JP5455331B2 - Aroma concentration method using reverse osmosis membrane - Google Patents

Aroma concentration method using reverse osmosis membrane Download PDF

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JP5455331B2
JP5455331B2 JP2008172763A JP2008172763A JP5455331B2 JP 5455331 B2 JP5455331 B2 JP 5455331B2 JP 2008172763 A JP2008172763 A JP 2008172763A JP 2008172763 A JP2008172763 A JP 2008172763A JP 5455331 B2 JP5455331 B2 JP 5455331B2
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怜 藤田
誠 高橋
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T Hasegawa Co Ltd
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Description

本発明は天然原料の良好な香気バランスが保持された、天然香気濃縮物の製造方法に関する。   The present invention relates to a method for producing a natural fragrance concentrate in which a good fragrance balance of a natural raw material is maintained.

逆浸透膜(以下、RO膜とも呼ぶ)は限外濾過膜、精密濾過膜とともに高分子分離膜の一種であり、医薬、食品、工業製品の濾過に普通に用いられている。精密濾過膜は0.01〜数μm程度の微粒子及び微生物が除去できるため除菌や濁質成分の除去に利用され、限外濾過膜はさらに小さな粒子である分子量数百〜数百万の溶質または粒子が分離できるため、醤油や果汁のおり成分の除去や除タンパクに利用されるのに対し、RO膜は浸透圧以上の圧力を高濃度溶液側に加えて溶媒と溶質を分離するため海水淡水化に利用されるほか、牛乳・果汁等の天然物の濃縮にも利用されている。   Reverse osmosis membranes (hereinafter also referred to as RO membranes) are a type of polymer separation membrane as well as ultrafiltration membranes and microfiltration membranes, and are commonly used for filtration of pharmaceuticals, foods, and industrial products. Microfiltration membranes can remove microparticles and microorganisms of about 0.01 to several μm, and are used for sterilization and removal of turbid components. Ultrafiltration membranes are solutes with molecular weights of several hundred to several millions, which are even smaller particles. Or, since the particles can be separated, it is used for removing soy sauce and fruit juice components and deproteinization, whereas RO membranes apply seawater pressure or higher pressure to the high-concentration solution side to separate the solvent and solute from seawater. In addition to desalination, it is also used to concentrate natural products such as milk and fruit juice.

さらに、天然原料を蒸留して得られる香気回収物(以下、回収香と呼ぶ)の濃縮にRO膜を用いるいくつかの提案がある。回収香は、天然原料に水を加えて抽出して得られる抽出物に比べ、香気成分を多く含み、これを抽出物あるいは食品に添加することにより、香気が強化、改善された品質の高い製品が得られるために広く利用されている。   Furthermore, there are some proposals that use RO membranes for concentration of aroma recovery products (hereinafter referred to as recovery aromas) obtained by distilling natural raw materials. Recovered incense contains high aroma components compared to extracts obtained by adding water to natural ingredients and is added to the extract or food to enhance the aroma and improve the quality. Is widely used to obtain

