JP4778937B2 - Method for producing roasted coffee beans - Google Patents
Method for producing roasted coffee beans Download PDFInfo
- Publication number
- JP4778937B2 JP4778937B2 JP2007190392A JP2007190392A JP4778937B2 JP 4778937 B2 JP4778937 B2 JP 4778937B2 JP 2007190392 A JP2007190392 A JP 2007190392A JP 2007190392 A JP2007190392 A JP 2007190392A JP 4778937 B2 JP4778937 B2 JP 4778937B2
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- Prior art keywords
- coffee
- coffee beans
- beans
- acid
- minutes
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
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Description
本発明は、焙煎コーヒー豆の製造方法に関する。 The present invention relates to a method for producing roasted coffee beans.
活性酸素の一つである過酸化水素は、変異原性、癌原性等の他、動脈硬化症、虚血性心疾患等の循環器系疾患、消化器疾患、アレルギー疾患、眼疾患など多くの疾患に深く関与しているといわれている(非特許文献1)。一方、コーヒーには、焙煎によって自然発生する過酸化水素が含まれており(非特許文献2)、カタラーゼ、ペルオキシダーゼ、抗酸化剤(特許文献1〜4)等を添加することにより、コーヒー中の過酸化水素を除去する技術が報告されている。
本発明者らが、過酸化水素を除去したコーヒーをラットに飲用させたところ、体内で過酸化水素が生成し、尿中過酸化水素濃度が上昇することが判明した。すなわち、従来の、コーヒー飲料中の過酸化水素除去技術によっては、コーヒー飲用後に体内での過酸化水素生成を抑制することはできなかった。 When the present inventors allowed rats to drink coffee from which hydrogen peroxide had been removed, it was found that hydrogen peroxide was produced in the body and the urine hydrogen peroxide concentration increased. That is, conventional hydrogen peroxide removal technology in coffee beverages has not been able to suppress the production of hydrogen peroxide in the body after drinking coffee.
本発明の目的は、飲用後の体内での過酸化水素の生成を抑制するコーヒー抽出液を供するコーヒー豆の製造方法を提供することにある。 The objective of this invention is providing the manufacturing method of the coffee bean which provides the coffee extract which suppresses the production | generation of hydrogen peroxide in the body after drinking.
本発明者は、コーヒー中の何らかの成分が生体内において過酸化水素を生成させるのではないかとの仮説に基づき、種々検討した結果、コーヒー中に含まれるヒドロキシヒドロキノンに、生体内で過酸化水素を生成させる作用があること、及びヒドロキシヒドロキノンの含有量を通常含まれる量より少なくすれば、生体内で過酸化水素生成が少ないコーヒー飲料組成物が得られることを見出した。(WO2005/072533)
さらに本発明者は、クロロゲン酸類が優れた血圧降下作用を示すにもかからず(特開2002−363075号公報、特開2002−22062号公報、特開2002−53464号公報)、クロロゲン酸類を多く含むコーヒー飲料が十分な血圧降下作用を示さないことに着目し(Eur. J. Clin. Nutr., 53(11), 831(1999))、血圧降下作用とコーヒー飲料の成分との関係について検討した結果、コーヒー飲料に含まれているヒドロキシヒドロキノンがクロロゲン酸類の血圧降下作用を阻害していることも見出した。
そして、更に検討した結果、コーヒー焙煎豆について特定の熟成処理を施すことによって、焙煎豆中のクロロゲン酸類量を一定範囲に保持しつつ、ヒドロキシヒドロキノン含量を低減させることができることを見出し、本発明を完成した。
即ち本発明は、焙煎したコーヒー豆に40〜150℃の温度条件下で、かつ焙煎温度よりも低い温度で熟成処理を施すコーヒー豆の製造方法である。
As a result of various studies based on the hypothesis that some component in coffee may generate hydrogen peroxide in vivo, the present inventor has added hydrogen peroxide to hydroxyhydroquinone contained in coffee in vivo. It has been found that a coffee beverage composition with little hydrogen peroxide production in vivo can be obtained if it has an action to be produced and if the content of hydroxyhydroquinone is less than the amount normally contained. (WO2005 / 072533)
Further, the inventor of the present invention, although chlorogenic acids show an excellent blood pressure lowering action (JP 2002-363075 A, JP 2002 22062 A, JP 2002-53464 A), chlorogenic acids Focusing on the fact that many coffee drinks do not show sufficient blood pressure lowering effect (Eur. J. Clin. Nutr., 53 (11), 831 (1999)) As a result of the examination, it was also found that hydroxyhydroquinone contained in the coffee beverage inhibits the blood pressure lowering action of chlorogenic acids.
And as a result of further investigation, it was found that by subjecting coffee roasted beans to a specific aging treatment, the hydroxyhydroquinone content can be reduced while maintaining the amount of chlorogenic acids in the roasted beans within a certain range. Completed the invention.
That is, the present invention is a method for producing coffee beans in which roasted coffee beans are subjected to aging treatment at a temperature lower than the roasting temperature under a temperature condition of 40 to 150 ° C.
本発明の処理を行ったコーヒー豆を使用すれば、コーヒー抽出液中のクロロゲン酸類量を一定範囲に保持しつつ、血圧降下作用を阻害するヒドロキシヒドロキノン含量が低減し、飲用後の体内での過酸化水素の生成が抑制できるコーヒー抽出液を提供することができる。 By using the coffee beans that have been treated according to the present invention, the content of chlorogenic acids in the coffee extract is kept within a certain range, while the content of hydroxyhydroquinone that inhibits the blood pressure lowering action is reduced, so that the excess in the body after drinking. A coffee extract capable of suppressing the production of hydrogen oxide can be provided.
