Method for producing a composition containing purified chlorogenic acid

Abstract

To provide a method for producing a purified chlorogenic acid-containing composition in which the raw bean odor is reduced without impairing the chlorogenic acids. [Solution] A method for producing a purified chlorogenic acid-containing composition comprising the following steps (a) and (b). (a) A process of bringing coffee beans, which are made by combining one requirement selected from the form requirements below and one requirement selected from the roasting requirements below, into contact with water, and discarding the water that has been in contact with the beans. (Form requirements) Ground coffee beans, or unground coffee beans (Roasting requirements) Roasted coffee beans or green coffee beans with an L value of 40 or higher (b) Step (a) Extracting coffee beans with water

Description

Technical Field

[0001] The present invention relates to a method for producing a purified chlorogenic acid-containing composition.

Background Art

[0002] Although various materials having physiological activity functions have been proposed, for example, polyphenols have physiological activity functions such as antioxidant action, blood pressure lowering action, and liver function improving action. Chlorogenic acids, which are one of the polyphenols, have been reported to have a high blood pressure lowering effect, and their application to supplements and food and drink products is expected.

[0003] Examples of materials rich in chlorogenic acids include raw coffee beans and lightly roasted coffee beans. Conventionally, regarding chlorogenic acid-containing compositions obtained by extraction from coffee beans, improvement in the recovery rate of chlorogenic acids, reduction of impurities such as caffeine, improvement of flavor, and improvement of hue have been studied. For example, a method has been proposed in which a raw coffee bean extract is dissolved in a mixed solution of an organic solvent and water with a mass ratio of 9 / 1 to 1 / 9 and contacted with activated carbon and / or activated clay or acid clay, and it has been reported that a purified chlorogenic acid-containing composition with good hue and flavor can be obtained without significantly changing the composition of chlorogenic acids while selectively removing caffeine (Patent Document 1).

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] However, the method described in Patent Document 1 requires solvent removal treatment for use in food products, and there are various limitations on the equipment for removing organic solvents, as well as the manufacturing process is complicated, so a simpler method was needed. In addition, in order to make the most of the chlorogenic acids in coffee beans, it is advantageous to use green coffee beans or lightly roasted coffee beans (hereinafter also referred to as "green coffee beans, etc."), but these coffee beans have a strong raw bean odor such as a grassy smell, which can be an obstacle to continuous consumption. Therefore, when green coffee beans, etc. are brought into contact with a solvent to remove the raw bean odor, the leaching of chlorogenic acids is unavoidable.

[0006] The object of the present invention is to provide a method for producing a purified chlorogenic acid-containing composition in which the raw bean odor is reduced without impairing the chlorogenic acids. [Means for solving the problem]

[0007] As a result of various studies, the inventors of the present invention found that the above problem can be solved by bringing coffee beans having specific properties into contact with water, discarding the water, and then extracting the coffee beans that were in contact with water.

[0008] In other words, the present invention provides a method for producing a purified chlorogenic acid-containing composition comprising the following steps (a) and (b). (a) A process of bringing coffee beans, which are made by combining one requirement selected from the form requirements below and one requirement selected from the roasting requirements below, into contact with water, and discarding the water that has been in contact with the beans. (Form requirements) Ground coffee beans, or unground coffee beans (Roasting requirements) Roasted coffee beans or green coffee beans with an L value of 40 or higher (b) Step (a) Extracting coffee beans with water [Effects of the Invention]

[0009] According to the present invention, a purified chlorogenic acid-containing composition with reduced raw bean odor can be produced by simple operations without damaging the chlorogenic acids. [Brief explanation of the drawing]

[0010] [Figure 1] This figure shows an example of the average contact time with water in process (a). [Figure 2] This figure shows an example of a method of contact with water in process (a). [Modes for carrying out the invention]

[0011] The present invention provides a method for producing a purified chlorogenic acid-containing composition, comprising steps (a) and (b). Each step will be described in detail below.

[0012] Process (a) This process involves bringing coffee beans into contact with water and then discarding the water. It is characterized by using coffee beans that meet one of the following morphological requirements and one of the following roasting requirements. This makes it possible to reduce the raw bean odor without damaging the chlorogenic acids.