具体的提案として、天然果実から得られる果汁を加熱し、蒸発する芳香成分及び水分を精留塔で濃縮して得られる回収香を逆浸透膜で2〜100倍に濃縮する果実芳香成分の高濃縮液の製造方法(特許文献1)、水産物原料を水蒸気蒸留して得られる香り成分を回収した蒸留液を逆浸透膜で濃縮エキスとし、これを呈味成分を含有する濃縮液と混合した香味の改良された水産物の濃縮エキスの製造方法(特許文献2)、コーヒー抽出液を膜濃縮または凍結濃縮または減圧濃縮して、濃縮液と濃縮除去液とに分け、濃縮除去液を逆浸透膜で濃縮して得られる濃縮香気液を前記濃縮液と混合し、濃縮コーヒー液を得る方法(特許文献3)、コーヒー抽出液を膜濃縮または凍結濃縮して、濃縮液と濃縮除去液とに分け、濃縮除去液を減圧濃縮して得られる濃縮香気液を前記濃縮液と混合し、濃縮コーヒー液を得る方法(特許文献4)、水産物原料を水蒸気蒸留して得た香り成分を逆浸透膜で濃縮しアロマ抽出物としこれと前記水蒸気蒸留残渣の抽出物、あるいはこれとは別に用意した水産物抽出物を混合して得られる香味の優れた水産物の抽出物の製造方法(特許文献5)などが提案されている。   As a concrete proposal, a fruit fragrance component that heats fruit juice obtained from natural fruits and concentrates the aroma component that evaporates and the recovered aroma obtained by concentrating moisture in a rectification tower 2 to 100 times with a reverse osmosis membrane. A method for producing a concentrated liquid (Patent Document 1), a distilled liquid obtained by recovering a fragrance component obtained by steam distillation of a marine product raw material as a concentrated extract with a reverse osmosis membrane, and mixing this with a concentrated liquid containing a taste component The improved method for producing a concentrated extract of marine products (Patent Document 2), the coffee extract is concentrated in a membrane, freeze-concentrated or concentrated under reduced pressure, and separated into a concentrated solution and a concentrated removal solution. The concentrated removal solution is separated by a reverse osmosis membrane. A method of obtaining a concentrated coffee liquid by mixing a concentrated aromatic liquid obtained by concentration with the concentrated liquid (Patent Document 3), membrane concentration or freeze concentration of the coffee extract, and dividing into a concentrated liquid and a concentrated removal liquid, Obtained by concentrating the concentrated removal liquid under reduced pressure A concentrated aroma liquid mixed with the concentrated liquid to obtain a concentrated coffee liquid (Patent Document 4), a fragrance component obtained by steam distillation of a marine product raw material is concentrated by a reverse osmosis membrane to obtain an aroma extract and the water vapor A method for producing an extract of a marine product with excellent flavor obtained by mixing an extract of a distillation residue or a marine product extract prepared separately (Patent Document 5) has been proposed.

しかしながら、前記の提案により得られる回収香の濃縮物の香気回収率はまだ改善の余地が大いにあるとともに、回収香の濃縮物の香気バランスが濃縮前と比較して著しく崩れ、良好な天然感が損なわれるという欠点があった。   However, there is still much room for improvement in the fragrance recovery rate of the recovered scent concentrate obtained by the above proposal, and the fragrance balance of the recovered scent concentrate is significantly disrupted compared to before concentration, and a good natural feeling is obtained. There was a drawback of being damaged.

特開平8−215号公報JP-A-8-215 特開平9−9908号公報Japanese Patent Laid-Open No. 9-9908 特開2003−204757号公報JP 2003-204757 A 特開2003−319749号公報JP 2003-319749 A 特開2004−89141号公報JP 2004-89141 A

本発明は、香気の減少が少なく、香気バランスの良い、優れた天然香気濃縮物の製造方法に関する。   The present invention relates to a method for producing an excellent natural fragrance concentrate having a small fragrance reduction and good fragrance balance.

本発明者らは、天然原料を蒸留して得られる回収香のRO膜を用いる濃縮方法の前記の欠点を克服すべく、種々の検討を行った。まず、本発明者が行った実験で、回収香をRO膜で濃縮すると、香気成分の一部が膜に吸着するという事実、また、香気成分のかなりの部分が膜を通過するという事実、通過液と元の回収香の香気成分の組成に違いがあるという事実を確認した。   The present inventors have made various studies in order to overcome the above-mentioned drawbacks of the concentration method using the RO membrane of recovered incense obtained by distilling natural raw materials. First, in the experiment conducted by the present inventor, when the collected incense is concentrated on the RO membrane, the fact that a part of the aroma component is adsorbed on the membrane, and the fact that a substantial part of the aroma component passes through the membrane, the passage The fact that there is a difference in the composition of the aroma components of the liquid and the original recovered incense was confirmed.

