JP6139219B2 - Containerized coffee beverage - Google Patents

Description

  The present invention relates to a packaged coffee beverage.

  Coffee beverages are widely favored as taste beverages, and are usually produced by blending coffee extracts. The flavors of coffee beverages include bitterness, sourness, sweetness, richness, aroma, and the like, and these flavors are characterized by roasted coffee beans used for the production of coffee extracts.

It is known that the flavor of the container-packed coffee beverage is inferior to that of regular coffee, and as an improvement method, heating is performed by adding ethyl isovalerate (Patent Document 1) or by adding L-histidine hydrochloride. A method for suppressing a sterilizing odor (Patent Document 2) is known.
Moreover, in roasting green coffee beans, it is known that free asparagine contained in green coffee beans is decomposed during roasting to produce acrylamide (Patent Document 3). The relationship is not known.

  Further, caffeine is known as a bitter component of a coffee beverage, and chlorogenic acids are also known as components having health effects.

JP 2010-75177 A JP 2005-137266 A JP-T-2006-503592

The present inventors have studied to develop a container-packed coffee beverage with high palatability. However, when the container-packed coffee beverage was sterilized by heating, it was found that the sourness and bitterness were excessively felt, and that the off-flavor was easily manifested when the chlorogenic acids were at a high concentration.
An object of the present invention is to provide a container-packed coffee beverage with good sourness and bitterness after heat sterilization.

  As a result of studying in view of the above problems, the present inventors have controlled the content of chlorogenic acids and the mass ratio of specific components to the chlorogenic acids within a specific range in a packaged coffee beverage containing a high concentration of chlorogenic acids. As a result, it was found that a container-packed coffee beverage having good sourness and bitterness after heat sterilization can be obtained.

That is, the present invention includes the following components (A), (B) and (C);
(A) Chlorogenic acids: 0.14 to 0.28% by mass
(B) contains caffeine (C) acrylamide,
The mass ratio [(B) / (A)] of the component (A) and the component (B) is 0.01 to 0.5, and the mass ratio of the component (A) and the component (C) [(C ) / (A)] is 10 × 10 ⁻⁶ or less,
A heat-sterilized containerized coffee beverage is provided.

The present invention also provides the following components (A), (B) and (C);
(A) Chlorogenic acids: 0.14 to 0.28% by mass
(B) A method for improving the bitterness of a heat-sterilized container-packed coffee beverage containing caffeine (C) acrylamide,
The mass ratio [(B) / (A)] of the component (A) to the component (B) is set to 0.01 to 0.5, and the mass ratio of the component (A) to the component (C) [(C) / (A)] is adjusted to 10 × 10 ⁻⁶ or less, and a method for improving bitterness sharpness is provided.

  According to the present invention, it is possible to provide a container-packed coffee beverage having good sourness and bitterness after heat sterilization. Moreover, according to this invention, the improvement method of the bitterness of the heat-sterilized container-packed coffee drink can be provided.

  The container-packed coffee beverage of the present invention contains chlorogenic acids as the component (A). Here, in this specification, “chlorogenic acids” means 3-caffeoylquinic acid, 4-caffeoylquinic acid and mono-caffeoylquinic acid of 5-caffeoylquinic acid, 3-ferlaquinic acid and 4-ferlaquina. It is a collective term for acid and monoferlaquinic acid such as 5-ferlaquinic acid, and in the present invention, at least one of the above six species may be contained.

  Although content of the component (A) in the container-packed coffee drink of this invention is 0.14-0.28 mass%, from a viewpoint of physiological activity, the improvement of a sharpness of a sour taste, and the improvement of a bitterness, it is 0.15. % By mass or more is preferable, 0.16% by mass or more is more preferable, 0.18% by mass or more is more preferable, and from the viewpoint of sourness reduction, improvement of sourness sharpness and bitterness, 0.26% by mass or less is Preferably, 0.24 mass% or less is more preferable, and 0.22 mass% or less is still more preferable. As a range of content of the component (A) in the container-packed coffee drink of this invention, Preferably it is 0.15-0.26 mass%, More preferably, it is 0.16-0.24 mass%, More preferably, it is 0. 18 to 0.22% by mass. In addition, content of a component (A) is defined based on the said 6 types total amount, and the analysis of a component (A) shall follow the method as described in an Example mentioned later.

  Further, the container-packed coffee beverage of the present invention contains caffeine as the component (B), and from the viewpoint of improving bitterness sharpness, the mass ratio of the component (A) to the component (B) [(B) / (A )] Is controlled to 0.01 to 0.5. The mass ratio [(B) / (A)] is preferably 0.4 or less, more preferably 0.3 or less, still more preferably 0.25 or less, from the viewpoint of further improving bitterness sharpness. The following is more preferable, and from the viewpoint of the flavor balance between acidity and bitterness, 0.02 or more is preferable, 0.04 or more is more preferable, 0.06 or more is further preferable, and 0.08 or more is even more preferable. The range of the mass ratio [(B) / (A)] in the containerized coffee beverage of the present invention is preferably 0.02 to 0.4, more preferably 0.04 to 0.3, still more preferably 0. 0.06 to 0.25, more preferably 0.08 to 0.2.