本発明において、コーヒー豆の種類は、特に限定されないが、例えばブラジル、コロンビア、タンザニア、モカ、キリマンジェロ、マンデリン、ブルーマウンテン等が挙げられる。コーヒー豆種としては、アラビカ種、ロブスタ種などがある。コーヒー豆は1種でもよいし、複数種をブレンドして用いてもよい。
コーヒー豆を焙煎により焙煎コーヒー豆とする方法については、特に制限はなく、焙煎温度、焙煎環境についても制限はないが、好ましい焙煎温度は100〜300℃であり、更に好ましくは150〜250℃、特に好ましくは180〜250℃である。好ましい焙煎方法としては直火式、熱風式、半熱風式があり、回転ドラムを有している形式が更に好ましい。また、風味の観点より焙煎後30分以内に0〜100℃まで、更に好ましくは10〜60℃まで冷却することが好ましい。
In the present invention, the type of coffee beans 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 is no limitation on the roasting temperature and roasting environment, but the preferred roasting temperature is 100 to 300 ° C, more preferably It is 150-250 degreeC, Most preferably, it is 180-250 degreeC. 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 30 minutes after roasting from a viewpoint of flavor, More preferably, it cools to 10-60 degreeC.
焙煎コーヒー豆の焙煎度としては、ライト、シナモン、ミディアム、ハイ、シティ、フルシティ、フレンチ、イタリアン等があり、ライト、シナモン、ミディアム、ハイ、シティが好ましい。焙煎度を色差計で測定したL値としては、通常10〜30、好ましくは15〜25である。尚、焙煎度の違うコーヒー豆を混合しても良い。 As roasting degree of roasted coffee beans, there are light, cinnamon, medium, high, city, full city, French, Italian and the like, and light, cinnamon, medium, high and city are preferable. As L value which measured the roasting degree with the color difference meter, it is 10-30 normally, Preferably it is 15-25. Note that coffee beans having different roasting degrees may be mixed.
本発明は、上記の条件で焙煎した焙煎コーヒー豆(焙煎後、室温まで放冷され、保管されたもの等も含む)について、焙煎温度よりも低い温度条件下の熟成処理を施すことにより、ヒドロキシヒドロキノン含有量を低減するものである。処理温度は40〜150℃、特に好ましくは80〜120℃の温度条件がよい。150℃を超えると有効成分であるクロロゲン酸類が著しく減少するので好ましくない。 In the present invention, roasted coffee beans roasted under the above conditions (including those roasted and then allowed to cool to room temperature and stored) are subjected to an aging treatment under a temperature condition lower than the roasting temperature. Therefore, the hydroxyhydroquinone content is reduced. The treatment temperature is 40 to 150 ° C, particularly preferably 80 to 120 ° C. If the temperature exceeds 150 ° C., chlorogenic acids as active ingredients are remarkably reduced, which is not preferable.
40〜150℃の温度条件下の熟成処理における処理時間としては、30分以上であれば良いが、低温ではなるべく処理時間を長くすると効果が高く、高温であるほど短時間で効果が得られる。好ましい処理時間を具体的に挙げると、40〜70℃では60日以上、70〜100℃では1日以上、100〜150℃であれば30分以上である。処理時間の上限としては、それぞれ、180日、30日、1日であることが、豆の品質を
良好な状態に保つ点で好ましい。
また、熟成処理は、常圧下、加圧下、減圧下、飽和水蒸気下で行うことも可能であるが、窒素などの不活性ガス下または減圧下において酸素濃度が20vol%以下、好ましくは2vol%以下、より好ましくは0.2vol%以下となる雰囲気で行うことが、風味の点で好ましい。
The treatment time in the aging treatment under a temperature condition of 40 to 150 ° C. may be 30 minutes or more, but the effect is high when the treatment time is increased as much as possible at low temperatures, and the effect is obtained in a short time at higher temperatures. Specifically, preferable treatment time is 60 days or more at 40 to 70 ° C, 1 day or more at 70 to 100 ° C, and 30 minutes or more at 100 to 150 ° C. The upper limit of the treatment time is preferably 180 days, 30 days, and 1 day, respectively, from the viewpoint of keeping the quality of the beans in a good state.
The aging treatment may be performed under normal pressure, under pressure, under reduced pressure, or saturated steam, but the oxygen concentration is 20 vol% or less, preferably 2 vol% or less under an inert gas such as nitrogen or under reduced pressure. More preferably, it is performed in an atmosphere of 0.2 vol% or less from the viewpoint of flavor.
熟成方法としては、焙煎後に室温まで冷却した後の焙煎豆に対して加温する方法や、焙煎後に相当時間をかけて徐冷し、40〜150℃の温度条件に焙煎豆を保持する方法が挙げられる。前者の方法が特定温度条件での熟成処理を制御しやすいので好ましい。 As a ripening method, a method of heating the roasted beans after cooling to room temperature after roasting, or a slow cooling over a considerable time after roasting, and the roasted beans to a temperature condition of 40 to 150 ° C. The method of holding is mentioned. The former method is preferable because the aging treatment under a specific temperature condition can be easily controlled.
また、処理するコーヒー焙煎豆は、未粉砕コーヒー豆であっても、粉砕コーヒー豆であっても良いが、未粉砕コーヒー豆を使用すると風味がよくなるので好ましい。
熟成の装置としては、特に制限はなく、焙煎豆静置型、焙煎豆移送型、焙煎豆攪拌型等の装置が使用でき、具体的には棚式乾燥機、コンベア式乾燥機、回転ドラム型乾燥機、回転V型乾燥機などが使用できる。また焙煎機を使用してもよい。加熱源としては、熱風、遠赤外線、赤外線、マイクロ波、過熱水蒸気などがあげられる。
The roasted coffee beans to be processed may be unground coffee beans or ground coffee beans, but the use of unground coffee beans is preferable because the flavor is improved.