本発明者らは、その原因を次のように推測した。すなわち、水蒸気蒸留などにより香気成分を分離、回収した回収香は、天然抽出物を濃縮する場合のような目詰まり(ファウリング)の原因となる水溶性成分、あるいは熱水には溶解し、常温あるいはそれ以下の温度で徐々に沈殿として析出する成分が除去されているために、RO膜による濃縮の際、水の通過速度が速く、濃縮時間は短いものの、香気成分が水の中に希薄な状態で存在するために膜に吸着され易くなり、膜も通過し易くなると推測するとともに、あえて水溶性成分を意図的に回収香に加えてRO膜濃縮を行えば、香気成分の吸着あるいは通過を押さえられるのではないかと考えた。   The present inventors speculated the cause as follows. In other words, the recovered fragrance, which is separated and recovered by steam distillation or the like, is dissolved in water-soluble components or hot water that cause clogging (fouling) as in the case of concentrating natural extracts, Alternatively, since the components that gradually precipitate as a precipitate at a temperature lower than that are removed, the concentration of the RO membrane is high, while the passing speed of water is high and the concentration time is short, but the aroma components are diluted in the water. It is presumed that it will be easily adsorbed on the membrane because it exists in the state, and the membrane will also pass easily. If the RO membrane concentration is intentionally added to the recovered incense, the adsorption or passage of the aroma component will be prevented. I thought it could be suppressed.

そこで天然原料を蒸留して香気を含む香気回収香を得た後、この蒸留残渣に水を加えて抽出するか、またはこれとは別に用意した天然原料に水を加えて抽出することにより得られる抽出液の一部または全量を香気を含む留出液に混合後、RO膜を用いて濃縮したところ、推測の通り、香気の減少が押さえられ、香気バランスの良い優れた天然香気濃縮物が得られることを見いだし、本発明を完成するに至った。   Therefore, after the natural raw material is distilled to obtain an aroma-recovered incense containing a fragrance, it is extracted by adding water to the distillation residue, or extracted by adding water to a natural raw material prepared separately. After mixing a part or all of the extract with a distillate containing fragrance and concentrating it using an RO membrane, as expected, the reduction of fragrance is suppressed, and an excellent natural fragrance concentrate with a good fragrance balance is obtained. As a result, the present invention has been completed.

かくして、本発明は、天然原料を蒸留して香気を含む留出液を得る工程、天然原料に水を加えて抽出して抽出液を得る工程、前記の香気を含む留出液に前記抽出液の一部または全量を混合後、逆浸透膜を用いて濃縮することを特徴とする天然香気濃縮物の製造方法を提供するものである。   Thus, the present invention provides a step of obtaining a distillate containing a fragrance by distilling a natural raw material, a step of obtaining an extract by adding water to the natural raw material, and extracting the extract into the distillate containing the fragrance. The present invention provides a method for producing a natural fragrance concentrate, which comprises mixing a part or the whole of the fragrance with a reverse osmosis membrane.

本発明は、天然原料を水蒸気蒸留して香気を含む留出液得るとともに、該留出液を得る際の水蒸気蒸留残渣を天然原料として、これに水を加えて抽出して抽出液を得ることを特徴とする前記に記載の方法を提供するものである。   The present invention provides a distillate containing a fragrance by steam distillation of a natural raw material, and a water vapor distillation residue when obtaining the distillate is used as a natural raw material, and water is added to this to obtain an extract. The above-mentioned method is provided.

本発明は、天然原料がコーヒーまたは茶類である前記のいずれかに記載の方法を提供するものである。   The present invention provides the method according to any one of the above, wherein the natural raw material is coffee or tea.

本発明によれば、コーヒー、茶、水産物原料などの回収香の濃縮において香気の減少が押さえられ、香気バランスの良い優れた天然香気濃縮物を提供することができる。本発明の方法により得られる天然香気濃縮物は、例えば、飲食品に配合することにより従来の方法によって得られる天然香気濃縮物を配合する場合に比べ、香気バランスが良く、香気の増強された飲食品を提供することができる。   ADVANTAGE OF THE INVENTION According to this invention, the reduction | decrease of a fragrance | flavor is suppressed in concentration of collection | recovery fragrance | flavors, such as coffee, tea, and a marine product raw material, and the outstanding natural fragrance | flavor concentrate with a favorable fragrance balance can be provided. The natural fragrance concentrate obtained by the method of the present invention has a better fragrance balance and a fragrance-enhanced food and drink, for example, by blending in a food and drink with a natural fragrance concentrate obtained by a conventional method. Goods can be provided.

