JP2007054056A - Method for producing coffee composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing coffee liquid having excellent blood pressure lowering action. <P>SOLUTION: This method for producing a coffee composition having excellent blood pressure lowering action comprises extracting coffee extracted solution from coffee beans in the existence of a porous adsorbent which has a volume of pore whose radius is ≤0.7 nanometer (nm) of ≥30% of the whole pore volume of the porous adsorbent, or extracting coffee extracted solution from coffee beans and bringing without cooling the coffee extracted solution into contact with a porous adsorbent which has a volume of pore whose radius is ≤0.7 nanometer (nm) of ≥30% of the whole pore volume of the porous adsorbent. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing a coffee composition having a high chlorogenic acid content, a low hydroxyhydroquinone content, and an improved flavor, and a method for producing soluble coffee.

It has been reported that chlorogenic acid, caffeic acid, ferulic acid and the like exhibit excellent blood pressure lowering action (Patent Documents 1 to 3). However, coffee beverages known to contain a large amount of chlorogenic acids do not have a clear blood pressure lowering effect, and there is a report that blood pressure is increased (Non-patent Document 1).
JP 2002-363075 A JP 2002-22062 A JP 2002-53464 A Eur. J. Clin. Nutr., 53 (11), 831 (1999)

  An object of the present invention is to provide a coffee composition having an excellent blood pressure lowering action and a refreshing flavor, and a method for producing soluble coffee.

  Therefore, the present inventor has paid attention to the fact that coffee beverages do not show sufficient blood pressure lowering action despite containing chlorogenic acids, and as a result of various studies on the relationship between blood pressure lowering action and coffee beverage ingredients, It has been found that hydroxyhydroquinone contained in beverages inhibits the blood pressure lowering action of chlorogenic acids. As a result of further investigation, the hydroxyhydroquinone content was reduced while maintaining the amount of chlorogenic acids in the coffee beverage within a certain range by performing an extraction operation from coffee beans in the presence of a porous adsorbent having a specific pore size. It has been found that a sufficient blood pressure lowering effect can be obtained and a clear flavor can be obtained.

  That is, the present invention relates to coffee in the presence of a porous adsorbent having a pore radius of 0.7 nanometers (nm) or less and having a pore volume of 30% or more of the total pore volume of the porous adsorbent. Extract coffee extract from beans, or extract coffee extract from coffee beans, and absorb pore volume with pore radius of 0.7 nanometers (nm) or less without cooling the extract The present invention provides a method for producing a coffee composition characterized by contacting with a porous adsorbent that is 30% or more of the total pore volume of the body.

  That is, the present invention relates to coffee in the presence of a porous adsorbent having a pore radius of 0.7 nanometers (nm) or less and having a pore volume of 30% or more of the total pore volume of the porous adsorbent. Extract coffee extract from beans, or extract coffee extract from coffee beans, and absorb pore volume with pore radius of 0.7 nanometers (nm) or less without cooling the extract The chlorogenic acid is contained in an amount of 0.01 to 1% by mass, and the hydroxyhydroquinone content is the amount of the chlorogenic acid. The present invention provides a method for producing a coffee composition that is less than 0.1% by mass.

  The present invention also provides coffee in the presence of a porous adsorbent having a pore radius of 0.7 nanometers (nm) or less and having a pore volume of 30% or more of the total pore volume of the porous adsorbent. Extract coffee extract from beans, or extract coffee extract from coffee beans, and absorb pore volume with pore radius of 0.7 nanometers (nm) or less without cooling the extract By contacting with a porous adsorbent that is 30% or more of the total pore volume of the body, the chlorogenic acids are contained in an amount of 0.01 to 1% by mass and the hydroxyhydroquinone content is 0.1% by mass of the chlorogenic acids The present invention provides a method for producing soluble coffee, characterized in that the coffee composition is less than%, and then the coffee composition is spray-dried or freeze-dried. By dissolving this soluble coffee in warm water or the like, a coffee liquid containing 0.01 to 1% by mass of chlorogenic acids and having a hydroxyhydroquinone content of less than 0.1% by mass of the amount of chlorogenic acids can be easily obtained. Can be prepared.

  According to the production method of the present invention, a coffee composition having an excellent blood pressure lowering action and a refreshing flavor can be obtained.

  The type of coffee beans used in the present invention is not particularly limited, and examples thereof include Brazil, Colombia, Tanzania, mocha, kilimangelo, mandelin, and blue mountain. Coffee beans include Arabica and Robusta. One kind of coffee beans may be used, or a plurality of kinds may be blended. There is no particular limitation on the method of making coffee beans by roasting coffee beans, and there are no restrictions on the roasting temperature and roasting environment, but the preferred roasting temperature is 100 to 300 ° C., more preferably 150-250 ° C. Preferred roasting methods include a direct fire method, a hot air method, and a semi-hot air method, and a type having a rotating drum is more preferable. Moreover, it is preferable to cool to 0-100 degreeC within 1 hour after roasting from a viewpoint of flavor, More preferably, to 10-60 degreeC.

  As roasting degree of roasted coffee beans, there are light, cinnamon, medium, high, city, full city, french and italian, and light, cinnamon, medium, high and city are preferred. The L value obtained by measuring the roasting degree with a color difference meter is usually 10 to 30, preferably 15 to 25. Note that coffee beans having different roasting degrees may be mixed.

