JP6454266B2 - Highly white rosemary extract and method for producing the same - Google Patents

Description

  The present invention relates to a rosemary extract with high whiteness and a method for producing the same.

  Rosemary (Rosmarinus officinalis), an Lamiaceae plant, is an evergreen shrub with straight and aromatic leaves, and is generally known as a spice for flavoring meat, soups, stews, etc. It has been.

  Moreover, the extract of rosemary has a deodorizing effect (patent documents 1, 2), a wrinkle prevention effect (patent document 3), etc., and is mix | blended with food-drinks and cosmetics.

  Furthermore, rosemary contains triterpenic acid oleanolic acid, betulinic acid, ursolic acid and diterpenic acid carnosic acid. It is known that oleanolic acid, ursolic acid, and betulinic acid inhibit transcription factor NF-κB and are useful for diabetes, cardiovascular disease, atherosclerosis, etc. (Non-patent Document 1). Carnosic acid is known to promote the production of nerve growth factors that play an important role in the maintenance of nerve cells (Non-patent Documents 1 and 2).

  For this reason, many products that contribute to health and products that have been given a deodorizing effect by blending rosemary extract into foods and beverages and cosmetics have been provided.

  Patent Document 1 discloses a method for producing a rosemary extract in which the content of carnosol, which is a cause of bitterness that occurs when a rosemary extract is added to a food or drink such as chewing gum, is adjusted to 0.5% by mass or less. Is described. Patent Document 3 describes a method for producing a rosemary extract that can increase the content of ursolic acid having a wrinkle-preventing effect.

  However, according to the method of Patent Document 1, although carnosol, which is a bitter component, can be reduced, triterpenic acid useful for the living body may also be removed in the filtration step before spray drying. The content is insufficient to provide products that contribute to health. Moreover, in the method of patent document 3, the extract obtained is green, and a commercial value will fall when it adds to food-drinks or cosmetics.

  Thus, the conventional rosemary extract usually has a green color, and when added to foods and beverages and cosmetics, there is a problem that an undesirable color is generated and the commercial value is lowered. In addition, the conventionally known rosemary extract has a low content of triterpenic acid and carnosic acid useful for the living body, and therefore, when providing foods and drinks that contribute to health, there is a problem that the amount added is increased. there were.

JP 2008-29221 A Japanese Patent Laid-Open No. 9-238648 JP 2009-249306 A

Yadav. VR. Et al., Toxins (2010) 2 (10), p.2428-2466 Kosaka. K. and Yokoi T., Biol. Pharm. Bull., (2003) 26 (11): 1620-1622

  An object of the present invention is to provide a rosemary extract having high whiteness. Furthermore, an object of the present invention is to provide a rosemary extract having a high content of rosemary-derived carnosic acid and triterpenic acid.

  As a result of intensive studies to solve the above problems, the inventors of the present invention concentrated and precipitated an extract extracted from rosemary under a suitable condition using a lower alcohol, thereby producing a rosemary extract with high whiteness. It was found that can be obtained. Furthermore, the rosemary extract with high whiteness obtained by this production method has also been found to have a high content of carnosic acid and triterpenic acid, thus completing the present invention.

  That is, the present invention provides the following [1] to [11].

[1] A rosemary extract having a whiteness of 61 or more.

[2] The rosemary extract according to the above [1], wherein the carnosic acid content is 30 mg / g or more by dry weight.

[3] The rosemary extract according to the above [1] or [2], wherein the total triterpenic acid content is 300 mg / g or more by dry weight.

[4] It is prepared by a method comprising treating a rosemary plant or a part thereof with a lower alcohol at 45 ° C. to 70 ° C. to obtain an extract, concentrating it, and collecting the resulting precipitate. The rosemary extract according to any one of [1] to [3].

[5] The rosemary extract according to [4], wherein the method further includes washing the precipitate.

[6] An additive for foods, cosmetics or pharmaceuticals comprising the rosemary extract according to any one of [1] to [5].

[7] A food containing the rosemary extract according to any one of [1] to [5].

[8] A cosmetic comprising the rosemary extract according to any one of [1] to [5].

[9] A pharmaceutical comprising the rosemary extract according to any one of [1] to [5].

[10] The above-mentioned [1], comprising treating a rosemary plant or a part thereof with a lower alcohol at 45 ° C. to 70 ° C. to obtain an extract, concentrating it, and collecting the resulting precipitate. ] The manufacturing method of the rosemary extract in any one of [5].