以下、本発明についてさらに詳細に説明する。
本発明の方法において原料で使用しうる天然原料として、例えば、コーヒー、茶類(緑茶、紅茶、中国茶、麦茶、玄米茶、ハブ茶など)、ハーブ類(ラベンダー、シソ、ジャスミン、 セージ、オレガノ、ベルガモット、ホップ、レモンバーム、カモミール、ローズマリー、 タイム、ミント、コリアンダーなど)、果実(リンゴ、ブドウ、パイナップル)、ナッツ類(クルミ、栗、ピーナッツなど)、水産物(鰹節、スルメ、甲殻類など)を挙げることができるがこれらに限定されるものではない。
Hereinafter, the present invention will be described in more detail.
Examples of natural raw materials that can be used as raw materials in the method of the present invention include coffee, tea (green tea, black tea, Chinese tea, barley tea, brown rice tea, hub tea, etc.) and herbs (lavender, perilla, jasmine, sage, oregano) , Bergamot, hops, lemon balm, chamomile, rosemary, thyme, mint, coriander), fruits (apples, grapes, pineapples), nuts (walnuts, chestnuts, peanuts, etc.) However, it is not limited to these.

これら天然原料は生のままで使用しても良いが、焙煎、焙焼などの加熱処理により、香気を増強あるいは改善して使用しても良い。また、必要に応じて粉砕を行い、蒸留による香気回収率の改善を行っても良い。   These natural raw materials may be used as they are, but they may be used after enhancing or improving the aroma by heat treatment such as roasting or roasting. Moreover, you may grind | pulverize as needed and may improve the aroma collection | recovery rate by distillation.

例えば、コーヒー豆の焙煎に使用する原料生豆としては、アラビカ種、リベリカ種、ロブスタ種等いずれでも良く、その種類、産地を問わずブラジル、コロンビア、インドネシア種等いずれの産地のコーヒー豆も使用することができる。また、原料生豆は、一種類の豆のみを単独で使用しても、またブレンドした二種類以上の豆を使用してもよい。   For example, raw green beans used for roasting coffee beans may be any of Arabica, Riberica, Robusta, etc., and any coffee beans of any origin, such as Brazil, Colombia, Indonesia, etc. Can be used. In addition, as raw raw beans, only one kind of beans may be used alone, or two or more kinds of blended beans may be used.

これらの生豆をコーヒーロースターにより焙煎したものを原料とすることができる。焙煎の方法としてはコーヒーロースターなどを用い常法により行うことができる。例えば、コーヒー生豆を回転ドラムの内部に投入し、この回転ドラムを回転攪拌しながら、下方からガスバーナー等で加熱することで焙煎できる。かかるコーヒー豆の焙煎の程度は、通常飲用に供される程度の焙煎であればいかなる範囲内でも良いが、L値として16〜30に焙煎することを例示できる。L値とはコーヒーの焙煎の程度を表す指標で、コーヒー焙煎豆の粉砕物の明度を色差計で測定した値である。黒をL値0で、白をL値100で表す。従って、コーヒー豆の焙煎が深いほど数値は低い値となり、浅いほど高い値となる。参考までに、通常飲用に利用される焙煎豆のL値はほぼ次に示す程度である。イタリアンロースト:16〜19、フレンチロースト:19〜21、フルシティーロースト:21〜23、シティーロースト:23〜25、ハイロースト:25〜27、ミディアムロースト:27〜29。   A raw material obtained by roasting these green beans with a coffee roaster can be used. As a roasting method, a coffee roaster or the like can be used in a conventional manner. For example, it can be roasted by putting green coffee beans inside a rotating drum and heating the rotating drum from below with a gas burner or the like while rotating and stirring. The degree of roasting of such coffee beans may be in any range as long as it is roasted to the extent that it is usually used for drinking, but roasting to 16-30 as the L value can be exemplified. The L value is an index representing the degree of roasted coffee, and is a value obtained by measuring the lightness of the crushed coffee beans with a color difference meter. Black is represented by an L value of 0 and white is represented by an L value of 100. Accordingly, the deeper the roasted coffee beans, the lower the value and the shallower the value, the higher the value. For reference, the L value of roasted beans that are normally used for drinking is approximately the following level. Italian roast: 16-19, French roast: 19-21, Full city roast: 21-23, City roast: 23-25, High roast: 25-27, Medium roast: 27-29.