[0013] (Form requirements) Ground coffee beans or unground coffee beans (Roasting Requirements) Roasted coffee beans or green coffee beans with an L value of 40 or higher.

[0014] The form requirement for coffee beans is either ground or unground. The size of the ground coffee beans can be appropriately selected. From the perspective of reducing the raw bean odor without impairing chlorogenic acids, the particle size is preferably 2 mm or more, more preferably 3 mm or more, and even more preferably 4 mm or more. The upper limit of the particle size of the ground coffee beans is not particularly limited. For example, it can be halved or quartered. Also, a mixture of coffee beans with different particle sizes is acceptable. Here, in this specification, the "particle size" refers to the particle size represented by the smallest mesh opening through which the coffee beans do not pass. As the sieve, for example, Tyler standard sieves, ASTM standard sieves, or JIS standard sieves can be used.

[0015] The roasting requirements for the coffee beans are either roasted coffee beans with an L value of 40 or more, or unroasted raw coffee beans. Here, in this specification, the "L value" is the lightness of the roasted coffee beans measured with a color difference meter, with black being L value 0 and white being L value 100. The L value of the roasted coffee beans is 40 or more. From the perspective of improving the yield of chlorogenic acids, 45 or more is preferable, 50 or more is more preferable, 55 or more is even more preferable, and being unroasted is even more preferable.

[0016] In the present invention, it is possible to use one or more types of coffee beans formed by combining one requirement of the morphological requirements described above and one requirement of the roasting requirements. Specifically, one or more of the coffee beans shown in the following (1) to (4) can be appropriately selected and used. When using two or more of the coffee beans shown in the following (1) to (4), the mixing ratio can be appropriately selected within a range that does not impair the effects of the present invention. (1) Ground roasted coffee beans with an L value of 40 or more (2) Ground raw coffee beans [[ID=1,6]](3) Un - ground roasted coffee beans with an L value of 40 or more (4) Un - ground raw coffee beans

[0017] Note that the coffee bean variety and origin are not particularly limited and can be appropriately selected. It is also possible to use one or more kinds of coffee beans with different varieties and origins by mixing them.

[0018] The contact time with water is defined by the average contact time described below. As a result, the raw coffee bean odor can be efficiently reduced without damaging the chlorogenic acids. Here, in this specification, the "average contact time" means that in any of the batch method and the continuous method described later, when the water level in the extractor is above the upper surface of the coffee beans filled in the extractor, the contact ratio between water and coffee beans is set to 1, and it is defined as the value obtained by integrating the contact ratio from the start of contact with water to the elapsed time t1 (minutes). When the coffee beans are put into the extractor after filling the extractor with water, the state where all the coffee beans in the extractor are immersed in water is regarded as the contact ratio between water and coffee beans being 1. That is, regardless of the method of contact with water, the state where the entire coffee beans filled in the extractor are immersed in water is regarded as the contact ratio between water and coffee beans being 1, and in that case, the water level is not particularly limited as long as it is above the upper surface of the coffee beans filled in the extractor. From the above, when the contact ratio between water and coffee beans in the extractor at the elapsed time t (minutes) from the start of contact with water is R(t), and the time from the start of contact between water and coffee beans in the extractor to the completion of water discharge is t1 (minutes), the average contact time can be expressed by the following formula (1).

[0019]

Equation

[0020] 〔In formula (1), t represents the elapsed time (minutes) from the start of contact with water, R(t) represents the contact ratio between water and coffee beans in the extractor, t1 represents the time (minutes) from the start of contact between water and coffee beans to the completion of water discharge.〕