[11] The method according to [10], further comprising washing the precipitate.

  According to the present invention, a rosemary extract having high whiteness and a high content of active ingredients such as carnosic acid and triterpenic acid can be provided.

  This specification includes the contents of Japanese Patent Application No. 2013-059133 which is the basis of the priority claim of the present application.

FIG. 1 is a flowchart for explaining an example of a process for producing a rosemary extract of the present invention.

  Hereinafter, embodiments of the present invention will be described. However, the modes described below are merely examples, and can be appropriately modified within a range obvious to those skilled in the art.

  The present invention relates to a method for obtaining a rosemary extract having high whiteness by concentrating and precipitating an extract extracted from rosemary using a lower alcohol. The high whiteness rosemary extract obtained by the process of the present invention also has a high carnosic acid content and total triterpenic acid content. The method for producing a rosemary extract having a high whiteness of the present invention is generally to extract a rosemary extract from a rosemary, for example, a dried product of rosemary leaves. In the present invention, a rosemary extract is obtained by a method comprising treating a rosemary plant or a part thereof with a lower alcohol to obtain an extract, concentrating it, and collecting the resulting precipitate. It is preferable. FIG. 1 is a flowchart for explaining a method for producing a rosemary extract of the present invention. As illustrated in FIG. 1, an example of a method for producing a rosemary extract with high whiteness includes an extraction step with a lower alcohol, a filtration / concentration step, a precipitate washing step, and a drying step. Yes. In the present invention, for example, the rosemary extract according to the present invention can be produced by concentrating an extract obtained by extracting a dried product of rosemary with a lower alcohol and washing the concentrate with purified water. it can.

  As a raw material of the rosemary extract with high whiteness of the present invention, a rosemary plant or a part thereof can be used. As a part of the plant body of rosemary, rosemary (Rosmarinus officinalis L.) leaves, branches, stems, combinations thereof, and the like are usually mentioned, but it is preferable to include leaves. The rosemary plant or a part thereof may be raw or dried. Rosemary leaves, particularly dried leaves, are more preferred as raw materials. When an extract is obtained using a rosemary leaf pulverized by, for example, pulverizing the raw material used in the present invention with a power mill, the whiteness is lowered. Therefore, in the present invention, a rosemary plant or a part thereof, particularly a rosemary Leaves are preferably used for extraction treatment using a lower alcohol without pulverization treatment. There are various origins of rosemary such as Albania, Morocco, and Spain, but the origin is not limited in the present invention.

  In the extraction step with a lower alcohol, a rosemary plant or a part thereof is treated with the lower alcohol to obtain an extract. For example, the extraction can be carried out by adding lower alcohol in a weight ratio of 1:10 to 1: 100 to a dried product of rosemary leaves. In the present invention, the lower alcohol means an alcohol having 5 or less carbon atoms, such as methanol, ethanol, propanol (1-propanol or 2-propanol), butanol (1-butanol, 2-methyl-1-propanol, 2- Butanol, 2-methyl-2-propanol), pentanol and the like. As the solvent in the extraction step, any of lower alcohols such as methanol, ethanol, propanol and butanol can be suitably used, and ethanol is more preferable among them. The lower alcohol may be an anhydrous alcohol or a hydrous alcohol. In the case of hydrous alcohol, the concentration is preferably 80% or more, more preferably 85% or more, and further preferably 90% or more. In the case of ethanol, a mixed solution with a small amount of water can be suitably used, and the ethanol concentration is preferably 80% or more, more preferably 85% or more, and further preferably 90% or more. For the purpose of further improving the whiteness, the concentration of the lower alcohol is particularly preferably 80% or more and less than 95%. For the purpose of increasing the carnosic acid content and the total triterpenic acid content, the lower alcohol concentration is preferably high, preferably 80% or more, more preferably 85% or more, and further preferably 90% or more.