There are no particular restrictions on the ripening device, and roasted bean stationary type, roasted bean transfer type, roasted bean stirring type, etc. can be used, specifically shelf type dryer, conveyor type dryer, rotating A drum type dryer, a rotary V type dryer or the like can be used. A roasting machine may also be used. Examples of the heating source include hot air, far infrared rays, infrared rays, microwaves, superheated steam and the like.
コーヒー豆からの抽出方法についても制限はなく、例えば未粉砕の焙煎コーヒー豆又は粉砕物から水〜熱水(0〜100℃)などの抽出溶媒を用いて10秒〜120分抽出する方法が挙げられる。粉砕度合いは、極細挽き(0.250-0.500mm)、細挽き(0.300-0.650mm)、中細挽き(0.530-1.000mm)、中挽き(0.650-1.500mm)、中粗挽き、粗挽き(0.850-2.100mm)、極粗挽き(1.000-2.500mm)や平均粒径3mmや同5mm、同10mm程度のカット品が挙げられる。抽出方法は、ボイリング式、エスプレッソ式、サイホン式、ドリップ式(ペーパー、ネル等)等が挙げられる。 There is no restriction | limiting also about the extraction method from a coffee bean, For example, the method of extracting for 10 second-120 minutes using extraction solvents, such as water-hot water (0-100 degreeC), from an unground roasted coffee bean or ground material. Can be mentioned. The degree of pulverization is as follows: extra fine grinding (0.250-0.500mm), fine grinding (0.300-0.650mm), medium fine grinding (0.530-1.000mm), medium grinding (0.650-1.500mm), medium coarse grinding, coarse grinding (0.850- 2.100 mm), ultra-coarse grind (1.000-2.500 mm), and cut products having an average particle size 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.).
抽出溶媒としては、水、アルコール含有水、ミルク、炭酸水などが挙げられる。抽出溶媒のpHは通常4〜10であり、風味の観点からは5〜7が好ましい。尚、抽出溶媒中にpH調整剤、例えば重炭酸水素ナトリウム、炭酸水素ナトリウム、L−アスコルビン酸、L−アルコルビン酸Naを含有させ、pH調整しても良い。 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. The pH may be adjusted by adding a pH adjusting agent such as sodium bicarbonate, sodium bicarbonate, L-ascorbic acid, or L-alcorbic acid Na to the extraction solvent.
抽出器としては、ペーパードリップ、不織布ドリップ、サイフォン、ネルドリップ、エスプレッソマシン、コーヒーマシン、パーコレーター、コーヒープレス、イブリック、ウォータードリップ、ボイリング、コーヒーカップへ実質的に懸架可能なペーパー又は不織布の袋状構造体、上部にスプレーノズル下部に実質的にコーヒー豆の固液分離可能な構造体(メッシュやパンチングメタルなど)を有するドリップ抽出器、上部及び下部に実質的にコーヒー豆の固液分離可能な構造体(メッシュやパンチングメタルなど)を有するカラム抽出器等が挙げられる。抽出器に加熱又は冷却可能な構造(例えば、電気ヒーター、温水や蒸気、冷水が通液可能なジャケット)を有していても良い。 The extractor includes paper drip, non-woven drip, siphon, nel drip, espresso machine, coffee machine, percolator, coffee press, ibrick, water drip, boiling, coffee or a bag-like non-woven bag structure that can be suspended in a coffee cup. Body, drip extractor having a structure (mesh, punching metal, etc.) capable of substantially separating coffee beans in the lower part of the spray nozzle, and structure capable of substantially separating coffee beans in the upper and lower parts. Examples include a column extractor having a body (such as a mesh or punching metal). 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).
抽出方法としてはバッチ式抽出法、半バッチ式抽出法、連続式抽出法が挙げられる。バッチ式抽出法又は半バッチ式抽出法の抽出時間は風味の観点より10秒〜120分が好ましく、更に30秒〜30分が好ましい。 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.
得られた抽出液のヒドロキシヒドロキノン含量をさらに低減させるために、抽出液を多孔質吸着体に接触させてもよい。
多孔質吸着体としては細孔半径が0.7ナノメーター(nm)以下の細孔の容量が多孔質吸着体の細孔容量全体に対して10%以上である多孔質吸着体を用いる。好ましくは細孔半径が0.7ナノメーター(nm)以下の細孔の容量が多孔質吸着体の細孔容量全体に対して30%以上、更に50%以上、特に70%以上のものが好ましい。細孔半径が0.7ナノメーター(nm)以下の細孔の容量が多孔質吸着体の細孔容量全体に対して10%未満の多孔質吸着体は、ヒドロキシヒドロキノン除去の選択性が低くなるため好ましくない。ここで、多孔質吸着体の細孔半径及び容量は、細孔半径1ナノメーター(nm)以下域においてはMP法により測定された値であり、細孔半径1ナノメーター(nm)超過域においてはKJH法により測定された値であり、細孔半径が0.7ナノメーター(nm)以下の細孔の容量が多孔質吸着体の細孔容量全体に対して10%であるか否かはMP法及びKJH法により得られた細孔分布曲線から判定することができる。ここで、MP法とは、Colloid and Interface Science, 26,46(1968)に記載された細孔測定方法であり、KJH法とは、J. Amer. Chem. Soc., 73, 373(1951)に記載の細孔測定方法であり、株式会社住化分析センター、株式会社東レリサーチセンターにて測定可能である。
In order to further reduce the hydroxyhydroquinone content of the obtained extract, the extract may be brought into contact with the porous adsorbent.