[0021] Figure 1 shows an example of the average contact time with water, illustrating an example where coffee beans packed in a column-type extraction machine are continuously brought into contact with water. Figure 1 shows that the vertical axis represents the contact ratio between water and coffee beans in the extraction machine, and the horizontal axis represents the elapsed time since the start of water contact. The average contact time with water is calculated as the area of ​​the shaded region in Figure 1. In Figure 1, A indicates the start of water supply into the column-type extraction machine filled with coffee beans. From A to B, the contact ratio between water and coffee beans increases at a constant rate, indicating that water is supplied to the extraction machine at a constant rate and the water level inside the extraction machine rises over time. B indicates that the contact ratio between water and coffee beans is 1, and the water level inside the extraction machine has reached above the top surface of the coffee beans filled inside the extraction machine. From B to D (the elapsed time shown in C), the contact ratio between water and coffee beans is maintained at 1, and water is discharged from the extraction machine at the same rate as the water supply rate, indicating that the water level inside the extraction machine remained above the top surface of the coffee beans for a certain period of time. From D to E, the contact ratio between water and coffee beans decreases at a constant rate. As the water supply to the extractor is stopped and the water discharge from the extractor continues, the water level inside the extractor is below the top surface of the coffee beans. E indicates that the water discharge from the extractor is complete and contact between water and coffee beans has ended.

[0022] The average contact time is preferably 1 minute or more, more preferably 5 minutes or more, even more preferably 10 minutes or more, and even more preferably 12 minutes or more, from the viewpoint of reducing the raw bean odor. Furthermore, from the viewpoint of suppressing the elution of chlorogenic acids and improving the yield of chlorogenic acids, it is preferably 150 minutes or less, more preferably 100 minutes or less, even more preferably 90 minutes or less, and even more preferably 80 minutes or less. The average contact time is preferably 1 to 150 minutes, more preferably 5 to 100 minutes, even more preferably 10 to 90 minutes, and even more preferably 12 to 80 minutes.

[0023] The amount of water to be brought into contact with the coffee beans (mass ratio to the coffee beans; hereafter referred to as "bath ratio") can be appropriately selected depending on the contact method and scale, but from the viewpoint of reducing the green bean odor, suppressing the elution of chlorogenic acids, and improving the yield of chlorogenic acids, a ratio of 0.8 or higher is preferred, 1.6 or higher is more preferred, 2.0 or higher is even more preferred, 30 or lower is preferred, 20 or lower is more preferred, and 10 or lower is even more preferred. The range of such water amount is preferably a mass ratio to the coffee beans of 0.8 to 30, more preferably 1.6 to 20, and even more preferably 2.0 to 10.

[0024] The method of contact between coffee beans and water is not particularly limited as long as water can come into contact with the surface of the coffee beans, but examples include batch and continuous methods. In the batch method, for example, coffee beans are immersed in water in a tank, and stirring may be performed as needed. On the other hand, in the case of a continuous extraction method, for example, a column-type extraction machine can be used, where coffee beans are packed into the column, and then water is passed through the column. The direction of water flow can be either an upward flow from the bottom to the top of the column-type extraction machine, or a downward flow from the top to the bottom. Furthermore, even when using a column-type extractor, if the column is filled with water and then left to stand without passing the water through it, and the water is subsequently drained, this specification refers to it as a batch process. However, if the extractor does not use a column-type extractor but still allows water to pass through it, it refers to it as a continuous process.

[0025] To explain the continuous type in more detail, a column-type extractor is equipped with, for example, a mesh for holding coffee beans inside, a nozzle for supplying water from the top of the column, and an outlet for draining water from the bottom of the column. As shown in Figure 2, a filling step is performed in which water is supplied from above into the column filled with coffee beans to immerse the entire coffee bean in water, and a draining step is performed after the filling step to drain all the water from the column. In order to maintain the filled state for a predetermined time, a flow step may be performed before the draining step, in which water is supplied to and drained from the column simultaneously as needed. Note that the water supply rate and the water draining rate in the flow step do not have to be different, but if they are set to be approximately the same, the water level in the column can be maintained at approximately the same level.

[0026] When coffee beans and water are brought into contact within the extraction machine and water is circulated, the water flow rate can be appropriately set according to the production scale, etc., but from the viewpoint of reducing the raw bean odor, 0.1 SV / h or more is preferred, 0.3 SV / h or more is more preferred, and 0.5 SV / h or more is even more preferred. Furthermore, from the viewpoint of suppressing the elution of chlorogenic acids and improving the yield of chlorogenic acids, 20 SV / h or less is preferred, 10 SV / h or less is more preferred, and 5.0 SV / h or less is even more preferred. The range of such supply rates is preferably 0.1 to 20 SV / h, more preferably 0.3 to 10 SV / h, and even more preferably 0.5 to 5.0 SV / h. The water supply rate when filling the column-type extractor with water and the water discharge rate when removing water from the column-type extractor are not particularly limited, but from the viewpoint of simplifying the process, it is preferable that they be the same as the water flow rate.