  The extraction temperature and time in the extraction step with the lower alcohol can be appropriately adjusted in consideration of the whiteness and the extraction efficiency of carnosic acid and triterpenic acid, which are active ingredients. For example, in the case where 90% ethanol is used as the solvent in the extraction step and extraction is performed at a room temperature, the extraction treatment time is 1 or 2 hours or more, preferably 3 hours or more, more preferably 4 hours or more, and 24 hours. Within 18 hours, preferably within 18 hours, more preferably within 13 hours, it is possible from the viewpoint of whiteness because pigment outflow from rosemary leaves can be suppressed. In the method of the present invention, for the purpose of increasing the whiteness, the extraction temperature should be closer to room temperature, for example, 70 ° C. or less, more preferably 55 ° C. or less, for example, 5 ° C. to 55 ° C. On the other hand, for the purpose of further increasing the carnosic acid content, the extraction temperature should be higher, preferably 45 ° C. or higher, more preferably 60 ° C. or higher. For the purpose of further increasing the total triterpenic acid content, the extraction temperature should not be too high, preferably 70 ° C. or lower, more preferably 60 ° C. or lower. In the method of the present invention, it is possible to adjust the balance of carnosic acid content and total triterpenic acid content by adjusting the temperature and time of extraction. For example, for the purpose of increasing the content of carnosic acid while maintaining high whiteness, the extraction temperature with the lower alcohol (that is, the temperature of the lower alcohol used for the extraction treatment) is preferably 45 ° C. or higher, particularly 45 ° C. to 70 ° C. The extraction time in that case is not limited to the following, but for the purpose of obtaining an extract having a higher whiteness, it is preferably 1 to 24 hours, more preferably 1 to 18 hours, and still more preferably 1 to 13 It can be hours or 1-8 hours, for example 1-4 hours. For the purpose of increasing the total triterpenic acid content while maintaining high whiteness, the extraction temperature with the lower alcohol is preferably 60 ° C. or lower, for example, 30 ° C. to 55 ° C. Furthermore, for the purpose of increasing the carnosic acid content and the total triterpenic acid content in a balanced manner while maintaining high whiteness, the extraction temperature with the lower alcohol is preferably 45 ° C to 55 ° C. The extraction at 45 ° C. to 55 ° C. with a lower alcohol may be performed, for example, for 1 to 24 hours or 1 to 13 hours, preferably 1 to 8 hours, more preferably 1 to 4 hours, for example 2 hours. The extraction may be performed at a constant temperature from the start of extraction to the end of extraction, and may be heated or cooled stepwise.

  The normal temperature in the present invention is a temperature range of 20 ° C. ± 15 ° C. defined by Japanese Industrial Standard (JIS Z8703).

  In the extraction step with a lower alcohol, it is preferable to extract with stirring. The stirring conditions are not particularly limited. However, excessive stirring is not preferable because pigments from leaves of rosemary and the like are excessively extracted and the whiteness is lowered. In one embodiment, it is preferable to stir at, for example, 50 rpm to 300 rpm. In addition, when extracting without stirring, it is necessary to make extraction time longer.

  As described above, an extract can be prepared from rosemary using a lower alcohol.

  After the extraction step, the extract is concentrated and the resulting precipitate is recovered. It is also preferable to perform filtration prior to concentration of the extract. In such a filtration / concentration step, an unnecessary liquid component (such as impurities) can be removed by filtering the extract obtained in the extraction step using the lower alcohol. A filtration process can be performed by arbitrary filtration methods, such as filtration with a funnel, filtration with a filter paper or a filter. Alternatively, prior to concentration of the extract, the extract may be centrifuged to separate and remove solid components (such as contaminants).

  In the concentration step, the extract obtained above, or the filtrate obtained by filtering it, the supernatant obtained by centrifugation, and the like are concentrated until a sufficient amount of precipitate is produced. In the present invention, “concentration” means removing moisture to increase the concentration of the component, and is not limited to the following, but includes, for example, vacuum concentration and heat concentration.

  The collected precipitate can be used as it is as a rosemary extract, but may be further subjected to treatments such as filtration and washing. For example, it is also preferable to further remove unnecessary solid components (such as impurities) by suspending the precipitate in water or the like and filtering the precipitate. It is also preferable to wash the precipitate with a washing liquid. The cleaning liquid may be water (for example, purified water such as filtered water, distilled water, deionized water, ultrapure water, well water, spring water, ground water, etc.), a buffer solution, or the like. In the precipitate washing step, for example, the precipitate obtained in the previous filtration / concentration step can be washed with a washing liquid such as purified water. Or you may wash | clean a deposit with a washing | cleaning liquid directly. The cleaning liquid such as purified water used in the cleaning process may be heated at room temperature, but from the viewpoint of further increasing the whiteness, it is preferable to use a room temperature cleaning liquid. On the other hand, for the purpose of further increasing the content of carnosic acid while maintaining a certain degree of whiteness, a warmed cleaning solution, for example, a cleaning solution of 35 ° C. to 70 ° C., preferably 45 ° C. to 55 ° C., can also be used.