As the porous adsorbent, a porous adsorbent having a pore radius of 0.7 nanometer (nm) or less and a volume of 10% or more of the entire pore volume of the porous adsorbent is used. Preferably, the volume of pores having a pore radius of 0.7 nanometer (nm) or less is 30% or more, more preferably 50% or more, particularly 70% or more with respect to the entire pore volume of the porous adsorbent. . A porous adsorbent having a pore radius of 0.7 nanometer (nm) or less and a pore volume of less than 10% 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 capacity of the porous adsorbent are values measured by the MP method in the region of pore radius of 1 nanometer (nm) or less, and in the region exceeding the pore radius of 1 nanometer (nm). Is a value measured by the KJH method, and whether the capacity of the pores having a pore radius of 0.7 nanometer (nm) or less is 10% with respect to the entire pore capacity of the porous adsorbent is determined. It can be determined from the pore distribution curves obtained by the MP method and the KJH method. Here, the MP method is a pore measurement method described in Colloid and Interface Science, 26, 46 (1968), and the KJH method is J. Amer. Chem. Soc., 73, 373 (1951). And can be measured at Sumika Chemical Analysis Service Co., Ltd. and Toray Research Center, Inc.
多孔質吸着体の種類としては、吸着技術便覧―プロセス・材料・設計―(平成11年1月11日、エヌ・ティー・エス発行、監修者:竹内 雍)に記載されている、炭素質吸着材、シリカ・アルミナ系吸着材、高分子吸着材、キトサン樹脂などが使用できる。コーヒー風味を残存させる観点から、炭素質吸着材が好ましい。
炭素質吸着材としては、ヒドロキシヒドロキノンを高い選択性をもって吸着する観点から、粉末状活性炭、粒状活性炭、活性炭繊維が好ましい。
粉末状及び粒状活性炭の由来原料としては、オガコ、石炭やヤシ殻などがあるが、ヤシ殻由来のヤシ殻活性炭が好ましく、特に、水蒸気などのガスにより賦活した活性炭が好ましい。このような水蒸気賦活活性炭の市販品としては、白鷺WH2c(日本エンバイロケミカルズ株式会社)、太閣CW(二村化学工業株式会社)、クラレコールGL(クラレケミカル株式会社)等を用いることができる。
As the types of porous adsorbents, the carbonaceous adsorption described in Adsorption Technology Handbook-Process / Material / Design- (January 11, 1999, issued by NTS, supervisor: Atsushi Takeuchi) Materials, silica / alumina-based adsorbents, polymer adsorbents, chitosan resins, 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 adsorbing hydroxyhydroquinone with high selectivity.
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 preferable, and activated carbon activated by gas such as water vapor is particularly preferable. As a commercially available product of such a steam activated activated carbon, Hakuho WH2c (Nippon Enviro Chemicals Co., Ltd.), Taiko CW (Nimura Chemical Industry Co., Ltd.), Kuraray Coal GL (Kuraray Chemical Co., Ltd.) and the like can be used.
粉末状及び粒状等の多孔質吸着体の粒子径は特に限定されないが、大きすぎると被吸着体との接触面積が小さくなり、吸着速度が遅くなる。小さすぎるとコーヒー抽出液と活性炭との分離に負荷がかかる。以上の点から平均粒径としては50μm以上2mm以下が好ましく、さらに150μm以上400μm以下が好ましい。 The particle size of the porous adsorbent such as powder or granular is not particularly limited, but if it is too large, the contact area with the adsorbent becomes small and the adsorption speed becomes slow. If it is too small, a load is imposed on the separation between the coffee extract and the activated carbon. From the above points, the average particle size is preferably 50 μm or more and 2 mm or less, and more preferably 150 μm or more and 400 μm or less.
活性炭繊維としては、ファインガード(東邦レーヨン製)のようなポリアクリロニトリル系、アドール(ユニチカ製)のようなピッチ系、クラクティブ(クラレ製)のようなフェノール系、Kフィルター(東洋紡績製)のようなセルロース系、その他フェノール系や綿花系などが挙げられる。 Activated carbon fibers include polyacrylonitriles such as Fineguard (manufactured by Toho Rayon), pitches such as ador (manufactured by Unitika), phenols such as krativ (manufactured by Kuraray), and K filters (manufactured by Toyobo). Such cellulose type, other phenol type, and cotton type.
また、多孔質吸着体の形状は特に限定されず、通常の粉体・粒状はもとより吸着体を繊維に練りこんだもの、各多孔質吸着剤同士で成型したもの、セルロース、不織布、バインダーを用い成型したものでも良い。
当該多孔質吸着体の使用量は、原料コーヒー抽出液の固形分に対して10質量%以上、更に10〜200質量%が好ましい。なお、原料コーヒー抽出液の固形分とは、凍結乾燥などにより原料コーヒー抽出液から水分を除去して得られたものを示す。
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. It may be molded.
The amount of the porous adsorbent used is preferably 10% by mass or more, more preferably 10 to 200% by mass, based on the solid content of the raw coffee extract. In addition, solid content of raw material coffee extract shows what was obtained by removing a water | moisture content from raw material coffee extract by freeze-drying etc.
接触処理手段としては、バッチ法又はカラム通液方法が挙げられる。
バッチ法としては、コーヒー抽出液を含む液に、多孔質吸着剤を加え−10〜100℃で0.5分〜5時間撹拌した後、吸着剤を除去すればよい。処理時の雰囲気としては、空気下、不活性ガス下(窒素ガス、アルゴンガス、ヘリウムガス、二酸化炭素)が挙げられるが、風味の観点より不活性ガス下が好ましい。
Examples of the contact treatment means include a batch method and a column flow method.