  The content of the component (B) in the container-packed coffee beverage of the present invention is preferably 400 ppm by mass or less, more preferably 375 ppm by mass or less, still more preferably 350 ppm by mass or less, from the viewpoint of improving bitterness. Mass ppm or less is still more preferred, 300 mass ppm or less is more preferred, and from the viewpoint of imparting bitterness, 50 mass ppm or more is preferred, 75 mass ppm or more is more preferred, 100 mass ppm or more is more preferred, 125 mass ppm. The above is more preferable, and 150 mass ppm or more is even more preferable. As a range of content of the component (B) in the container-packed coffee drink of this invention, Preferably it is 50-400 mass ppm, More preferably, it is 75-375 mass ppm, More preferably, it is 100-350 mass ppm, More preferably Is 125-325 mass ppm, more preferably 150-300 mass ppm. In addition, the analysis of a component (B) shall follow the method as described in an Example mentioned later.

Furthermore, although the container-packed coffee drink of this invention contains acrylamide as a component (C), the mass ratio with respect to the component (A) of the said acrylamide is significantly reduced rather than the quantity normally contained in a coffee drink. Specifically, the mass ratio [(C) / (A)] of the component (A) to the component (C) is 10 × 10 ⁻⁶ or less, but 9 × 10 6 from the viewpoint of improving sourness sharpness. ⁻⁶ or less is preferable, 8 × 10 ⁻⁶ or less is more preferable, and 7 × 10 ⁻⁶ or less is more preferable. The mass ratio [(C) / (A)] may be 0, but is preferably 0.5 × 10 ⁻⁶ or more and more preferably 1.0 × 10 ⁻⁶ or more from the viewpoint of production efficiency. Preferably, 1.5 × 10 ⁻⁶ or more is more preferable. The range of the mass ratio [(C) / (A)] in the containerized coffee beverage of the present invention is preferably 0.5 × 10 ^{−6 to} 9 × 10 ⁻⁶ , more preferably 1.0 × 10 ^{−. 6 ~8} × 10 ^-6, more preferably from ^{1.5 × 10 -6 ~7 × 10 -6} .

  0.03 mass ppm or less is preferable, as for content of the component (C) in the container-packed coffee drink of this invention, 0.025 mass ppm or less is more preferable, and 0.02 mass ppm or less is still more preferable. The content of the component (C) in the container-packed coffee beverage of the present invention may be 0 ppm by mass, but is preferably 0.001 ppm by mass or more, and 0.002 ppm by mass from the viewpoint of production efficiency. The above is more preferable, and 0.003 mass ppm or more is even more preferable. As a range of content of the component (C) in the container-packed coffee drink of this invention, Preferably it is 0.001-0.03 mass ppm, More preferably, it is 0.002-0.025 mass ppm, More preferably, it is 0. 0.003 to 0.02 mass ppm. The component (C) can be analyzed by the method described in Food Additives and Contaninants, Vol. 29, No. 5, 2012, 705-715. Follow the method described in the examples. In the analysis of the component (C), the content of 0 mass ppm is a concept including the case where the component is below the detection limit.

  From the viewpoint of flavor, the container-packed coffee beverage of the present invention preferably has an acidic liquidity. Specifically, the pH (20 ° C.) is preferably 4.5 or more, more preferably 4.8 or more. 5.1 or more is more preferable, 6.9 or less is preferable, 6.8 or less is more preferable, and 6.7 or less is more preferable. The range of pH (20 ° C.) is preferably 4.5 to 6.9, more preferably 4.8 to 6.8, and still more preferably 5.1 to 6.7.

  From the viewpoint of providing richness, the container-packed coffee beverage of the present invention has a Brix (20 ° C.) of preferably 0.8 or more, more preferably 0.9 or more, still more preferably 1.0 or more, and 1.1 or more. More preferably, it is preferably 3.0 or less, more preferably 2.5 or less, and further preferably 2.3 or less. The range of Brix is preferably 0.8 to 3.0, more preferably 0.9 to 2.5, still more preferably 1.0 to 2.5, and still more preferably 1.1 to 2.3. is there.

  In such a container-packed coffee beverage, for example, the content of the component (A), the mass ratio [(B) / (A)], and the mass ratio [(C) / (A)] are controlled within the above ranges. It is possible to prepare the coffee extract as it is or after diluting it with water, and the content, mass ratio [(B) / (A)] and mass ratio [(C) / (A )] Is within the above range, other coffee extracts may be blended if desired.