  There is no limitation on the extraction method from coffee beans, for example, using roasted coffee beans or pulverized products thereof using an extraction solvent such as water to hot water (0 to 100 ° C.) or steam, or pressurized steam of 100 ° C. or higher. The method of extracting for 2 seconds-120 minutes is mentioned. The extraction temperature is preferably 50 to 100 ° C., particularly preferably 80 to 100 ° C., and particularly preferably 90 to 100 ° C. from the viewpoint of the amount of chlorogenic acids recovered. The degree of grinding is as follows: extra fine grinding (0.250-0.500μm), fine grinding (0.300-0.650μm), medium fine grinding (0.530-1.000μm), medium grinding (0.650-1.500μm), medium coarse grinding, coarse grinding (0.850- 2.100 μm), ultra-coarse grind (1.000-2.500 μm), and cut products having an average particle diameter of 3 mm, 5 mm, and 10 mm. Examples of the extraction method include a boiling type, an espresso type, a siphon type, and a drip type (paper, flannel, etc.).

Examples of the extraction solvent include water, alcohol-containing water, milk, carbonated water, and the like. The pH of the extraction solvent is usually 4 to 10, and 5 to 7 is preferable from the viewpoint of flavor. In addition, a pH adjuster such as sodium bicarbonate, sodium bicarbonate, L-ascorbic acid, and L-alcorbic acid Na may be contained in the extraction solvent, and the pH may be adjusted as appropriate.
The amount of extraction solvent is usually 0.1 to 100 times the amount of 1 part by weight of coffee beans, and preferably 1 to 30 times the amount from the viewpoint of the recovered amount of chlorogenic acids.

  As the extractor, paper drip, non-woven drip, siphon, nell drip, espresso machine, coffee machine, percolator, coffee press, ibrick, water drip, boiling, etc. Drip extractor with structure (mesh, punched metal, etc.) that can substantially separate coffee beans at the bottom of the spray nozzle at the top, and solid and liquid separation of coffee beans at the top and / or bottom Column extractor having a simple structure (mesh, punching metal, etc.). The extractor may have a structure that can be heated or cooled (for example, an electric heater, a jacket through which hot water, steam, or cold water can flow).

Examples of the extraction method include a batch extraction method, a semi-batch extraction method, and a continuous extraction method. The extraction time of the batch extraction method or the semi-batch extraction method is preferably 10 seconds to 120 minutes, and more preferably 30 seconds to 30 minutes, from the viewpoint of flavor.
In addition, chlorogenic acids extracted from raw coffee beans and / or finely roasted beans having an L value of 30 to 60 can be added to the raw coffee extract of the present invention as necessary.

In the present invention, in order to reduce the hydroxyhydroquinone content, the pore volume with a pore radius of 0.7 nanometer (nm) or less is 30% or more with respect to the total pore volume of the porous adsorbent. Adsorbent is used. Preferably, the pore radius is 0.7 nanometer (nm) or less, more preferably 0.2 to 0.7 nanometer (nm), and the pore volume is 30 with respect to the total pore volume of the porous adsorbent. % Or more, further 30 to 98%, further 0 to 95%, more preferably 50 to 95%, particularly preferably 70 to 90%. A porous adsorbent having a pore radius of less than 0.7 nanometers (nm) and a pore volume of less than 30% of the total pore volume of the porous adsorbent has a low selectivity for removing hydroxyhydroquinone. Therefore, it is not preferable. Here, the pore radius and the capacity of the porous adsorbent are values measured by the MP method in the region where the pore radius is 1 nanometer (nm) or less, and in the region where the pore radius exceeds 1 nanometer (nm). Is a value measured by the KJH method, and whether or not the pore volume with a pore radius of 0.7 nanometer (nm) or less is 30% or more with respect to the total pore volume of the porous adsorbent Can be determined from pore distribution curves obtained by the MP method and the KJH method.
MP method pore radius 1 nanometer (nm) or less Total pore volume: VM (cm ³ / g)
Total pore volume in excess of 1 nanometer (nm) by the KJH method: VK (cm ³ / g)
Pore radius by MP method 0.7 nanometer (nm) or less Pore volume: V7 (cm ³ / g)
Ratio of pore volume having a pore radius of 0.7 nanometer (nm) or less to the total pore volume of the porous adsorbent: V% = V7 / (VM + VK) × 100%

  The MP method is a pore measurement method described in the literature (Colloid and Interface Science, 26, 46 (1968)), and the KJH method is the literature (J. Amer. Chem. Soc., 73.373 (1951)). And can be measured at Sumika Analysis Center, Inc., Toray Research Center, Inc., etc., respectively. As a pore measuring device, there is BELSORP-mini and the like, which can be measured using a nitrogen adsorption method.

Further, the porous adsorbent has an average pore radius in the micropore region of 0.5 nanometer (nm) or less, more preferably 0.2 to 0.5 nanometer (nm) or less, particularly 0.3 to 0. Preferably it is in the range of 5 nanometers (nm). Here, the micropore region indicates 1 nanometer (nm) or less, and the average pore radius is a value of the pore radius indicating the peak top of the pore distribution curve obtained by the MP method.
From the viewpoint of reducing the effect of hydroxyhydroquinone content, pore volume by the MP method of the porous adsorbent, 0.5 cm ³ / g or more, preferably further 0.5~2cm ³ / g, further 0.6 1 cm ³ / g is preferred.

  The particle size of the porous adsorbent is not particularly limited, but if it is too large, the contact area with the adsorbent becomes small and the adsorption speed becomes slow. From the above points, the average particle size is preferably 0.01 μm or more and 2 mm or less, more preferably 50 μm or more and 400 μm or less, and particularly preferably 50 μm or more and 200 μm or less.

Examples of porous adsorbents are described in Adsorption Technology Handbook-Process, Materials, and Design-(January 11, 1999, issued by NTS, Supervisor: Atsushi Takeuchi). Carbonaceous adsorbent, silica / alumina adsorbent, polymer adsorbent, chitosan resin, etc. can be used. From the viewpoint of leaving the coffee flavor, a carbonaceous adsorbent is preferred.
As the carbonaceous adsorbent, powdered activated carbon, granular activated carbon, and activated carbon fiber are preferable from the viewpoint of selectively adsorbing hydroxyhydroquinone. Furthermore, activated carbon fiber is preferable because the flavor of the extract is good and the amount of chlorogenic acids recovered is large.