As a batch method, a porous adsorbent is added to a liquid containing a coffee extract and stirred at −10 to 100 ° C. for 0.5 minutes to 5 hours, and then the adsorbent is removed. The atmosphere during the treatment includes air and inert gas (nitrogen gas, argon gas, helium gas, carbon dioxide), but inert gas is preferred from the viewpoint of flavor.
カラム通液法としては、吸着カラム内に吸着剤を充填し、コーヒー抽出液を含む液をカラム下部又は上部から通液させ、他方から排出させる。吸着剤の充填高さL及びD(径)の比L/Dは通常0.1〜10である。吸着剤のカラム内への充填量は、通液前に吸着カラムに充填できる量であれば良い。吸着カラムの上段又は下段の少なくとも1つにメッシュ(網)又はパンチングメタルなど有し実質的に吸着剤が漏れ出さない分離構造体を有していれば良い。分離構造体の開口径は、吸着剤の平均粒径より小さければ良く、好ましくは吸着剤の平均粒径の1/2以下、特に好ましくは1/3以下の目開きが良い。具体的な開口径は、0.1〜1000μmである。コーヒー抽出液を含む液の吸着処理温度は−10℃〜100℃で、風味の観点より0〜40℃が好ましい。吸着カラム内の吸着剤量(K[g])対するコーヒー抽出液を含む液流量(QC[g/分])の滞留時間(K/QC)は0.5〜300分である。 In the column liquid passing method, an adsorbent is filled in an adsorption column, and a liquid containing a coffee extract is passed from the lower or upper part of the column and discharged from the other. The ratio L / D of the adsorbent filling height L and D (diameter) is usually 0.1 to 10. The amount of the adsorbent packed into the column may be an amount that can be packed into the adsorption column before passing the liquid. It is sufficient that at least one of the upper and lower stages of the adsorption column has a separation structure that has a mesh (net) or punching metal and does not substantially leak the adsorbent. The opening diameter of the separation structure may be smaller than the average particle diameter of the adsorbent, and preferably has an opening of 1/2 or less, particularly preferably 1/3 or less of the average particle diameter of the adsorbent. A specific opening diameter is 0.1 to 1000 μm. The adsorption treatment temperature of the liquid containing the coffee extract is −10 to 100 ° C., and preferably 0 to 40 ° C. from the viewpoint of flavor. The residence time (K / QC) of the liquid flow rate (QC [g / min]) containing the coffee extract with respect to the adsorbent amount (K [g]) in the adsorption column is 0.5 to 300 minutes.
本発明方法により製造されたコーヒー豆から得られるコーヒー組成物には、糖成分として、グラニュー糖、上白糖、マルトース、スクラロース等が適宜配合でき、乳成分としては、生乳、牛乳、全粉乳、脱脂粉乳、生クリーム、濃縮乳、脱脂乳、部分脱脂乳、練乳等を適宜配合できる。また乳化剤として、ショ糖脂肪酸エステル、グリセリン脂肪酸エステル及びポリグリセンリン脂肪酸エステルなどが使用できる。上記乳化剤は、キサンタンガム、カラギーナンなどの多糖類、カゼイン蛋白質と組み合わせることができる。 In the coffee composition obtained from the coffee beans produced by the method of the present invention, granulated sugar, sucrose, maltose, sucralose and the like can be appropriately blended as sugar components. Powdered milk, fresh cream, concentrated milk, skim milk, partially skimmed milk, condensed milk, and the like can be appropriately blended. As the emulsifier, sucrose fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester and the like can be used. The above emulsifier can be combined with polysaccharides such as xanthan gum and carrageenan, and casein protein.
本発明で用いるコーヒー抽出液は、100gあたりコーヒー豆を生豆換算で1g以上使用したものをいう。好ましくはコーヒー豆を2.5g以上使用しているものである。更に好ましくはコーヒー豆を5g以上使用しているものである。 The coffee extract used in the present invention refers to a coffee bean used in an amount of 1 g or more in terms of green beans per 100 g. Preferably, 2.5 g or more of coffee beans are used. More preferably, 5 g or more of coffee beans are used.
このようなコーヒー抽出液は、通常クロロゲン酸類を0.01〜1質量%含有し、かつ該クロロゲン酸類量の約1質量%のヒドロキシヒドロキノンを含有している。ここで、当該クロロゲン酸類としてはモノカフェオイルキナ酸、フェルラキナ酸、ジカフェオイルキナ酸の三種が知られており、クロロゲン酸類の含有量はこれらの合計量で示される。モノカフェオイルキナ酸としては3−カフェオイルキナ酸、4−カフェオイルキナ酸及び5−カフェオイルキナ酸から選ばれる1種以上が挙げられる。またフェルラキナ酸としては、3−フェルラキナ酸、4−フェルラキナ酸及び3−フェルラキナ酸から選ばれる1種以上が挙げられる。ジカフェオイルキナ酸としては3,4−ジカフェオイルキナ酸、3,5−ジカフェオイルキナ酸及び4,5−ジカフェオイルキナ酸から選ばれる1種以上が挙げられる。 Such a coffee extract usually contains 0.01 to 1% by mass of chlorogenic acids and about 1% by mass of hydroxyhydroquinone in the amount of the chlorogenic acids. Here, as the chlorogenic acids, there are known three types 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.
当該クロロゲン酸類の含有量は、高速液体クロマトグラフィー(HPLC)により測定することができる。HPLCにおける検出手段としては、UV検出が一般的であるが、CL(化学発光)検出、EC(電気化学)検出、LC−Mass検出等により更に高感度で検出することもできる。 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.