  The coffee extract in which the content of the component (A), the mass ratio [(B) / (A)] and the mass ratio [(C) / (A)] are controlled within the above ranges is, for example, (i) raw material The coffee bean extract is subjected to various chromatographies such as reverse phase chromatography and liquid chromatography to fractionate components (B) and (C), and the mass ratio in the raw coffee bean extract [(B) / (A )] And the mass ratio [(C) / (A)] are controlled within the above range, or (ii) roasted coffee beans and activated carbon whose roasting degree and average particle size are controlled within a specific range. Prepared in the same container, supply the extraction solvent into the container to obtain a coffee extract, contact the coffee extract with activated carbon in the container, the amount of each component extracted from roasted coffee beans and It can be obtained by controlling the amount of adsorption to activated carbon. In the method (i), a known method can be appropriately employed as the fractionation method. Hereinafter, the method (ii) will be described.

The roasted coffee beans used in the present invention have an average particle size of preferably 0.90 to 1.40 mm, more preferably 0.96 to 1.33 mm. Here, the “average particle size” in this specification refers to a particle size obtained based on 6.3 of JIS K1474, then a particle size distribution obtained based on 6.4, and further based on 7) of the same item b). It means the calculated mass average particle diameter.
The roasted coffee beans have an L value measured by a color difference meter of preferably 15 to 60, more preferably 20 to 35, still more preferably 23 to 33, and coffee beans having different roasting degrees are mixed and used. You can also When coffee beans having different roasting degrees are mixed and used, the roasting degree of roasted coffee beans is a value obtained by multiplying the L value of roasted coffee beans to be used by the content ratio of the roasted coffee beans. For example, two or more roasted coffee beans having an L value of preferably 10 to 60, more preferably 15 to 35, are used so that the average value of the L values is within the above range. be able to. Moreover, the roasting method and roasting conditions are not particularly limited. Examples of the bean type of coffee beans include Arabica, Robusta, and Reberica, and can be used alone or in combination of two or more.

  The activated carbon used in the present invention has an average particle size of preferably 0.30 to 0.60 mm, more preferably 0.32 to 0.45 mm. The “average particle diameter” here is also a mass average particle diameter calculated based on JIS K1474. In addition, wood (for example, sawdust), coal, coconut shell, etc. are mentioned as a starting material of activated carbon, Among these, coconut shell activated carbon is preferable. Moreover, activated carbon activated by a gas such as water vapor or chemicals may be used, and among them, water vapor activated activated carbon is preferable. The amount of activated carbon used is preferably 10 to 35% by mass, more preferably 20 to 28% by mass, based on roasted coffee beans.

  The roasted coffee beans and activated carbon whose average particle size is controlled may be obtained by crushing roasted coffee beans and activated carbon as necessary, and sieving them to obtain a desired average particle size. The pulverization method is not particularly limited, and a known method and apparatus can be used. For classification of roasted coffee beans and activated carbon, for example, a sieve made by Tyler (JIS Z 8801-1) can be used.

Next, the roasted coffee beans and activated carbon are charged into a container. Examples of the container include a drip extractor and a column extractor.
Alternatively, after the activated carbon is charged into the container and before the roasted coffee beans are charged, the activated carbon may be washed by passing water through the container. The water used for cleaning is discharged outside the container. The temperature of water is preferably 60 to 100 ° C, more preferably 70 to 95 ° C. The amount of water used for washing is preferably 5 to 200 times by mass, more preferably 15 to 50 times by mass with respect to the activated carbon.

Next, the extraction solvent is supplied into a container charged with roasted coffee beans and activated carbon.
As the extraction solvent, water is preferable from the viewpoint of flavor, and tap water, natural water, distilled water, ion-exchanged water and the like can be appropriately selected and used. The temperature of the extraction solvent is preferably 70 to 90 ° C, more preferably 77 to 87 ° C.

  Further, after supplying a certain amount of the extraction solvent to the roasted coffee beans, the supply of the extraction solvent may be stopped and the state may be maintained for a predetermined time. In this case, the supply amount of the extraction solvent is preferably 0.5 to 10 times the mass of the roasted coffee beans, and the retention time is preferably 1 to 20 minutes, more preferably 5 from the viewpoint of flavor. ~ 16 minutes.

Next, the coffee extract is discharged out of the container, but it is preferable to stop the discharge when the extraction ratio of the coffee extract, that is, the amount of the coffee extract substance / the roasted coffee bean mass reaches a predetermined amount. The extraction ratio of the coffee extract is preferably 1 to 15 times by mass and more preferably 4 to 12 times by mass with respect to roasted coffee beans.
The discharged coffee extract may be treated by filtration, centrifugation, or the like as necessary after cooling.

  Thus, usually, the coffee extract in which the content of the component (A), the mass ratio [(B) / (A)] and the mass ratio [(C) / (A)] are controlled within the above ranges is used. Although it can obtain, about the obtained coffee extract, it analyzes about content of a component (A), mass ratio [(B) / (A)], and mass ratio [(C) / (A)], these Can be selected within the above range.