  As raw materials for powdered and granular activated carbon, there are sawdust, coal, coconut shell, etc., but coconut shell activated carbon derived from coconut shell is preferred. Specifically, Hakuho WH2C (Nippon Enviro Chemicals Co., Ltd.), Dazai CW (Nimura Chemical Co., Ltd.), Kuraray Coal GL (Kuraray Chemical Co., Ltd.), etc. can be used. In particular, activated carbon activated by a gas such as water vapor is preferable.

  Activated carbon fibers include polyacrylonitriles such as Fineguard (Toho Rayon Co., Ltd.), pitches such as Adol (Unitika Ltd.), phenols such as Kractive (Kuraray Co., Ltd.), K filters (Toyobo) Cellulose type such as Co., Ltd., and other phenol type and cotton type.

  In addition, the shape of the porous adsorbent is not particularly limited. In addition to ordinary powder and granular materials, the adsorbent is kneaded into fibers, molded with each porous adsorbent, cellulose, nonwoven fabric, and binder. Or molded.

  The amount of the porous adsorbent used is usually 1 to 300% by mass, preferably 5 to 100% by mass, and more preferably 8 to 50% by mass with respect to coffee beans.

  The porous adsorbent may be present during or immediately after the extraction operation. For example, the coffee beans and the porous adsorbent may be mixed and put into an extractor, or on the porous adsorbent layer. A coffee bean layer may be laminated and an extraction solvent may be added from the coffee bean layer side to obtain a coffee composition from the porous adsorbent layer side. Further, following the coffee extraction process from coffee beans, the porous adsorbent may be immersed in the coffee extract. In this case, the porous adsorbent may be brought into contact with the coffee extract without cooling the coffee extract, or the porous adsorbent may be brought into contact with the coffee extract after natural cooling. A porous adsorbent may be brought into contact with. From the viewpoint of leaving a good flavor and increasing the recovered amount of chlorogenic acids, it is preferable that the porous adsorbent is brought into contact with the coffee extract after cooling to -10 to 90 ° C, and further preferably cooled to 0 to 90 ° C. In particular, 5 to 40 ° C. is preferable.

  In the drip method, it is preferable to put a porous adsorbent on a filter such as paper or flannel. A porous adsorbent may be inserted between the filters. Further, a porous adsorbent may be placed on the extracted coffee extract side. When placing a porous adsorbent on the side of the extracted coffee extract, for example, a bag filled with the porous adsorbent is placed in the extracted coffee extract or a rod-shaped porous adsorbent is immersed in the coffee extract Preferably, the coffee extract can be further stirred with a rod-shaped porous adsorbent. When such a porous adsorbent is used, the removal of the porous adsorbent after the operation is facilitated.

  The bag or rod-shaped porous adsorbent filled with the porous adsorbent used in the method of the present invention is processed into a coffee liquid or a can or a coffee container composition packed in a PET container containing instant coffee dissolved in hot water at a processing temperature − Immerse in coffee extract in the range of 10-95 ° C. From the viewpoint of leaving a good flavor and increasing the recovered amount of chlorogenic acids, it is preferably treated at -10 to 90 ° C, more preferably 0 to 80 ° C, particularly preferably 5 to 60 ° C.

The material of the bag filled with activated carbon may be any material as long as the coffee extract can permeate and the activated carbon does not substantially leak out. Examples thereof include non-woven fabric, paper, and wire mesh. In addition, you may provide the auxiliary | assistant structure part attached to a string or a cup suitably in a bag or a container.
Examples of the rod-shaped porous adsorbent include various shapes formed by mixing activated carbon and a binder.

  The contact time of the porous adsorbent molded body and the coffee extract (residence time in the case of column passage) is usually 30 seconds to 100 hours, 30 seconds to 120 minutes when the temperature of the extract is higher than 10 ° C, The time of 1 to 60 minutes is particularly preferred from the viewpoint of reducing the hydroxyhydroquinone content and improving the flavor.

  Moreover, it is also preferable from the point of the hydroxyhydroquinone content reduction effect to perform extraction operation on the pressurization conditions of 0.01-5 Mpa. As a means for the pressure treatment, there is a method of extraction using a batch-type airtight container (FIG. 1) or a column extractor (FIG. 2).

The porous adsorbent can be used for processing coffee extract as a porous adsorbent holding tool incorporating the porous adsorbent. Therefore, according to the present invention, there is provided a porous adsorbent holding tool for removing hydroxyhydroquinone from a coffee extract comprising the porous adsorbent.
The porous adsorbent holding tool includes (1) a bag-type porous adsorbent holding tool in which the porous adsorbent is filled in a bag that does not substantially leak, and (2) the porous adsorbent substantially A molded-type porous adsorbent holding tool molded so as not to leak into the liquid, and (3) a filter-type porous adsorbent holding tool formed by shaping the porous adsorbent into a shape having a filtration function. Can be mentioned.

Examples of the bag-type porous adsorbent holding tool include a bag-like structure filled with a porous adsorbent through which a coffee extract permeates or passes and substantially does not leak out.
Examples of the bag-like structure include non-woven fabrics, filter papers, nets, and punching structures made into a bag shape. In addition, you may provide the auxiliary structure attached to a string or a cup suitably.

Molded type porous adsorbent holding tool (hereinafter also referred to as molded type porous adsorbent): paper made by mixing porous adsorbent with cellulose fiber, etc., molded non-woven fabric fiber and porous adsorbent , One formed by mixing and forming a porous adsorbent and a binder, one obtained by forming a porous adsorbent material into a porous adsorbent, one obtained by mixing and / or laminating activated carbon fibers and another porous adsorbent, In addition, the honeycomb activated carbon which is the activated carbon molded body described in the adsorption technology handbook-process, material, and design-(January 11, 1999, issued by NTS, supervisor: Atsushi Takeuchi) is mentioned. .
Examples of the porous adsorbent material after forming the porous adsorbent material include activated carbon fiber felt, activated carbon fiber knitted fabric, and activated carbon fiber such as activated carbon fiber fabric.