  The precipitate obtained as described above may be further dried. The drying method is not particularly limited, and any drying method can be used. For example, a method of placing under low humidity / high temperature conditions, a method of contacting dry air / high temperature dry air, a spray drying method, a freeze drying method Etc. The dried product may be powdered or solidified.

  The rosemary extract thus produced loses green to yellowish green color derived from the raw materials such as rosemary leaves, and exhibits a remarkably high whiteness. Therefore, the rosemary extract according to the present invention can be a useful material when added to other products in terms of whiteness. The whiteness of the rosemary extract according to the present invention is evaluated by Hunter whiteness in the L * a * b * color system. This whiteness is determined by measuring the L * a * b * value in the reflection mode using a spectrophotometer (for example, CM-5, manufactured by Konica Minolta) and calculating the whiteness (W). be able to. The calculation formula of whiteness used is described later in the examples. The rosemary extract of the present invention has a whiteness of 61 or more, preferably a whiteness of 70 or more, and more preferably a whiteness of 75 or more. If the whiteness of the rosemary extract of the present invention is 70 or more, even if it is added to a white product, the pigment derived from the rosemary extract does not affect the final product. The present invention also provides such a rosemary extract.

  The rosemary extract of the present invention not only has high whiteness, but also has an advantage that the total triterpenic acid content per 1 g of the extract is high. The “total triterpenic acid content” in the present invention means the total amount of betulinic acid, oleanolic acid, and ursolic acid contained in the rosemary extract. The total triterpenic acid content in the rosemary extract can be measured by a known method. For example, it can be measured using the triterpenic acid quantification method based on the HPLC method described in the examples described later. it can. The first feature of the rosemary extract of the present invention is high whiteness, but the total triterpenic acid content is, for example, 300 mg or more, preferably 350 mg or more, more preferably 1 g of rosemary extract in dry weight. It can be 400 mg or more. Since the rosemary extract of the present invention has a high total triterpenic acid content, it can be used as a material contributing to health and added to products such as foods and cosmetics to increase the added value of the products.

  Furthermore, the rosemary extract of the present invention not only has high whiteness, but also has an advantage of high carnosic acid content per gram of extract. The carnosic acid content in the rosemary extract can be measured by a known method, for example, it can be measured using a carnosic acid quantification method based on the HPLC method described in the examples described later. . The first feature of the rosemary extract of the present invention is high whiteness, but the carnosic acid content is, for example, 30 mg or more, preferably 60 mg or more, more preferably 70 mg, per 1 g of rosemary extract in dry weight. For example, it can be 80 mg or more. Since the rosemary extract of the present invention has a high carnosic acid content, it can be used as a material contributing to health and added to products such as foods and cosmetics to increase the added value of the products.

  In one preferred embodiment, the rosemary extract of the present invention has high whiteness (eg, 70-85) and has a total triterpenic acid content of 300 mg / g to 600 mg / g and 30 mg / g dry weight. Has a carnosic acid content of ˜200 mg / g. In another embodiment, the rosemary extract of the present invention has a high whiteness (eg, 70-85) and a total triterpenic acid content of 400 mg / g to 500 mg / g and 60 mg / g dry weight Has a carnosic acid content of ˜150 mg / g.

  The rosemary extract of the present invention has high whiteness, and depending on the purpose of use, the content of components contributing to health (carnosic acid and triterpenic acid) can be further increased. It can be used by adding it as a raw material to pharmaceuticals. Carnosic acid has been reported to have a strong antioxidant effect, an action for promoting the generation of nerve growth factors, and the like, and is effective for photoprotection, prevention of epilepsy, improvement of memory ability, and the like. It has been reported that oleanolic acid, betulinic acid, and ursolic acid have an NF-κB inhibitory action and are effective in improving symptoms such as diabetes, cardiovascular disease, and atherosclerosis. Therefore, the rosemary extract of the present invention can be used for imparting the action of these active ingredients to commodities such as foods and drinks, cosmetics and pharmaceuticals. Carnosic acid is also used in foods, cosmetics, pharmaceuticals, and the like as an antioxidant based on its antioxidant action, as a preservative based on its antibacterial action, and as a deodorant. Therefore, the rosemary extract of the present invention can also be used as an additive for foods, cosmetics, or pharmaceuticals such as antioxidants, preservatives, deodorants and the like.