  In addition, the container-packed coffee beverage of the present invention, if necessary, sweetener, milk component, antioxidant, fragrance, organic acid, organic acid salt, inorganic acid, inorganic acid salt, inorganic salt, pigment, emulsifier, storage One or more additives such as a seasoning, seasoning, acidulant, amino acid, pH adjuster, and quality stabilizer may be blended. The packaged coffee beverage of the present invention may be a packaged black coffee beverage or a packaged milk coffee beverage.

The container-packed coffee beverage of the present invention is one that has been sterilized by heating, but the sterilization method is particularly limited as long as the sterilization method is performed under the sterilization conditions stipulated in applicable laws and regulations (the Food Sanitation Law in Japan). Is not to be done.
The container-packed coffee beverage of the present invention is filled into a normal packaging container such as a molded container (so-called PET bottle) mainly composed of polyethylene terephthalate, a metal can, a paper container combined with a metal foil or a plastic film, or a bottle. For example, retort sterilization can be used when the container can be sterilized by heating after filling the container with a coffee beverage like a metal can. As for PET bottles and paper containers that cannot be sterilized by retort, the aseptic is used to pre-heat coffee sterilized by a method such as UHT sterilization under the same sterilization conditions as above and then sterilize in a sterile environment. Filling, hot pack filling, or the like can be employed.

Next, a method for improving the bitterness of the heat-sterilized containerized coffee beverage will be described.
The method for improving the bitterness of a heat-sterilized container-packed coffee beverage of the present invention is a heating containing 0.14 to 0.28% by mass of (A) chlorogenic acids, (B) caffeine and (C) acrylamide. In the sterilized container-packed coffee beverage, the mass ratio [(B) / (A)] of the component (A) to the component (B) is 0.01 to 0.5, the component (A) and the component (C) The mass ratio [(C) / (A)] is adjusted to 10 × 10 ⁻⁶ or less. Preferred embodiments of the content of the component (A), the mass ratio [(B) / (A)], and the mass ratio [(C) / (A)] are as described above.
Moreover, in the improvement method of the bitterness of the container-packed coffee beverage of the present invention, it is possible to adjust pH from the viewpoint of flavor and Brix from the viewpoint of imparting richness. The preferred embodiments of pH and Brix in the packaged coffee beverage are as described above.

  That is, the present invention further discloses the following heat-sterilized container-packed coffee beverage and a method for improving the bitterness of the bitterness relating to the above embodiment.

<1>
The following components (A), (B) and (C);
(A) Chlorogenic acids: 0.14 to 0.28% by mass
(B) contains caffeine (C) acrylamide,
The mass ratio [(B) / (A)] of the component (A) and the component (B) is 0.01 to 0.5, and the mass ratio of the component (A) and the component (C) [(C ) / (A)] is 10 × 10 ⁻⁶ or less,
Heat-sterilized containerized coffee beverage.

<2>
The following components (A), (B) and (C);
(A) Chlorogenic acids: 0.14 to 0.28% by mass
(B) A method for improving the bitterness of a heat-sterilized container-packed coffee beverage containing caffeine (C) acrylamide,
The mass ratio [(B) / (A)] of the component (A) to the component (B) is set to 0.01 to 0.5, and the mass ratio of the component (A) to the component (C) [(C) / (A)] is improved to 10 × 10 ⁻⁶ or less, respectively, to improve bitterness sharpness.