  As a filter type porous adsorbent holding tool, the molded type porous adsorbent is formed into a filterable bag shape that is a paper filter shape for a coffee maker, etc. The thing which fixed or installed the molded object type porous adsorption body can be illustrated.

The porous adsorbent used in the porous adsorbent holding tool may be used by appropriately mixing the various porous adsorbents.
The contact time of the porous adsorbent-holding tool with the coffee extract at −10 to 95 ° C. is preferably 30 seconds to 100 hours, more preferably 1 hour to 48 hours, from the viewpoint of the removal efficiency and flavor of hydroxyhydroquinone.

  The coffee composition obtained by the method of the present invention contains 0.01 to 1% by mass of chlorogenic acids, but preferably 0.05 to 1% by mass in terms of blood pressure lowering action and flavor. In addition, the coffee composition obtained by the method of the present invention has a hydroxyhydroquinone content of less than 0.1% by mass, more preferably 0.08% by mass or less, further 0.05% by mass or less, based on the amount of chlorogenic acids. Especially 0.03 mass% or less is preferable. If the amount of hydroxyhydroquinone is less than 0.1% by mass relative to the amount of chlorogenic acids, the blood pressure lowering action of chlorogenic acids is exhibited. If the amount of hydroxyhydroquinone is 0.03% by mass or less with respect to the amount of chlorogenic acids, the blood pressure lowering effect of chlorogenic acid appears remarkably. Here, the hydroxyhydroquinone content in the coffee composition of the present invention may be zero.

  As the chlorogenic acids, there are known three kinds of monocaffeoylquinic acid, ferlaquinic acid, and dicaffeoylquinic acid, and the content of chlorogenic acids is represented by the total amount thereof. Examples of monocaffeoylquinic acid include one or more selected from 3-caffeoylquinic acid, 4-caffeoylquinic acid, and 5-caffeoylquinic acid. Further, examples of ferulquinic acid include one or more selected from 3-ferlaquinic acid, 4-ferlaquinic acid, and 3-ferlaquinic acid. Examples of dicaffeoylquinic acid include one or more selected from 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid, and 4,5-dicaffeoylquinic acid.

  The content of the chlorogenic acids can be measured by high performance liquid chromatography (HPLC). As a detection means in HPLC, UV detection is generally used, but it can also be detected with higher sensitivity by CL (chemiluminescence) detection, EC (electrochemical) detection, LC-Mass detection, or the like.

  The hydroxyhydroquinone content can be measured by HPLC. As a detection means in HPLC, UV detection is generally used, but it can also be detected with higher sensitivity by CL detection, EC detection, LC-Mass detection, or the like. In addition, in measuring the hydroxyhydroquinone content by HPLC, it can also measure after concentrating a coffee solution, However, It is preferable to adjust to pH 3 or less beforehand by addition, such as phosphoric acid or hydrochloric acid.

In the coffee composition obtained by the method of the present invention, the ratio of chlorogenic acids to the coffee solids, that is, the mass ratio of chlorogenic acids / coffee solids is preferably 0.025 or more, more preferably 0.03 to 0.00. 9, particularly preferably 0.08 to 0.4. The coffee solid content here is not based on all the solid content in the beverage or the composition but is defined based on the following calculation formula, and the unit is based on mass.
Coffee solids [mass%]
= Brix-[milk solid content + sugar + dietary fiber + carbohydrate excluding sugar]
Here, each item described above is defined by the following calculation formula.
Milk solid content = lipid + 1.8 x lactose Sugar = glucose + fructose + sucrose + maltose

Here, the measurement method of each item is quantified by the following method.
-Brix: Represented by a refractometer reading for sugar at 20 ° C (° Brix).
For example, it can be analyzed with Atago RX-5000 (manufactured by Atago).
The latest soft drinks (issued September 30, 2003, published by Kojo Co., Ltd., page 243)
-Lipid: Rosette Gottlieb method-Lactose: High-performance liquid chromatographic method-Sugars: Glucose, fructose, sucrose, maltose: High-performance liquid chromatographic method-Carbohydrates excluding saccharides: High-performance liquid chromatographic method `` Is a saccharide added to the coffee composition, such as oligosaccharides such as trisaccharides and tetrasaccharides, sugar alcohols such as erythritol, xylitol, sorbitol, maltitol, and reduced starch syrup, polysaccharides such as starch, etc. Lactose from sugar-based sweeteners described in the literature (Sweetness genealogy and its science: published on June 20, 1986, published by Korin Co., Ltd., page 90, Table 2-1 Main sugar-based sweeteners) These are defined as monosaccharides, disaccharides, oligosaccharides and sugar alcohols excluding glucose, fructose, sucrose and maltose, which are four types defined as saccharides and sugars.
・ Dietary fiber: High-performance liquid chromatographic method (enzyme-HPLC method)
Here, dietary fiber refers to the nutrition labeling standard system for foods, second edition (issued July 1, 1999, edited by the Japan Health and Nutrition Food Association, Nutrition Food Department, pages 46-51). It refers to the object of analysis by the method.
In addition, the analysis method for each of the above items is the analysis method described in the product test series (12-5)-(issued in November 2001) issued by the Tokyo Consumer Life Center, dated April 26, 1999, Conforms to the notice of the Director of the Newly Developed Food Health Countermeasures Office, Food Health Division, Ministry of Health and Welfare, Ministry of Health and Welfare, and No. 13 “Analytical Methods for Nutritional Components, etc. in Nutrition Labeling Standards”.