  Food additives, foods, cosmetics, and pharmaceuticals containing the rosemary extract of the present invention include, for example, stabilizers, buffers, surfactants, pH adjusters, sweeteners, flavors, preservatives, colorants, An excipient, a thickener, a carrier, a solvent, a chelating agent, a lubricant, a coating agent and the like may further be included.

  For example, the form of the food and drink containing the rosemary extract of the present invention includes beverages such as energy drinks, soft drinks, tea, green tea, candy, cookies, tablet confectionery, chewing gum, jelly-like confectionery, and noodles. Cereals such as bread, cooked rice and biscuits, paste products such as sausages, ham and kamaboko, dairy products such as butter and yogurt, powdered protein beverages, powdered protein foods, dietary supplements and supplements (sport protein powder, beauty supplements) Functional foods such as, etc., sprinkles, seasonings and the like. The food or drink of the present invention may be in any shape such as solid, liquid, liquid food, jelly, tablet, granule and capsule. The food and drink of the present invention may further contain carbohydrates, proteins, lipids, dietary fibers, vitamins, minerals and the like. Examples of the protein include whole milk powder, skim milk powder, partially skimmed milk powder, casein, whey powder, whey protein, whey protein concentrate, whey protein isolate, α-casein, β-casein, κ-casein, β-lactoglobulin , Α-lactalbumin, lactoferrin, soy protein, chicken egg protein, meat protein and other animal and vegetable proteins, hydrolysates thereof, butter, whey minerals, cream, whey, non-protein nitrogen, sialic acid, phospholipid, lactose And various milk-derived components. Examples of the saccharide include general saccharides and processed starch (in addition to dextrin, soluble starch, British starch, oxidized starch, starch ester, starch ether, etc.). Examples of the lipid include animal oils such as lard, fish oil, etc., fractionated oils, hydrogenated oil, transesterified oil, etc .; palm oil, safflower oil, corn oil, rapeseed oil, coconut oil, fractionated oils thereof, Examples include vegetable oils such as hydrogenated oils and transesterified oils. Examples of dietary fiber include inulin dietary fiber, polydextrose, indigestible dextrin, fucoidan and the like. Examples of vitamins include vitamin A, carotene, vitamin B group, vitamin C, vitamin D group, vitamin E, vitamin K group, vitamin P, vitamin Q, niacin, nicotinic acid, pantothenic acid, biotin, inositol, choline. And minerals include, for example, calcium, potassium, magnesium, sodium, copper, iron, manganese, zinc, selenium, and whey minerals.

  Cosmetics containing the rosemary extract of the present invention include, for example, face wash, lotion, emulsion, cream, gel, cleansing cream, serum, pack, mask, foundation, eyeliner, mascara, eye shadow, ointment, etc. It may be. The cosmetics of the present invention may be in the form of liquid preparations such as liquids, suspensions and syrups, gel preparations, tablets, granules, solid preparations such as powders, pills and capsules, and powders. The cosmetic of the present invention may contain other medicinal ingredients such as other antioxidants, humectants, ultraviolet absorbers, anti-inflammatory agents, astringents and the like.

  The pharmaceutical containing the rosemary extract of the present invention may be in any dosage form such as a tablet, coated tablet, capsule, granule, powder, solution, syrup, emulsion and the like. The pharmaceutical product of the present invention may be used orally or parenterally.

  When the rosemary extract of the present invention is added to or blended with foods, beverages, cosmetics, pharmaceuticals, etc. to give a composition, it varies depending on the dosage form and form, but usually 0.1 to 100 by dry weight in the whole composition. % By weight, preferably about 1 to 95% by weight can be added.