<3>
(A) The chlorogenic acids are preferably at least one selected from 3-caffeoylquinic acid, 4-caffeoylquinic acid, 5-caffeoylquinic acid, 3-ferlaquinic acid, 4-ferlaquinic acid and 5-ferlaquinic acid. The above-described <1> heat-sterilized container-packed coffee beverage or <2> the method for improving the bitterness-crisp (hereinafter, “the heat-sterilized container-packed coffee beverage or the method for improving the bitterness-crisp”) Are referred to as “contained coffee beverages”).
<4>
(A) The content of chlorogenic acids is preferably 0.15% by mass or more, more preferably 0.16% by mass or more, still more preferably 0.18% by mass or more, and preferably 0.26% by mass or less. More preferably, it is 0.24 mass% or less, More preferably, it is 0.22 mass% or less, The container-packed coffee drink as described in any one of said <1>-<3> etc.
<5>
(A) The content of chlorogenic acids is preferably 0.15 to 0.26% by mass, more preferably 0.16 to 0.24% by mass, and still more preferably 0.18 to 0.22% by mass. The container-packed coffee drink according to any one of <1> to <4>.
<6>
The mass ratio [(B) / (A)] is preferably 0.4 or less, more preferably 0.3 or less, still more preferably 0.25 or less, still more preferably 0.2 or less, preferably The container-packed coffee according to any one of <1> to <5>, which is 0.02 or more, more preferably 0.04 or more, still more preferably 0.06 or more, and still more preferably 0.08 or more. Beverages etc.
<7>
The mass ratio [(B) / (A)] is preferably 0.02 to 0.4, more preferably 0.04 to 0.3, still more preferably 0.06 to 0.25, and still more preferably 0. The container-packed coffee drink according to any one of <1> to <6>, which is 0.08 to 0.2.
<8>
(B) The content of caffeine is preferably 400 mass ppm or less, more preferably 375 mass ppm or less, still more preferably 350 mass ppm or less, still more preferably 325 mass ppm or less, and still more preferably 300 mass ppm or less. Preferably, it is 50 mass ppm or more, more preferably 75 mass ppm or more, still more preferably 100 mass ppm or more, still more preferably 125 mass ppm or more, still more preferably 150 mass ppm or more, <1 > To <7> The container-packed coffee drink according to any one of the above.
<9>
(B) The content of caffeine is preferably 50 to 400 ppm by mass, more preferably 75 to 375 ppm by mass, still more preferably 100 to 350 ppm by mass, still more preferably 125 to 325 ppm by mass, and still more preferably. The container-packed coffee beverage or the like according to any one of <1> to <8>, which is 150 to 300 ppm by mass.
<10>
The mass ratio [(C) / (A)] is preferably 9 × 10 ⁻⁶ or less, more preferably 8 × 10 ⁻⁶ or less, still more preferably 7 × 10 ⁻⁶ or less, preferably 0 or more, More preferably 0.5 × 10 ⁻⁶ or more, ^still more preferably 1.0 × 10 ⁻⁶ or more, and even more preferably 1.5 × 10 ⁻⁶ or more, any one of <1> to <9> The packaged coffee drink according to 1.

<11>
The mass ratio [(C) / (A)] is preferably 0.5 × 10 ^{−6 to} 9 × 10 ⁻⁶ , more preferably 1.0 × 10 ⁻⁶ to 8 × 10 ⁻⁶ , and still more preferably 1. The container-packed coffee beverage or the like according to any one of <1> to <10>, which is 5 × 10 ^{−6 to} 7 × 10 ⁻⁶ .
<12>
(C) The content of acrylamide is preferably 0.03 mass ppm or less, more preferably 0.025 mass ppm or less, still more preferably 0.02 mass ppm or less, preferably 0 mass ppm or more, more preferably Is 0.001 mass ppm or more, more preferably 0.002 mass ppm or more, and still more preferably 0.003 mass ppm or more, and the container-packed coffee beverage according to any one of the above <1> to <11> etc.
<13>
The content of (C) acrylamide is preferably 0.001 to 0.03 mass ppm, more preferably 0.002 to 0.025 mass ppm, and still more preferably 0.003 to 0.02 mass ppm. <1>-<12> The container-packed coffee drink as described in any one of <12>.
<14>
The pH (20 ° C.) is preferably 4.5 or more, more preferably 4.8 or more, still more preferably 5.1 or more, preferably 6.9 or less, more preferably 6.8 or less, still more preferably Is 6.7 or less, the container-packed coffee drink according to any one of <1> to <13>.
<15>
The pH (20 ° C.) is preferably 4.5 to 6.9, more preferably 4.8 to 6.8, and still more preferably 5.1 to 6.7, in the above <1> to <14> A packaged coffee drink or the like according to any one of the above.
<16>
Brix (20 ° C.) is preferably 0.8 or more, more preferably 0.9 or more, still more preferably 1.0 or more, still more preferably 1.1 or more, preferably 3.0 or less, more The container-packed coffee drink according to any one of <1> to <15>, which is preferably 2.5 or less, more preferably 2.3 or less.
<17>
Brix (20 ° C.) is preferably 0.8 to 3.0, more preferably 0.9 to 2.5, still more preferably 1.0 to 2.5, and still more preferably 1.1 to 2.3. The container-packed coffee drink according to any one of <1> to <16>.
<18>
The packaged coffee beverage according to any one of <1> to <17>, wherein the packaged coffee beverage is preferably a packaged black coffee beverage or a packaged milk coffee beverage.
<19>
The container stuffing according to any one of the above items <1> to <18>, wherein the heat sterilization is preferably performed under sterilization conditions stipulated in applicable regulations (Food Sanitation Law in Japan). Coffee drinks etc.
<20>
The packaged coffee drink according to any one of <1> to <19>, wherein the heat sterilization is preferably retort sterilization or UHT sterilization.

<21>
Furthermore, preferably sweeteners, milk ingredients, antioxidants, fragrances, organic acids, organic acid salts, inorganic acids, inorganic acid salts, inorganic salts, pigments, emulsifiers, preservatives, seasonings, acidulants, amino acids, pH Heat-sterilized container-packed coffee drink according to any one of <1> and <3> to <20>, which contains one or more additives selected from a regulator and a quality stabilizer .