  The coffee composition obtained by the present invention preferably uses 1 g or more of coffee beans in terms of green beans per 100 g, more preferably 2.5 g or more of coffee beans, and more preferably coffee beans. Is used 5g or more.

Moreover, raw milk, cow milk, whole milk powder, skim milk powder, fresh cream, concentrated milk, skim milk, partially skimmed milk, condensed milk, etc. can be suitably blended as a milk component in the coffee composition produced by the method of the present invention.
Moreover, if the coffee composition obtained as described above is spray-dried or freeze-dried, soluble coffee capable of adjusting the coffee composition having the composition can be obtained. Further, by concentrating the coffee composition obtained as described above, a pasty coffee capable of adjusting the coffee liquid of the composition can be obtained. In addition, the coffee composition obtained as described above is appropriately formulated and sterilized, then filled into a container such as a plastic bottle or cup, and tightened, or filled into a container such as a can and sterilized after being tightened, and then sterilized. A beverage is obtained.

  Here, the spray drying method and the freeze drying method are not particularly limited. For example, in the case of spray drying, the coffee composition is sprayed from a nozzle and passed through hot air of usually 150 to 310 ° C, preferably about 210 to 310 ° C, to form a porous, water-soluble coffee powder. it can. On the other hand, in the case of freeze-drying, the coffee composition is frozen in liquid nitrogen, a freezer, etc., crushed, sieved, and then sublimated in vacuum to obtain a dry powder by reducing the moisture to 3% or less. be able to.

  The coffee composition and soluble coffee obtained by the present invention contain an effective amount of chlorogenic acids having an antihypertensive effect, the amount of hydroxyhydroquinone is reduced, and the flavor is improved, so that the beverage is continuously drinked. Is possible.

Example 1
Colombian beans were roasted to L value = 22 as regular coffee beans. Obtain 130g of coffee beans crushed to medium grind, 40g of activated carbon (WH2CLSS, steam activated product, manufactured by Nippon Enviro) in an extractor with an 80 mesh wire mesh at the bottom of a cylindrical tube, and uniform thickness of activated carbon in the lower layer of the extractor Then, coffee beans were laminated on the upper layer, extracted with 90 ° C. ion exchange water at a flow rate of 12 g / min, cooled to 20 ° C., and then 1040 g of a coffee composition was obtained (see FIG. 3). .
Activated carbon was removed from the treated activated carbon-containing coffee composition using a 0.5 μm filter to obtain a coffee extraction treatment liquid. A baking beverage composition was prepared by adding baking soda to the coffee extraction treatment liquid until the pH reached a specified value according to the formulation shown in Table 1. The coffee beverage composition was filled into a beverage can and sealed, and then sterilized using a retort sterilizer to obtain a product. Sterilization was performed under the sterilization conditions (temperature × time) shown in Table 2 to obtain a packaged coffee drink.
Nippon Enviro activated carbon: WH2C 42/80 LSS (particle size 200-400 μm)
Results of pore volume measurement by BELSORP-mini Total pore volume 0.837 mL / g, 0.7 nm or less pore volume 0.651 mL / g
MP70 pore volume 0.670 mL / g
Average pore radius in the micropore region 0.35 nm
0.7 nm or less pore volume / total pore volume = 78%
0.2-0.7 nm pore volume / total pore volume = 78%

Example 2
A coffee beverage composition was prepared by adding baking soda to the coffee extraction treatment liquid obtained in Example 1 until the pH reached a specified value according to the formulation shown in Table 1. The coffee beverage composition was concentrated to Brix 25% using a vacuum concentrator, and a soluble coffee (instant coffee) product was obtained using a spray dryer.
6 g of soluble coffee (instant coffee) was dissolved in hot water at 80 ° C. to obtain a coffee beverage composition.

Comparative Example 1
A packaged coffee beverage was produced in the same manner as in Example 1 except that the activated carbon was not used.

Example 3
Colombian beans were roasted to L value = 22 as regular coffee beans. 130 g of coffee beans crushed to a medium grind were obtained, 40 g of the coffee beans and activated carbon (WH2CLSS, steam activated product, manufactured by Nippon Enviro) and 1040 g of 93 ° C. ion-exchanged water were added to a stirrable cylindrical container, and the temperature was maintained for 30 minutes. After extraction and cooling to 20 ° C., 1040 g of a coffee composition was obtained.
Activated carbon was removed from the treated activated carbon-containing coffee composition using a 0.5 μm filter to obtain a coffee extraction treatment liquid.

  In addition, the chlorogenic acid in the coffee solution of Examples 1-3 and the comparative example 1 was measured on the following analytical conditions, and the hydroxyhydroquinone was measured with the HPLC-electrochemical detector.

Method for Analyzing Chlorogenic Acids: Analyzing Conditions The method for analyzing chlorogenic acids in a packaged coffee beverage or coffee composition is as follows. The analytical instrument used was HPLC. The model numbers of the unit units are as follows. UV-VIS detector: L-2420 (Hitachi High-Technologies Corporation), column oven: L-2300 (Hitachi High-Technologies Corporation), pump: L-2130 (Hitachi High-Technologies Corporation), autosampler: L-2200 (Hitachi High-Technologies Corporation), column: Cadenza CD-C18 inner diameter 4.6 mm × length 150 mm, particle diameter 3 μm (intact Inc.).
The analysis conditions are as follows. Sample injection volume: 10 μL, flow rate: 1.0 mL / min, UV-VIS detector set wavelength: 325 nm, column oven set temperature: 35 ° C., eluent A: 0.05 M acetic acid, 0.1 mM 1-hydroxyethane-1 , 1-diphosphonic acid, 10 mM sodium acetate, 5 (V / V)% acetonitrile solution, eluent B: acetonitrile.