[0027] Examples of water include tap water, distilled water, deionized water, and natural water, but are not limited to these.

[0028] From the viewpoint of reducing the raw bean odor, the water temperature is preferably 1°C or higher, more preferably 10°C or higher, even more preferably 20°C or higher, and even more preferably 25°C or higher. From the viewpoint of improving the yield of chlorogenic acids and temperature control, the water temperature is preferably 100°C or lower, more preferably 95°C or lower, even more preferably 80°C or lower, even more preferably 70°C or lower, and even more preferably 60°C or lower. The range of such temperatures is preferably 1 to 100°C, more preferably 10 to 95°C, even more preferably 20 to 80°C, even more preferably 25 to 70°C, and even more preferably 25 to 60°C.

[0029] Process (b) This step involves extracting the coffee beans after step (a) with water. This allows for the efficient extraction of chlorogenic acids. Here, in this specification, "chlorogenic acids" refers to the collective term for monocaffeoylquinic acids (3-caffeoylquinic acid, 4-caffeoylquinic acid, and 5-caffeoylquinic acid) and monoferulaquinic acids (3-ferulaquinic acid, 4-ferulaquinic acid, and 5-ferulaquinic acid). In this invention, it is sufficient to contain at least one of the above six types of chlorogenic acids. The chlorogenic acids may also be in the form of salts or hydrates. The salts are not particularly limited as long as they are physiologically acceptable, but examples include alkali metal salts.

[0030] As for the extraction method, known methods such as stirring extraction, column extraction, and drip extraction can be employed. From the viewpoint of extraction efficiency of chlorogenic acids, the water temperature used for extraction is preferably 70°C or higher, more preferably 75°C or higher, and even more preferably 80°C or higher. From the viewpoint of temperature control, it is preferably 100°C or lower, more preferably 95°C or lower, and even more preferably 90°C or lower. The range of water temperature is preferably 70 to 100°C, more preferably 75 to 95°C, and even more preferably 80 to 90°C.

[0031] Furthermore, while the same type of water as described above can be used, ion-exchanged water is preferred in terms of taste.

[0032] The amount of water used for extraction (as a mass ratio to the coffee beans used in step (a); hereafter referred to as the "bath ratio") can be appropriately selected depending on the extraction method, but from the viewpoint of extraction efficiency of chlorogenic acids, a ratio of 2 or more is preferred, 3 or more is more preferred, and 4 or more is even more preferred. From the viewpoint of reducing the concentration load, a ratio of 30 or less is preferred, 25 or less is more preferred, and 20 or less is even more preferred. Such a bath ratio is preferably 2 to 30, more preferably 3 to 25, and even more preferably 4 to 20.

[0033] Furthermore, the extraction time is defined in the same way as the "average contact time" in step (a) above and is referred to as the "average extraction time". The average extraction time is not uniform depending on the scale, etc., but for example, from the viewpoint of improving the yield of chlorogenic acids, it is preferably 10 minutes or more, more preferably 30 minutes or more, and even more preferably 60 minutes or more. From the viewpoint of production efficiency, it is preferably 720 minutes or less, more preferably 660 minutes or less, and even more preferably 600 minutes or less. The range of such average extraction time is preferably 10 to 720 minutes, more preferably 30 to 660 minutes, and even more preferably 60 to 600 minutes.

[0034] When performing column extraction, it is possible to use the column extractor described in step (a). Using a column extractor allows steps (a) and (b) to be performed consecutively, thus enabling the efficient production of purified chlorogenic acid compositions. When performing column extraction, the water supply rate is preferably within the range described in step (a) of the filling step, from the viewpoint of extraction efficiency of chlorogenic acids, and may be the same as the water supply rate in the filling step.