1. Determination of chlorogenic acids and caffeine HPLC was used as an analytical instrument. The model numbers of the constituent units of the apparatus 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 Co.).
·Detector

The analysis conditions are as follows.
-Sample injection volume: 10 μL,
-Flow rate: 1.0 mL / min,
UV-VIS detector setting wavelength: 325 nm,
-Column oven set temperature: 35 ° C
Eluent A: 0.05M 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 6 types of chlorogenic acids / monocaffeoylquinic acid: 5.3 minutes, 8.8 minutes, 11.6 minutes, 3 points in total, monoferlaquinic acid: 13.0 minutes, 19.9 minutes 3 points in total for 21.0 minutes From the area values of the six types of chlorogenic acids determined here, 5-caffeoylquinic acid was used as a standard substance, and mass% was determined.
The analysis of caffeine was carried out in the same manner as chlorogenic acids except that UV-VIS detector set wavelength: 270 nm and caffeine was used as a standard substance. Caffeine retention time is 18.9 minutes.

2. Quantitative analysis of acrylamide After precisely weighing 3.0 g of sample, 100 mL of water, 20 mL of hexane and an internal standard substance (d ₃ -acrylamide) were added and extracted, and after centrifugation, the aqueous layer was separated. Next, a Sep-Pak C18 cartridge was connected to the upper side, and a Sep-Pak AC-2 cartridge was connected to the lower side. After preconditioning with methanol and then with water, 40 mL of the aqueous layer was passed through. After removing water in the Sep-Pak AC-2 cartridge with nitrogen gas, acrylamide was eluted with 5 mL of methanol. The solvent of the eluate was removed, 1 mL of methanol, 0.1 mL of xanthohydrol 5% by weight methanol solution and 0.1 mL of hydrochloric acid 0.3 mol / L methanol solution were added to the residue, and the mixture was reacted for 2 hours at 40 ° C. did. The solvent of the derivatization liquid was removed, water and sodium chloride were added to the residue, and ethyl acetate was further added for extraction. The ethyl acetate layer was collected and subjected to analysis. It measured by GC-MS on the following conditions.

<GC-MS measurement conditions>
・ Analyzer: 6890N / 5973N GC-MS Agilent
<GC>
Column: DB-5MS (30 m × 0.25 mm × 0.25 μm)
Column temperature: 40 ° C (hold for 2 minutes) → 20 ° C / minute (temperature increase) → 300 ° C (hold for 5 minutes)
・ Column flow rate: 1 mL / min Helium gas ・ Injection method: Splitness injection mode ・ Inlet temperature: 250 ° C.
<MS>
-Ion source temperature: 230 ° C
・ Ionization energy: 70 eV
SIM: acrylamide derivative 251 m / z, d ₃ -acrylamide derivative 254 m / z

3. Measurement of Brix The refractometer reading (Brix) for sugar at 20 ° C. of the sample was measured using a sugar meter (Atago RX-5000 (manufactured by Atago)).

4). Sensory evaluation Five specialized panels sampled each container-packed coffee beverage and evaluated the strength of sourness, sharpness of sourness, sharpness of bitterness, and flavor balance according to the following criteria, and then the final score was determined by consultation.

Evaluation criteria of sourness strength 5: Strong 4: Slightly strong 3: Neither can be said 2: Slightly weak 1: Weak

Evaluation criteria for sour sharpness 5: Good 4: Slightly good 3: Not good 2: Slightly bad 1: Bad

Evaluation criteria for bitterness sharpness 5: Good 4: Slightly good 3: Neither can be said 2: Slightly bad 1: Bad

Evaluation criteria for flavor balance 5: Good 4: Slightly good 3: Not good 2: Slightly bad 1: Bad