Concentration gradient condition Time Eluent A Eluent B
0.0 minutes 100% 0%
10.0 minutes 100% 0%
15.0 minutes 95% 5%
20.0 minutes 95% 5%
22.0 minutes 92% 8%
50.0 minutes 92% 8%
52.0 minutes 10% 90%
60.0 minutes 10% 90%
60.1 minutes 100% 0%
70.0 minutes 100% 0%

In HPLC, 1 g of a sample was precisely weighed, made up to 10 mL with eluent A, filtered through a membrane filter (GL chromatodisc 25A, pore size 0.45 μm, GL Sciences Inc.), and subjected to analysis.
Retention time of chlorogenic acids (unit: minutes)
(A ¹ ) Monocafe oil quinic acid: 5.3, 8.8, 11.6, total 3 points (A ² ) Ferlaquinic acid: 13.0, 19.9, 21.0, total 3 points (A ³ ) Dicaffeoylquinic acid: 36.6, 37.4, 44.2 in total. From the area values of the nine types of chlorogenic acids determined here, 5-caffeoylquinic acid was used as a standard substance, and the mass% was determined.

Analysis method of hydroxyhydroquinone by HPLC-electrochemical detector The analysis method of hydroxyhydroquinone in coffee beverage is as follows. The analytical instrument used was a Couloarray system (model 5600A, development / manufacturing: ESA, USA, import / sales: MC Medical Co., Ltd.) which is an HPLC-electrochemical detector (coulometric type). The names and model numbers of the constituent units of the apparatus are as follows.
Analytical Cell: Model 5010, Couloarray Organizer, Couloarray Electronics Module / Software: Model 5600A, Solvent Delivery Module: Model 582, Gradient Mixer, Autosampler: Model 542, Pulse Damper, Degasser: Degasys Ultimate DU3003, Column Oven : 505. Column: CAPCELL PAK C18 AQ inner diameter 4.6 mm × length 250 mm Particle diameter 5 μm (Shiseido Co., Ltd.).

The analysis conditions are as follows.
Sample injection volume: 10 μL, flow rate: 1.0 mL / min, applied voltage of electrochemical detector: 0 mV, column oven set temperature: 40 ° C., eluent A: 0.1 (W / V)% phosphoric acid, 0. 1 mM 1-hydroxyethane-1,1-diphosphonic acid, 5 (V / V)% methanol solution, eluent B: 0.1 (W / V)% phosphoric acid, 0.1 mM 1-hydroxyethane-1,1 -Diphosphonic acid, 50 (V / V)% methanol solution.

  Eluents A and B were prepared by using distilled water for high performance liquid chromatography (Kanto Chemical Co., Ltd.), methanol for high performance liquid chromatography (Kanto Chemical Co., Ltd.), phosphoric acid (special grade, Wako Pure Chemical Industries, Ltd.) )), 1-hydroxyethane-1,1-diphosphonic acid (60% aqueous solution, Tokyo Chemical Industry Co., Ltd.).

Concentration gradient condition Time Eluent A Eluent B
0.0 minutes 100% 0%
10.0 minutes 100% 0%
10.1 min 0% 100%
20.0 minutes 0% 100%
20.1 minutes 100% 0%
50.0 minutes 100% 0%

  The analysis sample was prepared and analyzed in the following procedure. After accurately weighing 5 g of the sample, it was made up to 10 mL with 0.5 (W / V)% phosphoric acid, 0.5 mM 1-hydroxyethane-1,1-diphosphonic acid, 5 (V / V)% methanol solution. The solution was centrifuged to obtain a supernatant. This supernatant was passed through Bond Elut SCX (solid phase filling amount: 500 mg, reservoir volume: 3 mL, GL Sciences Inc.), and about 0.5 mL of the first passage solution was removed to obtain a passage solution. The passing liquid was filtered through a membrane filter (GL chromatodisc 25A, pore size 0.45 μm, GL Sciences Inc.) and immediately subjected to analysis.

  In the analysis under the above conditions of the HPLC-electrochemical detector, the retention time of hydroxyhydroquinone was 6.38 minutes. From the obtained peak area value, mass% was determined using hydroxyhydroquinone (Wako Pure Chemical Industries, Ltd.) as a standard substance.

(Evaluation of clean feeling)
Sensory evaluation was carried out by five professional panelists, and a five-step evaluation of 1 (not refreshing) to 5 (strong feeling of refreshing) was performed.

Example 4
Filled with 2 g of activated carbon (WH2CLSS, particle size 200-400 μm, manufactured by Nippon Enviro) into a bag made of nonwoven fabric, heat-sealed the activated carbon inlet to prevent the activated carbon from leaking, and attached a string or holding paper to a commercial coffee drink (soluble coffee) It was set as a bag-type porous adsorbent holding tool for a dissolving liquid, a can or a coffee drink packed in a PET container (see FIG. 4).

Example 5
Activated carbon fiber was formed into a paper filter shape of Carita 102 (for 2 to 4 persons) to obtain a filter type porous adsorbent holding tool.
Colombian beans were roasted to L value = 24 as regular coffee beans to obtain 40 g of coffee beans that were finely ground.
Two pieces of the filter hydroxyhydroquinone removal tool (see FIG. 5) are laminated in a paper filter, and the coffee beans are extracted using a coffee maker (NC-471M, extraction temperature of about 90 ° C.) manufactured by Matsushita Electric Industrial Co., Ltd. A coffee extraction treatment liquid was obtained using 400 g of ion-exchanged water.