[0035] In this way, the purified chlorogenic acid-containing composition of the present invention can be obtained. However, from the viewpoint of further reducing the raw bean odor, the extract obtained in step (b) may be brought into contact with an adsorbent after step (b). The adsorbent is not particularly limited as long as it is commonly used in the food industry, but from the viewpoint of adsorption efficiency, porous adsorbents are preferred. As a porous adsorbent, for example, at least one selected from activated carbon, activated clay, and acid clay can be used. Among these, activated carbon is preferred from the viewpoint of heterogeneous suppression and selective removal of caffeine.

[0036] Examples of raw materials for activated carbon include sawdust, coal, and coconut shells, but coconut shell-derived activated carbon is preferred. Furthermore, activated carbon activated with a gas such as water vapor is preferably used. The activated carbon may be in powder, granular, or fibrous form, but from the viewpoint of adsorption efficiency, powder and granular forms are preferred, and granular forms are even more preferred. Commercially available activated carbon products such as Kuraraycol GW (manufactured by Kuraray Chemical Co., Ltd.) and Taiko SG (manufactured by Futamura Chemical Co., Ltd.) can be used.

[0037] Methods of contact with the porous adsorbent include, for example, batch type and continuous type. Among these, from the viewpoint of production efficiency, the continuous type, in which the porous adsorbent is packed into a column and passed through continuously, is preferred. In the case of the continuous type, the adsorbent may be supplied from the bottom to the top (upward flow) or from the top to the bottom (downward flow), and this can be selected as appropriate. When using the continuous type, the supply rate of the extract can be set as appropriate.

[0038] From the viewpoint of reducing green bean odor and caffeine, the amount of porous adsorbent used is preferably 50% by mass or more, more preferably 80% by mass or more, and even more preferably 150% by mass or more, relative to the solid content of the purified chlorogenic acid-containing composition. From the viewpoint of chlorogenic acid yield, it is preferably 400% by mass or less, more preferably 370% by mass or less, and even more preferably 350% by mass or less. The range of the amount of porous adsorbent used is preferably 50 to 400% by mass, more preferably 80 to 370% by mass, and even more preferably 150 to 350% by mass, relative to the solid content of the purified chlorogenic acid-containing composition.

[0039] Furthermore, from the viewpoint of reducing the raw bean odor and selectively removing caffeine, the contact temperature with the porous adsorbent is preferably 30°C or higher, more preferably 40°C or higher, even more preferably 50°C or higher, and even more preferably 60°C or higher. From the viewpoint of yielding chlorogenic acids, it is preferably 150°C or lower, more preferably 120°C or lower, and even more preferably 100°C or lower. The range of such contact temperatures is preferably 30 to 150°C, more preferably 40 to 120°C, even more preferably 50 to 100°C, and even more preferably 60 to 100°C.

[0040] After contact with the porous adsorbent, the porous adsorbent treatment liquid may be subjected to solid-liquid separation as needed. The solid-liquid separation method is not particularly limited as long as it is a method commonly used in the food industry, but examples include filter paper filtration, centrifugal separation, membrane filtration, etc., and one or more of these can be used in appropriate combinations.

[0041] The purified chlorogenic acid-containing composition of the present invention can take various forms, such as liquid, slurry, semi-solid, and solid. If a liquid product is preferred, it can be concentrated using known concentration methods such as atmospheric pressure concentration, reduced pressure concentration, or reverse osmosis membrane concentration. If a solid product is preferred, it can be converted into a powder using known drying methods such as spray drying or freeze-drying.

[0042] The purified chlorogenic acid-containing composition of the present invention is rich in chlorogenic acids and has reduced raw bean odor, making it useful as a raw material for oral products. Oral products are not particularly limited as long as they can be taken orally, but examples include food and beverages, pharmaceuticals, or quasi-drugs. Food and beverages are preferred among these. Oral products can be manufactured according to conventional methods, depending on their type.