当該ヒドロキシヒドロキノン含量は、HPLCにより測定することができる。HPLCにおける検出手段としては、UV検出が一般的であるが、CL検出、EC検出、LC−Mass検出等により更に高感度で検出することもできる。なお、HPLCによるヒドロキシヒドロキノン含量の測定にあたっては、コーヒー溶液を濃縮した後に測定することもできるが、リン酸や塩酸などの添加であらかじめpH3以下に調整するのが好ましい。 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.
実施例1
200℃以上で焙煎された焙煎コーヒー豆粉砕品としてコロンビア豆(L値24)中挽きを使用し、大気下で110℃、20時間の熟成処理を実施した。熟成処理はヤマト科学(株)真空定温乾燥機ADP300を使用した。得られた熟成処理豆0.4kgを80メッシュの金網を備えた内径72mmのカラム抽出機(図1)に仕込み、イオン交換水0.25kg(93℃)をカラム抽出機下部から供給した。次いで、カラム抽出機上部からイオン交換水1.02kg(93℃)を供給したのち、供給を停止し、6分間保持した。その後、カラム抽出機上部からイオン交換水(93℃)を供給しながらカラム抽出機下方から抽出液を抜き出し、1.97kgの抽出液を得た。イオン交換水の供給流量および抽出液の抜き出し速度は4.92kg/hで行った。
Example 1
Colombian beans (L value 24) medium ground was used as a roasted coffee bean pulverized product roasted at 200 ° C. or higher, and aged at 110 ° C. for 20 hours in the atmosphere. The maturing process used Yamato Scientific Co., Ltd. vacuum constant temperature dryer ADP300. 0.4 kg of the resulting ripened beans were charged into a 72 mm inner diameter column extractor (FIG. 1) equipped with an 80 mesh wire net, and 0.25 kg (93 ° C.) of ion-exchanged water was supplied from the bottom of the column extractor. Next, after supplying 1.02 kg (93 ° C.) of ion-exchanged water from the top of the column extractor, the supply was stopped and held for 6 minutes. Thereafter, while supplying ion-exchanged water (93 ° C.) from the upper part of the column extractor, the extract was extracted from below the column extractor to obtain 1.97 kg of extract. The ion exchange water supply flow rate and the extraction liquid extraction rate were 4.92 kg / h.
実施例2
実施例1で使用した焙煎コーヒー豆粉砕品と同じものを、大気下で150℃、20時間の熟成処理を実施した。得られた熟成処理豆0.4kgを使用し、実施例1と同様の条件で抽出を行い、抽出液1.97kgを得た。
Example 2
The same crushed roasted coffee beans used in Example 1 were subjected to aging treatment at 150 ° C. for 20 hours in the atmosphere. Extraction was performed under the same conditions as in Example 1 using 0.4 kg of the resulting ripened beans, and 1.97 kg of an extract was obtained.
実施例3
実施例1で使用した焙煎コーヒー豆粉砕品と同じものに対して、低酸素下で110℃、20時間の熟成処理を実施した。熟成処理はヤマト科学(株)真空定温乾燥機ADP300を使用し、チャンバー内を窒素で置換した後、−0.08MPaGに減圧した雰囲気下で行った。得られた熟成処理豆を中挽きに粉砕し、実施例1と同様の条件で抽出操作を行い、抽出液1.97kgを得た。
Example 3
The same crushed roasted coffee beans used in Example 1 were subjected to aging treatment at 110 ° C. for 20 hours under low oxygen. The aging treatment was performed under an atmosphere reduced to −0.08 MPaG after substituting the inside of the chamber with nitrogen using a vacuum constant temperature dryer ADP300 manufactured by Yamato Scientific Co., Ltd. The resulting ripened beans were ground into medium grinds and subjected to an extraction operation under the same conditions as in Example 1 to obtain 1.97 kg of an extract.
比較例1
実施例1で使用した焙煎コーヒー豆粉砕品と同じものを0.4kg使用し、熟成処理を施さず、実施例1と同様の条件で抽出操作を行い、抽出液1.97kgを得た。
Comparative Example 1
0.4 kg of the same roasted coffee bean pulverized product used in Example 1 was used, an aging treatment was not performed, and an extraction operation was performed under the same conditions as in Example 1 to obtain 1.97 kg of an extract.
実施例1〜3及び比較例1のコーヒー抽出液中のクロロゲン酸類およびヒドロキシヒドロキノン量を分析した。クロロゲン酸は分析条件Kで測定し、ヒドロキシヒドロキノンはHPLC−電気化学検出器により測定した。結果を表1に示す。 The amounts of chlorogenic acids and hydroxyhydroquinone in the coffee extracts of Examples 1 to 3 and Comparative Example 1 were analyzed. Chlorogenic acid was measured under analytical condition K, and hydroxyhydroquinone was measured with an HPLC-electrochemical detector. The results are shown in Table 1.
実施例4
200℃以上で焙煎された焙煎コーヒー豆未粉砕品としてコロンビア豆(L値22)を使用し、低酸素下で110℃、20時間の熟成処理を実施した。熟成処理はヤマト科学(株)真空定温乾燥機ADP300を使用し、チャンバー内を窒素で置換した後、-0.08MPaGに減圧した雰囲気下で行った。得られた熟成処理豆を粉砕し(デロンギ社 KG-100 極粗挽き)、粉砕豆0.04kgに対して10倍量のイオン交換水を使用してコーヒーメーカー(メリタ社 JCM1041)で抽出操作を行った。
Example 4
Colombian beans (L value 22) were used as unmilled roasted coffee beans roasted at 200 ° C. or higher, and aged at 110 ° C. for 20 hours under low oxygen. The aging treatment was performed in an atmosphere using a vacuum constant temperature dryer ADP300 manufactured by Yamato Scientific Co., Ltd., after substituting the inside of the chamber with nitrogen and then reducing the pressure to -0.08 MPaG. The resulting aged beans are pulverized (Delonghi KG-100 ultra-coared ground) and extracted with a coffee maker (Melita JCM1041) using 10 times the amount of ion-exchanged water for 0.04 kg of pulverized beans. It was.