  Since the rosemary extract of the present invention has a high content of carnosic acid and / or triterpenic acid, carnosic acid and the food, beverage, cosmetics and pharmaceuticals containing the rosemary extract of the present invention and The efficacy of triterpenic acid can be provided to the subject. Specifically, by orally or parenterally administering to the subject the rosemary extract of the present invention, or a food, beverage, cosmetic or pharmaceutical product containing the same, a strong antioxidant effect by carnosic acid, an antibacterial effect, The deodorizing effect and the like can be exhibited in the subject. As a result, the administration can be effective for, for example, prevention of photoaging (eg, prevention of hemorrhoids), cancer prevention, sterilization, odor removal, and the like. Moreover, the NF-κB inhibitory effect of triterpenic acid, etc. can be exhibited in the subject by orally or parenterally administering to the subject the rosemary extract of the present invention or food / beverage products, cosmetics or pharmaceuticals containing the same. it can. As a result, the administration may be effective in improving symptoms such as diabetes, cardiovascular disease, and atherosclerosis. The dosage of the food / beverage products, cosmetics or pharmaceuticals of the present invention can be set to an amount of 0.01 mg to 0.5 mg / dose, for example, with the content (dry weight) of the rosemary extract of the present invention.

  EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated further in detail, this invention is not limited by this. In Examples, “%” indicates “% by weight” unless otherwise specified.

[raw materials]
A dried rosemary product from Albania (Otsuya Shoten (Japan)) was used.

[Method of quantifying triterpenic acid]
In the following tests, the contents of oleanolic acid, ursolic acid, and betulinic acid contained in the dry powder were measured by HPLC. Specifically, a 5 mg sample (rosemary extract) or a standard product of each component was suspended in 76% ethanol and made up to 50 mL. The standard product was further diluted 2 to 16 times. They were analyzed by the HPLC method under the following conditions, and the total triterpenic acid content per gram of the extract was determined from the prepared calibration curve.

Analysis conditions
LC (liquid chromatograph): HPLC (Agilent)
Column: XDB-C18 3.0 mm x 150 mm, 2 columns connected Column temperature: 50 ° C
Mobile phase: A 0.2% ammonium acetate aqueous solution
B Methanol flow rate: 0.5 mL / min
Injection volume: 10 μL
UV detection: 215 nm

[Quantitative method of carnosic acid]
In the following test, the content of carnosic acid contained in the dry powder was measured by HPLC. Specifically, a 5 mg sample (rosemary extract) or a standard product was suspended in 100% ethanol and made up to 5 mL. The standard product was further diluted 2-64 times. They were analyzed by the HPLC method under the following conditions, and the amount of carnosic acid per gram of the extract was determined from the prepared calibration curve.

Analysis conditions
LC: HPLC (Agilent)
Column: XDB-C18 3.0mm x 50mm
Column temperature: 40 ° C
Mobile phase: A 0.1% formic acid aqueous solution
B Acetonitrile flow rate: 0.6 mL / min
Injection volume: 10 μL
UV detection: 215nm

[Measurement method of whiteness]
In the following tests, Hunter whiteness in dry powder L * a * b * color system was measured. The lightness is represented by L *, and the chromaticity indicating hue and saturation is represented by a * and b *. Specifically, using a spectroscopic color difference meter (spectral colorimeter) (CM-5, manufactured by Konica Minolta Co., Ltd.), put the powder so that there is no gap in the glass cell, and set the L * a * b * value in reflection mode. It was measured. Based on the result, the whiteness was calculated from the following equation.
W (whiteness) = 100-sqr [(100-L) 2+ (a ² + b ² )]

[Judgment method of comprehensive evaluation]
The overall evaluation was performed as shown in Table 3. First, the overall evaluation was “D” for those with a whiteness of less than 61. For those with a whiteness of 61 or more, the content of carnosic acid per gram of extract is less than 30 mg and the total triterpenic acid content per gram of extract is less than 300 mg Was satisfied, and even if added to the raw material, the effect on the commercial value is low, but because there are not enough ingredients to contribute to health, it was evaluated as “C”. In addition, if the carnosic acid content per gram of extract is 30 mg or more, or the total triterpenic acid content per gram of extract is 300 mg or more, it contains ingredients that contribute to health. “B” was evaluated and “A” was evaluated because a material satisfying both components more than the specified value can be a material with high added value.

[Comparative Example] Examination of extraction method described in JP-A-2009-249306 According to the method described in paragraphs [0018] to [0019] of JP-A-2009-249306, a rosemary extract was obtained. That is, after the rosemary leaf was extracted with hot water, the residue was collected and dried. Thereafter, the dried product was pulverized. 20 g of a dried product was added to 400 mL of 95% ethanol, and the mixture was extracted with stirring at 200 rpm using a stirrer at 40 ° C. for 2 hours. To the filtrate (310 g) obtained by filtering the extract, half the amount of purified water (155 g) or twice the amount of purified water (620 g) was added and stirred. After standing for about 2 hours, the deposited components were centrifuged to collect the precipitate, and dried at 80 ° C. to obtain a rosemary extract.