[0043] Furthermore, the purified chlorogenic acid-containing composition of the present invention may be heat-sterilized. The heat-sterilization method is not particularly limited as long as it conforms to the conditions stipulated in the applicable laws and regulations (Food Sanitation Law in Japan), but examples include retort sterilization, high-temperature short-time sterilization (HTST), and ultra-high temperature sterilization (UHT). [Examples]

[0044] Example 1 <Process (a)> 450g of unground Robusta coffee beans were packed into an extraction column. Next, 1140g of 20°C water was supplied to the extraction column at a rate of 38mL / min from a supply valve at the top of the extraction column. Ten minutes after the start of water supply, the contact ratio of water to coffee beans reached 1. Twenty minutes later, 20°C water was supplied from the top of the extraction column at a rate of 38mL / min, while water was simultaneously discharged from the bottom of the extraction column at a rate of 38mL / min. After 90 minutes, the water supply from the supply valve at the top of the extraction column was stopped, and the water in the column was discharged from the supply valve at the bottom of the extraction column at a rate of 38mL / min over 28 minutes. At this point, 18 minutes after the water supply from the supply valve at the top of the extraction column was stopped, the contact ratio of water to coffee beans fell below 1. The bath ratio was 6.7, and the average contact time was 138 minutes. <Process (b)> Next, 765g of 90°C hot water was supplied to the extraction column at a rate of 38mL / min from the supply valve above the extraction column, filling it so that the contact ratio of water to coffee beans was 1 or more. The time it took for this contact ratio to reach 1 was 10 minutes. Then, 90°C hot water was supplied from above the extraction column at a rate of 7mL / min, while the extract was discharged from below the extraction column at a rate of 7mL / min. 360 minutes after the start of hot water supply after filling, the water supply from the supply valve above the extraction column was stopped, and the discharge of the extract from the supply valve below the extraction column was stopped. The average extraction time was 375 minutes. <Post-processing> An activated carbon column packed with 92.5 g of activated carbon and filled with deionized water was continuously supplied at 75°C with the extract discharged from the bottom of the extraction column, while simultaneously being discharged from the bottom of the column to obtain 2453 g of activated carbon treated solution. Next, the obtained activated carbon treated solution was concentrated under reduced pressure in an evaporator at 50°C and 95 mmHG to obtain a concentrated solution. The obtained concentrated solution was then treated in a UHT sterilizer at 130°C for 30 seconds to obtain a disinfectant solution. The obtained disinfectant solution was then treated in a spray dryer at an intake air temperature of 190°C and an exhaust air temperature of 95°C to obtain a purified chlorogenic acid-containing composition.

[0045] Example 2 In step (a), 760g of 20°C water was supplied instantaneously (within 10 seconds), and then the water supply and discharge were stopped, and this state was maintained for 30 minutes, after which the water was discharged instantaneously (within 10 seconds) from the bottom of the column. The same procedure as in Example 1 was followed to obtain a purified chlorogenic acid-containing composition. The bath ratio in step (a) was 1.7, and the average contact time was 30 minutes.

[0046] Example 3 In step (a), 760 g of 30°C water was supplied at a rate of 38 mL / min. Ten minutes after the start of water supply, the contact ratio between water and coffee beans reached 1. Ten minutes after that, the water supply from the supply valve above the extraction column was stopped, and the water in the column was drained from below the extraction column at a rate of 38 mL / min over 17 minutes. At this time, seven minutes after the water supply from the supply valve above the extraction column was stopped, the contact ratio between water and coffee beans fell below 1. The bath ratio in step (a) was 1.7, and the average contact time was 27 minutes. Step (b) was performed in the same manner as in Example 1 to obtain a purified chlorogenic acid-containing composition.

[0047] Example 4 In step (a), 760 g of 40°C water was first supplied to the extraction column at a rate of 38 mL / min for 20 minutes. After this time, the water supply from the supply valve at the top of the extraction column was stopped, and 225 g of unground Robusta coffee beans were loaded into the extraction column over 3 minutes and held for 4 minutes. Next, another 225 g of unground Robusta coffee beans were loaded into the extraction column over 3 minutes and held for 5 minutes. Subsequently, the water in the column was discharged from the supply valve at the bottom of the extraction column at a rate of 92 mL / min over 7 minutes. At this time, the contact ratio between water and coffee beans fell below 1 4 minutes after the start of water discharge from the supply valve at the bottom of the extraction column. The bath ratio in step (a) was 1.7, and the average contact time was 15 minutes. Step (b) was performed in the same manner as in Example 1 to obtain a purified chlorogenic acid-containing composition.

[0048] Example 5 A purified chlorogenic acid-containing composition was obtained by the same procedure as in Example 3, except that the water temperature was changed to 40°C in step (a).