Production Example 1
Production of purified chlorogenic acid-containing preparation Robusta coffee beans were extracted with hot water, and the resulting extract was dried by spray drying to obtain a raw material chlorogenic acid-containing composition. The raw material chlorogenic acid-containing composition has a (A) chlorogenic acid content of 28.6% by mass, (B) a caffeine content of 8.2% by mass, and a mass ratio [(B) / (A)]. It was 0.287.
9. 189 g of raw material chlorogenic acid-containing composition, 756 g of ethanol aqueous solution having an ethanol concentration of 52.4 mass%, 189 g of acid clay (Mizuka Ace # 600, manufactured by Mizusawa Chemical Co., Ltd.), filter aid (Solka Flock, manufactured by Nippon Mining Procurement) By mixing with 7 g, 1145 g of “chlorogenic acid-containing slurry” was obtained. The pH in the “chlorogenic acid-containing slurry” was 5.7.
Next, 1051 g of “chlorogenic acid-containing slurry” and 189 g of an aqueous ethanol solution having an ethanol concentration of 52.4 mass% were filtered with No. 2 filter paper on which diatomaceous earth was deposited as a precoat agent, and 1054 g of “filtrate” was recovered.
Next, a column filled with 200 mL of activated carbon (Kuraray Coal GW, manufactured by Kuraray Chemical Co., Ltd.) and a column packed with 105 mL of H-type cation exchange resin (SK1BH, manufactured by Mitsubishi Chemical Co., Ltd.), 1019 g of “filtrate” and an ethanol concentration of 52 231 g of a 4 mass% ethanol aqueous solution was passed in this order to recover 1072 g of “column treatment liquid”.
Next, 1038 g of the “column treatment liquid” was filtered through a 0.2 μm membrane filter, and then ethanol was distilled off using a rotary evaporator to obtain 225 g of a chlorogenic acid-containing composition solution. Hereinafter, this solution is referred to as “solution A of a chlorogenic acid-containing composition”.
The content of (A) chlorogenic acids in the “solution A of chlorogenic acids-containing composition” is 15.7% by mass, the content of (B) caffeine is 0% by mass, and the mass ratio [(B) / (A) ] Was 0, the ethanol concentration was 0% by mass, and the pH was 3.1.
Next, after adjusting the concentration of chlorogenic acids in the “solution A of chlorogenic acids-containing composition” to 6% by mass with distilled water, centrifugation is performed at 3000 rpm, 15 ° C., 60 minutes, A chlorogenic acid-containing preparation ”was obtained.

Example 1
A drip extractor (inner diameter 73 mm, volume 11 L) was charged with 90 g of steam-activated coconut shell activated carbon (average particle size 0.358 mm). Next, 85 ° C. warm water was supplied from the shower for 10 minutes to sterilize the activated carbon. The supply amount of warm water was 25 mass times with respect to activated carbon. Thereafter, 400 g of roasted coffee beans of L25.6 (average particle size 1.26 mm) were put on the activated carbon. Next, 0.25 kg of 85 ° C. warm water was supplied from the bottom of the drip extractor, and bottom water was poured. Next, 85 ° C. warm water was supplied from the shower at a rate of 1.25 g / sec, then the hot water supply was stopped, and the state was maintained for 10 minutes. The amount of hot water supplied was 2.55 times the mass of roasted coffee beans. After holding, hot water at 85 ° C. was supplied from the shower at a rate of 1.25 g / sec, and the coffee extract was discharged at the same rate. When the amount of collected liquid reached 2.4 kg, the discharge of the coffee extract was stopped, and this sample was used as the coffee extract. The Brix and pH of the obtained coffee extract are measured, adjusted to 1.75 with ion-exchanged water and further adjusted to pH 6.3 with 10% by mass aqueous sodium hydrogen carbonate solution. After being adjusted to, a metal can was filled and heat sterilized at 129 ° C. for 8 minutes 30 seconds to obtain a container-packed coffee beverage. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Example 2
A coffee extract was collected by the same operation as in Example 1. Next, the Brix and pH of the obtained coffee extract were measured, adjusted with ion-exchanged water so that the Brix of the coffee extract was 0.87, and then containing the purified chlorogenic acids obtained in Production Example 1 After 0.33% by mass of the preparation (Brix 49.72) was added, the pH was adjusted to 6.3 with a 10% by mass aqueous sodium hydrogen carbonate solution, and then filled into a metal can, at 129 ° C. for 8 minutes 30 Second sterilization was carried out to obtain a packaged coffee drink. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Example 3
The same operation as in Example 1 except that the roasted coffee beans L25.2 (average particle size 1.26 mm) were used instead of the roasted coffee beans L25.6 (average particle size 1.26 mm). A coffee extract was collected. Next, the Brix and pH of the obtained coffee extract are measured, adjusted to have a Brix of 1.85 with ion-exchanged water, and further adjusted to a pH of 6.3 with a 10% by mass aqueous sodium bicarbonate solution. After adjusting as described above, it was filled in a metal can and sterilized by heating at 129 ° C. for 8 minutes and 30 seconds to obtain a container-packed coffee beverage. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Example 4
A coffee extract was collected in the same manner as in Example 3. Next, the Brix and pH of the obtained coffee extract were measured, and after adjusting the Brix of the coffee extract to 0.92 with ion-exchanged water, the purified chlorogenic acids obtained in Production Example 1 contained After adding 0.60% by mass of the preparation (Brix 49.72), the pH was adjusted to 6.3 with a 10% by mass aqueous sodium hydrogen carbonate solution, and then filled into a metal can, at 129 ° C. for 8 minutes 30 Second sterilization was carried out to obtain a packaged coffee drink. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Example 5
A coffee extract was collected by the same operation as in Example 1. Next, the Brix and pH of the obtained coffee extract were measured, and after adjusting the Brix of the coffee extract to 0.92 with ion-exchanged water, the purified chlorogenic acids obtained in Production Example 1 contained After 0.93% by mass of the preparation (Brix49.72) was added, the pH was adjusted to 6.3 with a 10% by mass aqueous sodium hydrogen carbonate solution, and then filled in a metal can, at 129 ° C. for 8 minutes 30 Second sterilization was carried out to obtain a packaged coffee drink. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Comparative Example 1
Instead of roasted coffee beans of L25.6 (average particle size 1.26 mm), roasted coffee beans (average particle size 1.26 mm) mixed at a ratio of L30.6 / L17.5 = 23/77 are used. A coffee extract was collected in the same manner as in Example 1 except that it was. Next, the Brix and pH of the obtained coffee extract were measured, and after adjusting the Brix of the coffee extract to 2.21 with ion-exchanged water, the purified chlorogenic acids obtained in Production Example 1 contained After adding 0.26% by mass of the preparation (Brix 49.72), the pH was adjusted to 6.0 with a 10% by mass aqueous sodium hydrogen carbonate solution, and then filled into a metal can, at 129 ° C. for 8 minutes 30 Second sterilization was carried out to obtain a packaged coffee drink. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Comparative Example 2
The same operation as in Example 1 except that L22.3 roasted coffee beans (average particle size 1.26 mm) were used instead of L25.6 roasted coffee beans (average particle size 1.26 mm). A coffee extract was collected. Next, Brix and pH of the obtained coffee extract were measured, and after adjusting the Brix of the coffee extract to 0.66 with ion-exchanged water, the purified chlorogenic acids obtained in Production Example 1 contained After 0.16% by mass of the preparation (Brix 49.72) was added, the pH was adjusted to 6.3 with a 10% by mass aqueous sodium hydrogen carbonate solution, and then filled into a metal can, at 129 ° C. for 8 minutes 30 Second sterilization was carried out to obtain a packaged coffee drink. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Comparative Example 3
The same operation as in Example 1 except that the roasted coffee beans L23.3 (average particle size 1.26 mm) were used instead of the roasted coffee beans L25.6 (average particle size 1.26 mm). A coffee extract was collected. Next, the Brix and pH of the obtained coffee extract are measured, adjusted to have a Brix of 1.54 with ion-exchanged water, and further adjusted to a pH of 6.3 with a 10% by mass aqueous sodium bicarbonate solution. After adjusting as described above, it was filled in a metal can and sterilized by heating at 129 ° C. for 8 minutes and 30 seconds to obtain a container-packed coffee beverage. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