  The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

The results are shown in Table 4. The rosemary extract obtained by the method described in JP-A-2009-249306 has a low whiteness and is visually green.

[Example 1] Examination of lower alcohol concentration in extraction process
20 g of dried rosemary leaves were added to 400 mL of 95, 90, 85, and 80% ethanol, respectively, and extracted with stirring at 200 rpm using a stirrer at 50 ° C. for 2 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 100 mL of purified water and powdered by lyophilization. The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

Table 5 shows the results. Compared with the rosemary extract of the above comparative example, the whiteness was remarkably high at any ethanol concentration, and reached a maximum of 72.4 by extraction at an ethanol concentration of 90%. The carnosic acid content and the total triterpenic acid content tended to increase as the ethanol concentration of the solvent increased.

[Example 2] Examination of extraction temperature
20 g of dried rosemary leaves were added to 400 mL of 90% ethanol. Extraction was performed with stirring at 200 rpm using a stirrer at 30, 40, 60, or 70 ° C. for 2 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 200 mL of purified water and filtered. Further, the deposit remaining on the filter paper was filtered with 400 mL of purified water at room temperature and washed. The obtained precipitate was suspended in 100 mL of purified water and powdered by lyophilization. The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

Table 6 shows the results. Whiteness exceeded 61 at any extraction temperature. In particular, when the extraction temperature was 30 ° C. or 40 ° C., the whiteness exceeded 80. On the other hand, the samples extracted under the conditions of extraction temperatures of 40 ° C. and 30 ° C. had a low carnosic acid content, and when the extraction temperature was 70 ° C. or 60 ° C., the carnosic acid content increased significantly. Therefore, it was clarified that in the method for producing a rosemary extract of the present invention, the amount of carnosic acid can be controlled by controlling the extraction temperature.

[Example 3] Examination of extraction time
20 g of dried rosemary leaves were added to 400 mL of 90% ethanol. Extraction was performed with stirring at 200 rpm using a stirrer at 40 ° C. for 4, 8, 13, or 24 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 200 mL of purified water and filtered. Further, the deposit remaining on the filter paper was filtered with 400 mL of purified water at room temperature and washed. The obtained precipitate was suspended in 100 mL of purified water and powdered by lyophilization. The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

Table 7 shows the results. Whiteness exceeded 61 at any extraction time, but when extracted at 40 ° C using a 90% ethanol solvent, the whiteness increased and the total triterpenic acid content increased as the extraction time decreased. The tendency to do was recognized. On the other hand, when the carnosic acid content was extracted at 40 ° C. using a 90% ethanol solvent, the content increased as the extraction time increased.

[Example 4] Examination of stirring method and rotation speed
20 g of dried rosemary leaves were added to 400 mL of 90% ethanol. Extraction was performed with stirring at 50, 200, or 300 rpm using a three-one motor at 50 ° C. for 2 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 200 mL of purified water and filtered. Further, the deposit remaining on the filter paper was filtered with 400 mL of purified water at room temperature and washed. The obtained precipitate was suspended in 100 mL of purified water and powdered by lyophilization. The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

The results are shown in Table 8. Regardless of the stirring method and rotation speed during extraction, the whiteness was high, and the carnosic acid content and the total triterpenic acid content were high.

[Example 5] Examination of presence or absence of washing at room temperature extraction
20 g of dried rosemary leaves were added to 400 mL of 90% ethanol. Extraction was performed with stirring at 200 rpm using a stirrer at room temperature for 18 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 200 mL of purified water and filtered. Further, the deposit remaining on the filter paper was filtered with 400 mL of purified water at room temperature and washed. Moreover, what was not wash | cleaned was created, and the precipitate was suspended in 100 mL purified water, and was pulverized by freeze-drying. The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

The results are shown in Table 9. When extracted at room temperature for 18 hours, there was no effect on the whiteness, carnosic acid content, and total triterpenic acid content by washing.