[0049] Example 6 In step (a), the water temperature was set to 40°C, and after filling, 40°C water was supplied from above the extraction column at a rate of 38 mL / min. At the same time, the time until the start of water discharge from below the extraction column at a rate of 38 mL / min was 45 minutes. After stopping the water supply from the supply valve above the extraction column, the contact ratio between water and coffee beans was set to less than 1 17 minutes later, and the water discharge time was set to 27 minutes. The same procedure as in Example 1 was followed to obtain a purified chlorogenic acid-containing composition. The bath ratio in step (a) was 6.2, and the average contact time was 92 minutes.

[0050] Example 7 A purified chlorogenic acid-containing composition was obtained by the same procedure as in Example 3, except that the water temperature was changed to 50°C in step (a).

[0051] Example 8 In step (a), the water temperature was set to 50°C, and after filling, 50°C water was supplied from above the extraction column at a rate of 38 mL / min. At the same time, the time until the water was discharged from below the extraction column at a rate of 38 mL / min was 30 minutes. After stopping the water supply from the supply valve above the extraction column, the contact ratio between water and coffee beans was set to less than 1 17 minutes later, and the water discharge time was set to 27 minutes. The same procedure as in Example 1 was followed to obtain a purified chlorogenic acid-containing composition. The bath ratio in step (a) was 5.0, and the average contact time was 77 minutes.

[0052] Example 9 A purified chlorogenic acid-containing composition was obtained by the same procedure as in Example 3, except that the water temperature was changed to 70°C in step (a).

[0053] Example 10 In step (a), a purified chlorogenic acid-containing composition was obtained by performing the same procedure as in Example 1, except that 760g of 70°C water was supplied instantaneously (within 10 seconds), the condition was maintained for 1 minute, and then the water was discharged instantaneously (within 10 seconds) from the bottom of the column. The bath ratio in step (a) was 1.7 and the average contact time was 1 minute.

[0054] Example 11 A purified chlorogenic acid-containing composition was obtained by the same procedure as in Example 3, except that the water temperature was changed to 95°C in step (a).

[0055] Example 12 In step (a), 450 g of green Robusta coffee beans with an average particle size of 4 mm were packed into the extraction column. Next, 760 g of 20°C water was supplied to the extraction column instantaneously (within 10 seconds) from the supply valve above the extraction column to fill it. This state was then maintained for 30 minutes. Next, the water was discharged instantaneously (within 10 seconds) from the bottom of the extraction column. The bath ratio in step (a) was 1.7 and the average contact time was 30 minutes. In step (b), a purified chlorogenic acid-containing composition was obtained by the same procedure as in Example 1.

[0056] Example 13 In step (a), a purified chlorogenic acid-containing composition was obtained by the same procedure as in Example 3, except that 450g of green coffee beans were roasted to 412g of L59 coffee beans and the water temperature was changed to 40°C. The reason the mass of the coffee beans decreased to 412g is that volatile components were removed by roasting, resulting in a bath ratio of 1.8.

[0057] Comparative Example 1 A purified chlorogenic acid-containing composition was obtained by the same procedure as in Example 1, except that step (a) was omitted.

[0058] 1. Evaluation Method (1) Sensory evaluation (green bean odor) Three expert panel members agreed to evaluate the compositions according to the following criteria. They then measured out 0.15g of the purified chlorogenic acid-containing compositions obtained in the examples and comparative examples using a spoon, ingested it, and evaluated the "raw bean odor." Four expert panel members then deliberated and determined the final scores.

[0059] Evaluation criteria for green bean odor The green bean odor score of the purified chlorogenic acid-containing composition obtained in Comparative Example 1 was set to "1", and the green bean odor score of the purified chlorogenic acid-containing composition obtained in Example 9 was set to "5", and they were evaluated according to the following criteria.

[0060] Evaluation Criteria Rating 5: No raw bean odor (equivalent to Example 9) 4: Almost no raw bean smell. 3: Has a slight raw bean smell. 2: Has a raw bean smell. 1: Has a strong raw bean odor (similar to Comparative Example 1)

[0061] (2) Chlorogenic acid washing loss rate The composition of the waste liquid discharged from the column in step (a) of each example was analyzed, and the chlorogenic acid concentration was quantified. Next, the chlorogenic acid washing loss rate was calculated using the following formula.