Activated carbon fiber: Toho Rayon FE-200 (activated carbon fiber felt)
Results of pore volume measurement by BELSORP-mini Total pore volume 0.379 mL / g, 0.7 nm or less pore volume 0.345 mL / g
Pore volume by MP method 0.356mL / g
Average pore radius in the micropore region 0.3 nm
0.7 nm or less pore volume / total pore volume = 92%
0.2-0.7 nm pore volume / total pore volume = 92%

Example 6
A coffee extraction treatment liquid was obtained in the same manner as in Example 5 except that the activated carbon fiber was changed to the following varieties.
Activated carbon fiber: Toho Rayon FE-400 (activated carbon fiber felt)
Results of pore volume measurement by BELSORP-mini Total pore volume 0.759 mL / g, 0.7 nm or less pore volume 0.521 mL / g
MP94 pore volume 0.594mL / g
Average pore radius in the micropore region 0.4 nm
0.7 nm or less pore volume / total pore volume = 69%
0.2-0.7 nm pore volume / total pore volume = 69%

Comparative Example 2
A coffee extraction treatment liquid was obtained in the same manner as in Example 5 except that the activated carbon fiber was not used.

  Table 2 shows the amounts of chlorogenic acids and hydroxyhydroquinone in the coffee compositions obtained in Example 5 and Comparative Example 2. In sensory evaluation, in Examples 5 and 6, the evaluation was 4 and the flavor was good, but in Comparative Example 2, it was not preferable in Evaluation 2.

Example 7
The activated carbon fiber was fixed (adhered or fused) to a plastic container through which liquid can be passed to obtain a filter-type porous adsorbent holding tool (FIG. 6). Note that the plastic container has a handle and a guide portion that matches the inner diameter of the cup.

Example 8
A bag type with 50g of activated carbon (WH2C SS, particle size 200-400μm, manufactured by Nippon Enviro) in a non-woven bag (Fig. 7) that has liquid permeability and does not leak from the inside of the bag. A porous adsorbent holding tool was obtained. One bag-type porous adsorbent holding tool was put into a container containing 1000 mL of coffee extract, and left in a refrigerator at 5 ° C. for 12 hours to obtain a coffee extract processing solution.

Nippon Enviro activated carbon: WH2C 42/80 SS (particle size 200-400 μm)
Results of pore volume measurement by BELSORP-mini Total pore volume 0.699 mL / g, 0.7 nm or less pore volume 0.463 mL / g
MP72 pore volume 0.472 mL / g
Average pore radius in the micropore region 0.3 nm
0.7 nm or less pore volume / total pore volume = 78%
0.2-0.7 nm pore volume / total pore volume = 78%

Example 9
A container containing 1000 mL of coffee extract is filled with 50 g of activated carbon (EHS SS, particle size 50 to 100 μm, manufactured by Nippon Enviro) and is a bag-type porous adsorbent holding tool. A non-woven fabric bag (FIG. 7) having a structure with no ink was attached and left in a refrigerator at 5 ° C. for 12 hours to obtain a coffee extraction treatment liquid.

Nippon Enviro Activated Carbon: EHSS (particle size 50-100 μm)
Results of pore volume measurement by BELSORP-mini Total pore volume 0.618 mL / g, 0.7 nm or less pore volume 0.503 mL / g
Pore volume by MP method 0.514mL / g
Average pore radius in the micropore region 0.3 nm
0.7 nm or less pore volume / total pore volume = 81%
0.2-0.7 nm pore volume / total pore volume = 81%

Example 10
A container containing 1000 mL of coffee extract was attached as a molded porous adsorbent holding tool filled with 10 g of activated carbon fibers (FIG. 8), and left in a refrigerator at 5 ° C. for 12 hours to obtain a coffee extract processing solution.

Activated carbon fiber: KURAACTIVE FT305-20 (activated carbon fiber felt), Kuraray BELSORP-mini pore volume measurement result Total pore volume 0.920 mL / g, 0.7 nm or less pore volume 0.825 mL / g
MP44 pore volume 0.844mL / g
Average pore radius in the micropore region 0.4 nm
0.7 nm or less pore volume / total pore volume = 90%
0.2-0.7 nm pore volume / total pore volume = 90%

Comparative Example 3
A container containing 1000 mL of coffee extract was left in a refrigerator at 5 ° C. for 12 hours.

  Table 3 shows the analysis results of chlorogenic acids and hydroxyhydroquinone in the coffee compositions obtained in Examples 8 to 10 and Comparative Example 3. In sensory evaluation, in Examples 8, 9, and 10, the evaluation was 4 and the flavor was good, but in Comparative Example 3, it was not preferable in Evaluation 2.

Example 11
Colombian beans were roasted to L value = 24 as regular coffee beans to obtain 40 g of coffee beans that were finely ground.
The following granular activated carbon 16 g and the above ground beans are mixed in a paper filter of Carita 102, and 400 g of the coffee beans are extracted using a coffee maker (NC-471M, extraction temperature about 90 ° C.) manufactured by Matsushita Electric Industrial Co., Ltd. A coffee extraction solution was obtained using ion-exchanged water.
Granular activated carbon: EHSS made by Nippon Enviro (particle size 50-100μm)
Results of pore volume measurement by BELSORP-mini Total pore volume 0.618 mL / g, 0.7 nm or less pore volume 0.503 mL / g
Pore volume by MP method 0.514mL / g
Average pore radius in the micropore region 0.3 nm
0.7 nm or less pore volume / total pore volume = 81%
0.2-0.7 nm pore volume / total pore volume = 81%

Comparative Example 4
A coffee extraction treatment liquid was obtained in the same manner as in Example 11 except that the activated carbon was changed to the following.
Granular activated carbon: KL Made by Nippon Enviro (particle size 500-2000 μm)
Results of pore volume measurement by BELSORP-mini Total pore volume 2.051 mL / g, 0.7 nm or less pore volume 0.479 mL / g
Pore volume by MP method 0.771mL / g
Average pore radius in the micropore region 0.6 nm
0.7 nm or less pore volume / total pore volume = 23%
0.2-0.7 nm pore volume / total pore volume = 23%

  Table 4 shows the analysis results of chlorogenic acids and hydroxyhydroquinone in the coffee compositions obtained in Example 11 and Comparative Example 4. In sensory evaluation, in Example 11, evaluation was 4 and the flavor was good, but in Comparative Example 4, evaluation 2 was not preferable.