Comparative Example 4
The same operation as in Example 1 except that the roasted coffee beans L24.3 (average particle size 1.26 mm) were used instead of the roasted coffee beans L25.6 (average particle size 1.26 mm). A coffee extract was collected. Next, the Brix and pH of the obtained coffee extract are measured, adjusted to 1.36 with ion-exchanged water and further adjusted to 6.3 with 10% by mass aqueous sodium hydrogen carbonate solution. After adjusting as described above, it was filled in a metal can and sterilized by heating at 129 ° C. for 8 minutes and 30 seconds to obtain a container-packed coffee beverage. The obtained container-packed coffee beverage was analyzed and subjected to a sensory test. The results are shown in Table 1.

  From Table 1, by controlling the contents of chlorogenic acids and the mass ratios of (B) caffeine / (A) chlorogenic acids and (C) acrylamide / (A) chlorogenic acids within a specific range, after heat sterilization It was confirmed that a soaked coffee beverage with good bitterness can be obtained.

Claims (7)

The following components (A), (B) and (C);
(A) Chlorogenic acids: 0.14 to 0.28% by mass
(B) contains caffeine (C) acrylamide,
The mass ratio [(B) / (A)] of the component (A) and the component (B) is 0.01 to 0.5, and the mass ratio of the component (A) and the component (C) [(C ) / (A)] is 1.5 × 10 ^{−6 to} 9 × 10 ⁻⁶ ,
Heat-sterilized containerized coffee beverage.   The container-packed coffee drink of Claim 1 whose content of a component (B) is 400 mass ppm or less.   The container-packed coffee drink of Claim 1 or 2 whose content of a component (C) is 0.03 mass ppm or less.   The container-packed coffee drink according to any one of claims 1 to 3, wherein the pH is 4.5 to 6.9.   The container-packed coffee drink as described in any one of Claims 1-4 whose Brix is 0.8-3.0.   The container-packed coffee drink according to any one of claims 1 to 5, wherein the heat sterilization is retort sterilization or UHT sterilization. The following components (A), (B) and (C);
(A) Chlorogenic acids: 0.14 to 0.28% by mass
(B) A method for improving the sourness and bitterness of a heat-sterilized containerized coffee beverage containing caffeine (C) acrylamide,
The mass ratio [(B) / (A)] of the component (A) to the component (B) is set to 0.01 to 0.5, and the mass ratio of the component (A) to the component (C) [(C) / (A)] is adjusted to 1.5 × 10 ^{−6 to} 9 × 10 ⁻⁶ or less, respectively, to improve sourness and bitterness.