実施例5
実施例4で使用した焙煎コーヒー豆未粉砕品と同じものを、コーヒーミルにて粉砕し(デロンギ社 KG-100 極粗挽き)、低酸素下で120℃、20時間の熟成処理を実施した。熟成処理はヤマト科学(株)真空定温乾燥機ADP300を使用し、チャンバー内を窒素で置換した後、-0.08MPaGに減圧した雰囲気下で行った。得られた熟成処理豆0.04kgに対して実施例4と同様に抽出操作を行い、抽出液を得た。
Example 5
The same roasted coffee beans unground product used in Example 4 was pulverized in a coffee mill (Delonghi KG-100 ultra-coared ground), and aged at 120 ° C. for 20 hours under low oxygen. . The aging treatment was performed in an atmosphere using a vacuum constant temperature dryer ADP300 manufactured by Yamato Scientific Co., Ltd., after substituting the inside of the chamber with nitrogen and then reducing the pressure to -0.08 MPaG. An extraction operation was performed on 0.04 kg of the resulting ripened beans in the same manner as in Example 4.
実施例6
実施例4で使用した焙煎コーヒー豆未粉砕品と同じものを、低酸素下で150℃、0.5時間の熟成処理を実施した。熟成処理はヤマト科学(株)真空定温乾燥機ADP300を使用し、チャンバー内を窒素で置換した後、-0.08MPaGに減圧した雰囲気下で行った。得られた熟成処理豆を粉砕し(デロンギ社 KG-100 極粗挽き)、粉砕豆0.04kgに対して実施例4と同様に抽出操作を行い、抽出液を得た。
Example 6
The same crushed roasted coffee beans used in Example 4 were subjected to aging treatment at 150 ° C. for 0.5 hours under low oxygen. The aging treatment was performed in an atmosphere using a vacuum constant temperature dryer ADP300 manufactured by Yamato Scientific Co., Ltd., after substituting the inside of the chamber with nitrogen and then reducing the pressure to -0.08 MPaG. The obtained ripened beans were pulverized (Delonghi KG-100 ultra-coared ground), and 0.04 kg of pulverized beans were extracted in the same manner as in Example 4 to obtain an extract.
比較例2
焙煎コーヒー豆未粉砕品としてコロンビア豆(L値22)を、コーヒーミルにて粉砕(デロンギ社 KG-100 極粗挽き)し、粉砕豆0.04kgに対して実施例4と同様に抽出操作を行い、抽出液を得た。
Comparative Example 2
Colombian beans (L value 22) as unroasted roasted coffee beans are ground in a coffee mill (Delonghi Co., Ltd. KG-100 ultra-coarse ground), and extraction operation is performed in the same manner as in Example 4 on 0.04 kg of ground beans. And an extract was obtained.
実施例4〜6及び比較例2のコーヒー抽出液中のクロロゲン酸類およびヒドロキシヒドロキノン量を分析した。クロロゲン酸は分析条件で測定し、ヒドロキシヒドロキノンはHPLC−電気化学検出器により測定した。結果を表2に示す。 The amounts of chlorogenic acids and hydroxyhydroquinone in the coffee extracts of Examples 4 to 6 and Comparative Example 2 were analyzed. Chlorogenic acid was measured under analytical conditions, and hydroxyhydroquinone was measured by HPLC-electrochemical detector. The results are shown in Table 2.
実施例7
実施例1で使用した焙煎コーヒー豆粉砕品と同じものを、低酸素下で40℃、60日間熟成処理を実施した。熟成処理は、焙煎コーヒー豆粉砕品を、窒素で置換した後、-0.08MPaGに減圧したデシケーター内に入れ、これをヤマト科学(株)社製のインキュベーターIC801に入れて行った。得られた熟成処理豆0.04kgに対して10倍量のイオン交換水を使用してコーヒーメーカーで抽出を行い、抽出液を得た。抽出にはメリタ社 JCM1041を使用した。
Example 7
The same crushed roasted coffee beans used in Example 1 were subjected to aging treatment at 40 ° C. for 60 days under low oxygen. The ripening treatment was carried out by replacing the roasted coffee bean ground product with nitrogen and then placing it in a desiccator decompressed to -0.08 MPaG, and placing it in an incubator IC801 manufactured by Yamato Scientific Co., Ltd. Extraction was performed with a coffee maker using 10 times the amount of ion-exchanged water for 0.04 kg of the resulting ripened beans. Melita JCM1041 was used for extraction.
比較例3
実施例1で使用した焙煎コーヒー豆粉砕品と同じもの0.04kgに対して実施例7と同様に抽出を行い、抽出液を得た。
実施例7及び比較例3のコーヒー抽出液中のクロロゲン酸類およびヒドロキシヒドロキノン量を分析した。クロロゲン酸は分析条件Kで測定し、ヒドロキシヒドロキノンはHPLC−電気化学検出器により測定した。結果を表3に示す。
Comparative Example 3
Extraction was carried out in the same manner as in Example 7 on 0.04 kg of the same crushed roasted coffee beans used in Example 1, and an extract was obtained.