[0062] Chlorogenic acid water wash loss rate (%) = (Amount of chlorogenic acid in waste liquid) / (Amount of chlorogenic acid in unground green coffee beans) × 100

[0063] The amount of chlorogenic acids in unground green coffee beans was determined by analyzing the extract obtained by the following method. 10g of Robusta coffee beans, with a particle size of 1.3mm, were packed into the extraction column. Next, 95°C coffee was injected into the extraction column at a rate of 3.5mm / min through a supply valve located below the extraction column. Water was supplied. The extract flowing out from the discharge valve above the extraction column was collected, and 150 minutes after the flow was stopped, the water supply from the supply valve below the extraction column was stopped, and 500g of extract was collected. We obtained the extract.

[0064] (3) Chlorogenic acid yield The amount of chlorogenic acids in the recovered activated carbon treated solution was calculated using the following formula.

[0065] Chlorogenic acid yield (%) = (X × Y / 100) / (W × Z / 100) × 100

[0066] [In the formula, X represents the mass of the activated carbon treatment solution (g), Y represents the amount of chlorogenic acids in the activated carbon treatment solution (mass%), W represents the mass of unground green coffee beans (g), and Z represents the amount of chlorogenic acids in the unground green coffee beans (mass%).]

[0067] 2. Analysis of chlorogenic acids The sample solution was filtered through a filter (0.45 μm), and chromatography was performed using a gradient method with an ultrahigh-performance liquid chromatograph (model Waters AQUITY UPLC, manufactured by Waters Japan Ltd.) equipped with a column [AQUITY UPLC TM C18 (1.7 μm, 2.1 mmφ × 100 mm)] at a column temperature of 35 °C. Mobile phase A was a 5% acetonitrile solution containing 0.05 mol / L acetic acid, 0.01 mol / L sodium acetate, and 0.1 mmol / L HEDPO, and mobile phase B was an acetonitrile solution. The flow rate was 0.5 mL / min, the sample injection volume was 10 μL, and the UV detector wavelength was 325 nm. The gradient conditions were as follows:

[0068] Concentration gradient conditions Time (minutes) Solution A concentration (volume%) Solution B concentration (volume%) 0 100% 0% 2.5 100% 0% 3.5 95% 5% 5 95% 5% 6 92% 8% 16 92% 8% 16.5 10% 90% 19 100% 0%

[0069] [Table 1]

[0070] Table 1 shows that by using coffee beans with specific properties, contacting them with water, discarding the water, and then extracting the coffee beans with water, a purified chlorogenic acid-containing composition with reduced green bean odor can be obtained without damaging the chlorogenic acids.

Claims

1. A method for producing a purified chlorogenic acid-containing composition, comprising the following steps (a) and (b). (a) A process of bringing coffee beans, which are made by combining one requirement selected from the form requirements below and one requirement selected from the roasting requirements below, into contact with water, and discarding the water that has been in contact with the beans. (Form requirements) Ground coffee beans, or unground coffee beans (Roasting requirements) Roasted coffee beans or green coffee beans with an L value of 40 or higher (b) Step of extracting coffee beans after step (a) with water.

2. A method for producing a purified chlorogenic acid-containing composition according to claim 1, wherein in step (a), contact with water is carried out such that the average contact time calculated by the following formula (1) is 1 to 150 minutes. [Math 1] [In formula (1), t represents the elapsed time (in minutes) since the start of water filling. R(t) indicates the contact ratio between water and coffee beans inside the extraction machine. t 1 This indicates the time (in minutes) from the start of contact between water and coffee beans to the completion of contact with water.

3. A method for producing a purified chlorogenic acid-containing composition according to claim 1 or 2, wherein the particle size of the ground coffee beans used in step (a) is 2 mm or more.

4. A method for producing a purified chlorogenic acid-containing composition according to claim 1 or 2, wherein the temperature of the water brought into contact in step (a) is 10 to 95°C.

5. A method for producing a purified chlorogenic acid-containing composition according to claim 1 or 2, wherein the temperature of the water used for extraction in step (b) is 70 to 100°C.

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