Reference example 1
20 g of commercial instant coffee (Nescafe (registered trademark) Gold Blend Red Label, Nestlé Japan)) was dissolved in 1400 mL of distilled water to obtain a raw coffee solution. As a result of HPLC analysis, the raw coffee solution contained 660 ppm of chlorogenic acid and 5.0 ppm of hydroxyhydroquinone.
To 1400 mL of this raw coffee solution, 30 g of activated carbon white WH2C 28/42 (Nippon EnviroChemicals, Inc.) was added and stirred for 1 hour, and then filtered using a membrane filter (0.45 μm). About 1300 mL of coffee solution was obtained. As a result of HPLC analysis, chlorogenic acid was contained at 590 ppm, but no hydroxyhydroquinone peak was detected.
Further, the obtained filtrate was freeze-dried to obtain 15.8 g of soluble coffee powder.

Reference example 2
Evaluation of blood pressure lowering of coffee powder prepared in Reference Example 1 i) Experimental materials and methods (a) 13-14 weeks old male spontaneously hypertensive rats (SHR) preliminarily commercially available for 5 consecutive days The blood pressure measurement was carried out by using a blood pressure measuring apparatus (manufactured by Softron Co., Ltd.) to sufficiently familiarize the rat with the blood pressure operation, and then the evaluation test was measured. All rats were housed under conditions of 25 ± 1 ° C., 55 ± 10% relative humidity, and 12 hours of illumination (7 am to 7 pm) (rat room breeding room).
(B) Administration method and dose: In the test group, the coffee powder (activated carbon coffee) prepared in Example 1 was used. The control group used commercial instant coffee. Activated charcoal-treated coffee and instant coffee were each dissolved in physiological saline to prepare a total chlorogenic acid amount of 200 mg / kg. The administration method was oral administration using an oral sonde. The dose was 5 mL / kg.

(C) Test method: 4 to 6 SHRs were used per group. The systolic blood pressure of the tail vein before and 12 hours after oral administration was measured, and the blood pressure change rate after 12 hours was calculated from the blood pressure before administration.
(D) Statistical processing method: The measurement results obtained were subjected to Student's t-test representing the mean value and standard error, and the significance level was 5%.

ii) Results As is apparent from Table 5, when the coffee obtained according to the present invention was ingested, a significant decrease in blood pressure was observed as compared with the case of ingesting ordinary instant coffee.

A specific example of the batch type extraction method will be shown. A specific example of the column type extraction method is shown. A specific example of the drip extraction method will be shown. The specific example of a bag type porous adsorbent holding tool is shown. The specific example of a filter type | mold porous adsorption body holding tool is shown. The specific example of a filter type | mold porous adsorption body holding tool is shown. The specific example of a bag type porous adsorbent holding tool is shown. The specific example of a molded object type | mold porous adsorption body holding tool is shown.

Claims (9)

  In the presence of a porous adsorbent whose pore radius is 0.7 nanometers (nm) or less and whose pore volume is 30% or more of the total pore volume of the porous adsorbent, the coffee extract is removed from the coffee beans. A method for producing a coffee composition to be extracted. Extracting coffee extract from coffee beans, and cooling the extract with a pore radius of 0.7 nanometers (nm) or less has a pore volume of 30% or more of the total pore volume of the porous adsorbent The manufacturing method of the coffee composition made to contact the porous adsorbent which is.   The porous adsorbent is a porous adsorbent in which the volume of pores having a pore radius of 0.7 nanometer (nm) or less is 30 to 98% of the total pore volume of the porous adsorbent. Or the manufacturing method of the coffee composition of 2.   The method for producing a coffee composition according to any one of claims 1 to 3, wherein an average pore radius in a micropore region of the porous adsorbent is 0.2 to 0.5 nanometer (nm). The manufacturing method of soluble coffee which spray-drys or freeze-drys the coffee composition of any one of Claims 1-4.   In the presence of a porous adsorbent whose pore radius is 0.7 nanometers (nm) or less and whose pore volume is 30% or more of the total pore volume of the porous adsorbent, the coffee extract is removed from the coffee beans. A method for producing a coffee composition which is extracted and contains 0.01 to 1% by mass of chlorogenic acids and the content of hydroxyhydroquinone is less than 0.1% by mass of the amount of chlorogenic acids.   Extracting coffee extract from coffee beans, and cooling the extract with a pore radius of 0.7 nanometers (nm) or less has a pore volume of 30% or more of the total pore volume of the porous adsorbent A method for producing a coffee composition, which is brought into contact with a porous adsorbent, and contains 0.01 to 1% by mass of chlorogenic acids, and the content of hydroxyhydroquinone is less than 0.1% by mass of the amount of chlorogenic acids.   In the presence of a porous adsorbent whose pore radius is 0.7 nanometers (nm) or less and whose pore volume is 30% or more of the total pore volume of the porous adsorbent, the coffee extract is removed from the coffee beans. To obtain a coffee composition containing 0.01 to 1% by mass of chlorogenic acids and having a hydroxyhydroquinone content of less than 0.1% by mass of the chlorogenic acids, and then spray drying or A method for producing soluble coffee to be freeze-dried.   Extracting coffee extract from coffee beans, and cooling the extract with a pore radius of 0.7 nanometers (nm) or less has a pore volume of 30% or more of the total pore volume of the porous adsorbent To obtain a coffee composition containing 0.01 to 1% by mass of chlorogenic acids and having a hydroxyhydroquinone content of less than 0.1% by mass of the chlorogenic acids, Next, a method for producing soluble coffee, wherein the coffee composition is spray-dried or freeze-dried.