The amounts of chlorogenic acids and hydroxyhydroquinone in the coffee extracts of Example 7 and Comparative Example 3 were analyzed. Chlorogenic acid was measured under analytical condition K, and hydroxyhydroquinone was measured with an HPLC-electrochemical detector. The results are shown in Table 3.
クロロゲン酸類の分析方法:分析条件
容器詰コーヒー飲料又はコーヒー組成物のクロロゲン酸類の分析法は次の通りである。分析機器はHPLCを使用した。装置の構成ユニットの型番は次の通り。UV−VIS検出器:L−2420((株)日立ハイテクノロジーズ)、カラムオーブン:L−2300((株)日立ハイテクノロジーズ)、ポンプ:L−2130((株)日立ハイテクノロジーズ)、オートサンプラー:L−2200((株)日立ハイテクノロジーズ)、カラム:Cadenza CD−C18 内径4.6mm×長さ150mm、粒子径3μm(インタクト(株))。
分析条件は次の通りである。サンプル注入量:10μL、流量:1.0mL/min、UV−VIS検出器設定波長:325nm、カラムオーブン設定温度:35℃、溶離液A:0.05M 酢酸、0.1mM 1−ヒドロキシエタン−1,1−ジホスホン酸、10mM 酢酸ナトリウム、5(V/V)%アセトニトリル溶液、溶離液B:アセトニトリル。
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.
濃度勾配条件
時間 溶離液A 溶離液B
0.0分 100% 0%
10.0分 100% 0%
15.0分 95% 5%
20.0分 95% 5%
22.0分 92% 8%
50.0分 92% 8%
52.0分 10% 90%
60.0分 10% 90%
60.1分 100% 0%
70.0分 100% 0%
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%
HPLCでは、試料1gを精秤後、溶離液Aにて10mLにメスアップし、メンブレンフィルター(GLクロマトディスク25A,孔径0.45μm,ジーエルサイエンス(株))にて濾過後、分析に供した。
クロロゲン酸類の保持時間(単位:分)
(A1)モノカフェオイルキナ酸:5.3、8.8、11.6の計3点(A2)フェルラキナ酸:13.0、19.9、21.0の計3点(A3)ジカフェオイルキナ酸:36.6、37.4、44.2の計3点。ここで求めた9種のクロロゲン酸類の面積値から5−カフェオイルキナ酸を標準物質とし、質量%を求めた。
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.
HPLC−電気化学検出器によるヒドロキシヒドロキノンの分析方法
コーヒー飲料のヒドロキシヒドロキノンの分析法は次の通りである。分析機器はHPLC−電気化学検出器(クーロメトリック型)であるクーロアレイシステム(モデル5600A、開発・製造:米国ESA社、輸入・販売:エム・シー・メディカル(株))を使用した。装置の構成ユニットの名称・型番は次の通りである。
アナリティカルセル:モデル5010、クーロアレイオーガナイザー、クーロアレイエレクトロニクスモジュール・ソフトウエア:モデル5600A、溶媒送液モジュール:モデル582、グラジエントミキサー、オートサンプラー:モデル542、パルスダンパー、デガッサー:Degasys Ultimate DU3003、カラムオーブン:505。カラム:CAPCELL PAK C18 AQ 内径4.6mm×長さ250mm 粒子径5μm((株)資生堂)。
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
分析条件は次の通りである。
サンプル注入量:10μL、流量:1.0mL/min、電気化学検出器の印加電圧:0mV、カラムオーブン設定温度:40℃、溶離液A:0.1(W/V)%リン酸、0.1mM 1−ヒドロキシエタン−1,1−ジホスホン酸、5(V/V)%メタノール溶液、溶離液B:0.1(W/V)%リン酸、0.1mM 1−ヒドロキシエタン−1,1−ジホスホン酸、50(V/V)%メタノール溶液。
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.
溶離液A及びBの調製には、高速液体クロマトグラフィー用蒸留水(関東化学(株))、高速液体クロマトグラフィー用メタノール(関東化学(株))、リン酸(特級、和光純薬工業(株))、1−ヒドロキシエタン−1,1−ジホスホン酸(60%水溶液、東京化成工業(株))を用いた。 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.).
濃度勾配条件
時間 溶離液A 溶離液B
0.0分 100% 0%
10.0分 100% 0%
10.1分 0% 100%
20.0分 0% 100%
20.1分 100% 0%
50.0分 100% 0%
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%
分析試料の調製は、試料5gを精秤後、0.5(W/V)%リン酸、0.5mM 1−ヒドロキシエタン−1,1−ジホスホン酸、5(V/V)%メタノール溶液にて10mLにメスアップし、この溶液について遠心分離を行い上清を得た。この上清について、ボンドエルートSCX(固相充填量:500mg、リザーバ容量:3mL、ジーエルサイエンス(株))に通液し、初通過液約0.5mLを除いて通過液を得た。この通過液について、メンブレンフィルター(GLクロマトディスク25A,孔径0.45μm,ジーエルサイエンス(株))にて濾過し、速やかに分析に供した。 The analytical sample was prepared by accurately weighing 5 g of the sample, and then adding 0.5 (W / V)% phosphoric acid, 0.5 mM 1-hydroxyethane-1,1-diphosphonic acid, 5 (V / V)% methanol solution. The volume was made up to 10 mL, and this 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.
HPLC−電気化学検出器の上記の条件における分析において、ヒドロキシヒドロキノンの保持時間は、6.38分であった。得られたピークの面積値から、ヒドロキシヒドロキノン(和光純薬工業(株))を標準物質とし、質量%を求めた。 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.
1 カラム抽出機
1A シャワーノズル
2 熱水供給ライン
3 焙煎粉砕豆分離メッシュ
4 熱水供給ライン
5 抽出液抜き出しライン
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