[Example 6] Examination of cleaning method
20 g of dried rosemary leaves were added to 400 mL of 90% ethanol. The mixture was extracted with stirring at 200 rpm using a stirrer at 50 ° C. for 2 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 200 mL of purified water and filtered. Further, the precipitate remaining on the filter paper was filtered and washed with purified water at normal temperature or purified water heated to 50 ° C. The amount of purified water was 400 mL or 1200 mL. The precipitate obtained by the above treatment was suspended in 100 mL of purified water and powdered by lyophilization. The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

The results are shown in Table 10. The whiteness was remarkably high at any concentration, and in particular, when washed with purified water at room temperature, the whiteness exceeded 80. There were no differences in the degree of whiteness, carnosine content, or total triterpenic acid content due to differences in the amount of purified water to be washed.

[Example 7] Examination of extraction using pulverized raw material
To 400 mL of 90% ethanol, 20 g of powder obtained by pulverizing dried rosemary leaves with a mill and passing through a 10 mesh sieve (10 mesh pass) was added. The mixture was extracted with stirring at 200 rpm using a stirrer at 50 ° C. for 2 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 200 mL of purified water and filtered. Further, the deposit remaining on the filter paper was filtered with 400 mL of purified water at room temperature and washed. The obtained precipitate was suspended in 100 mL of purified water and powdered by lyophilization. The whiteness, solid content recovery rate, carnosic acid content per gram of extract, and total triterpenic acid content per gram of extract were measured for overall evaluation.

The results are shown in Table 11. By carrying out the extraction step after grinding the raw material, the content of carnosic acid was increased, but the whiteness was significantly reduced.

[Example 8] Manufacture of tablet confectionery
20 g of dried rosemary leaves were added to 400 mL of 90% ethanol. The mixture was extracted with stirring at 200 rpm using a stirrer at 50 ° C. for 2 hours. The extract was filtered through a Kiriyama funnel and concentrated under reduced pressure. The obtained precipitate was suspended in 200 mL of purified water and filtered. Further, the deposit remaining on the filter paper was filtered with 400 mL of purified water at room temperature and washed. The obtained precipitate was suspended in 100 mL of purified water and pulverized by freeze-drying to prepare a rosemary extract. The solid content recovery was 9.8%, the whiteness of the obtained rosemary extract was 79.4, and the total triterpenic acid content per 1 g of the extract was 431.2 mg. Using this rosemary extract, tablet confectionery was produced with the following composition.
Rosemary extract of the present invention 0.1
Sucrose 95.9
Citric acid 2.0
Gum arabic 1.0
Calcium stearate 1.0
Total 100.0

  The manufactured tablet confectionery had no color derived from the rosemary extract and was white.

  The rosemary extract of the present invention has a higher whiteness than the conventional rosemary extract, and when added to foods and drinks and cosmetics, there is no undesirable coloring derived from the rosemary extract, thus impairing the commercial value. It can be used without any problems. Moreover, since the rosemary extract of the present invention has a high content of carnosic acid and triterpenic acid, it can be added to and blended with foods and beverages and cosmetics to provide high-value-added products that contribute to health. It can be used as a useful raw material.

  All publications, patents and patent applications cited herein are incorporated herein by reference in their entirety.

Claims (9)

A rosemary plant or a part thereof is treated with a lower alcohol at 45 ° C. to 70 ° C. for 1 to 4 hours without pulverizing to obtain an extract, which is concentrated, and the resulting precipitate is collected. A method for producing a rosemary extract having a whiteness of 61 or more and containing carnosic acid and triterpenic acid, comprising recovering , wherein the lower alcohol is ethanol having a concentration of 85% or more and less than 95% .   The method of claim 1, further comprising washing the precipitate. The method according to claim 1 or 2 , wherein the treatment with a lower alcohol is carried out at 50 ° C to 70 ° C. The method according to claim 1 or 2 , wherein the treatment with a lower alcohol is carried out at 45 ° C to 55 ° C. The method according to claim 1 or 2 , wherein the treatment with a lower alcohol is performed at 60 ° C to 70 ° C. Rose plants Marie or portion thereof, comprises a leaf rosemary A method according to any one of claims 1-5. And the carnosic acid content in rosemary extract dry weight 30 mg / g or more, a total triterpenic acid content is dry weight 300 mg / g or more, according to any one of claims 1 to 6 Method. The method according to any one of claims 1 to 7 manufactured rosemary extract, comprising adding or mixing it into food products, the manufacturing method of food or drink. Manufactured rosemary extract by the method according to any one of claims 1 to 7 comprising adding or mixing it in cosmetics, cosmetics manufacturing method.

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