006058657A JP5088846B2 (en) | 2006-03-03 | 2006-03-03 | A fraction of Tochu Nakaha extract and an anti-obesity agent containing the fraction |
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| WO2007102438A1 true WO2007102438A1 (en) | 2007-09-13 |
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| PCT/JP2007/054083 WO2007102438A1 (en) | 2006-03-03 | 2007-03-02 | Fractionation product of aqueous extract of eucommia ulmoides oliver leaf, and anti-obesity agent comprising the fractionation product |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012518A (en) * | 2012-12-14 | 2013-04-03 | 湘西自治州奥瑞克医药化工有限责任公司 | Production process for simultaneously extracting asperuloside and chlorogenic acid from folium cortex eucommiae |
| CN104435068A (en) * | 2014-11-28 | 2015-03-25 | 普正药业股份有限公司 | Eucommia ulmoides composition with antiobesity effect and preparation of eucommia ulmoides composition |
| CN107249582A (en) * | 2015-02-25 | 2017-10-13 | 小林制药株式会社 | Orally administered composition |
| CN107951921A (en) * | 2018-01-12 | 2018-04-24 | 郑州中科新兴产业技术研究院 | A kind of method that flavones is extracted in the powder from eucommia Bark male flower |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5588134B2 (en) * | 2009-08-07 | 2014-09-10 | 小林製薬株式会社 | Capsule film |
| JP5561984B2 (en) * | 2009-09-29 | 2014-07-30 | 小林製薬株式会社 | New beverage |
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| JPH0363231A (en) * | 1989-08-02 | 1991-03-19 | Hitachi Zosen Corp | Extract originated from eucommia ulmoides |
| JPH04368336A (en) * | 1991-06-18 | 1992-12-21 | Hitachi Zosen Corp | Agent for inhibiting angiotensin converting enzyme activity originated from alphatochuyobeta extract |
| JPH10117748A (en) * | 1996-10-16 | 1998-05-12 | Shigeki Ishihara | Storage of tea leaf of totyuu and production of totyuu tea |
| JP2005289950A (en) * | 2004-03-31 | 2005-10-20 | Kobayashi Pharmaceut Co Ltd | Lipase inhibitor comprising water extraction component of eucommia ulmoides leaf |
| WO2005099488A1 (en) * | 2004-03-31 | 2005-10-27 | Kobayashi Pharmaceutical Co., Ltd. | Green du-zhong tea leaves and process for producing green du-zhong tea leaf powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0363231A (en) * | 1989-08-02 | 1991-03-19 | Hitachi Zosen Corp | Extract originated from eucommia ulmoides |
| JPH04368336A (en) * | 1991-06-18 | 1992-12-21 | Hitachi Zosen Corp | Agent for inhibiting angiotensin converting enzyme activity originated from alphatochuyobeta extract |
| JPH10117748A (en) * | 1996-10-16 | 1998-05-12 | Shigeki Ishihara | Storage of tea leaf of totyuu and production of totyuu tea |
| JP2005289950A (en) * | 2004-03-31 | 2005-10-20 | Kobayashi Pharmaceut Co Ltd | Lipase inhibitor comprising water extraction component of eucommia ulmoides leaf |
| WO2005099488A1 (en) * | 2004-03-31 | 2005-10-27 | Kobayashi Pharmaceutical Co., Ltd. | Green du-zhong tea leaves and process for producing green du-zhong tea leaf powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012518A (en) * | 2012-12-14 | 2013-04-03 | 湘西自治州奥瑞克医药化工有限责任公司 | Production process for simultaneously extracting asperuloside and chlorogenic acid from folium cortex eucommiae |
| CN104435068A (en) * | 2014-11-28 | 2015-03-25 | 普正药业股份有限公司 | Eucommia ulmoides composition with antiobesity effect and preparation of eucommia ulmoides composition |
| CN104435068B (en) * | 2014-11-28 | 2016-01-13 | 普正药业股份有限公司 | A kind of Cortex Eucommiae compositions and preparation thereof with antiobesity action |
| CN107249582A (en) * | 2015-02-25 | 2017-10-13 | 小林制药株式会社 | Orally administered composition |
| CN107951921A (en) * | 2018-01-12 | 2018-04-24 | 郑州中科新兴产业技术研究院 | A kind of method that flavones is extracted in the powder from eucommia Bark male flower |
Also Published As
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| JP2007238449A (en) | 2007-09-20 |
| JP5088846B2 (en) | 2012-12-05 |
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