焙煎コーヒー豆は引き続き粉砕を行うが、粉砕方法についても特に制限はなく、いかなる粉砕方法、粉砕粒度も採用することができ、粉砕装置も、特に限定されるものではない。しかしながら、外気と接触せず、不活性気体中で適宜冷却でき短時間で粉砕できる装置を採用することにより香気の飛散が防止できるためより好ましい。   The roasted coffee beans are subsequently pulverized, but the pulverization method is not particularly limited, any pulverization method and pulverization particle size can be adopted, and the pulverization apparatus is not particularly limited. However, it is more preferable to employ an apparatus that can be appropriately cooled in an inert gas and can be pulverized in a short time without coming into contact with the outside air, since it can prevent the fragrance from being scattered.

茶類、ハーブ類、ナッツ類、水産物などの焙煎または焙焼品は、市販品を用いるか、あるいは焙煎または焙焼に通常、使用される装置を用い、嗜好に適した焙煎または焙焼を行うことにより得ることもできる。   For roasting or roasting products such as teas, herbs, nuts, marine products, etc., commercially available products are used, or roasting or roasting suitable for taste is performed using equipment normally used for roasting or roasting. It can also be obtained by baking.

水蒸気蒸留法は天然原料に水蒸気を通気し、水蒸気に伴われて留出してくる香気成分を水蒸気とともに凝縮させる方法であり、加圧水蒸気蒸留、常圧水蒸気蒸留、減圧水蒸気蒸留、気−液多段式交流接触蒸留(スピニングコーンカラム)などの方法を採用することができる。   The steam distillation method is a method in which steam is passed through a natural raw material, and the aromatic component distilled out accompanying the steam is condensed together with the steam, pressurized steam distillation, atmospheric steam distillation, vacuum steam distillation, gas-liquid multistage type A method such as AC catalytic distillation (spinning cone column) can be employed.

例えば、常圧水蒸気蒸留を用いる方法は、焙煎コーヒー豆を仕込んだ水蒸気蒸留釜の底部から水蒸気を吹き込み、上部の留出側に接続した冷却器で留出蒸気を冷却することにより、凝縮物として香気を含む留出液を捕集することができる。必要に応じて、この香気捕集装置の先に冷媒を用いたコールドトラップを接続することにより、より低沸点の香気成分をも確実に捕集することができる。また、水蒸気蒸留の際に、窒素ガスなどの不活性ガス及び/又はビタミンCなどの抗酸化剤の存在下で蒸留すると、香気成分の加熱による劣化を効果的に防止することができるので好適である。水蒸気蒸留では蒸留の初期に香気が多く留出し、その後、徐々に香気の留出が少なくなる。どこで蒸留を終了するかは、何回かの結果を参考に経済性等も考慮して決めるが、その結果、焙煎コーヒー豆に対する回収香の割合は重量換算で1:0.5〜1:5程度となり、Bx0.5〜5°程度の回収香が得られる。   For example, in the method using atmospheric steam distillation, steam is blown from the bottom of a steam distillation kettle charged with roasted coffee beans, and the condensate is cooled by cooling the distillate with a cooler connected to the upper distillate side. A distillate containing a fragrance can be collected. If necessary, by connecting a cold trap using a refrigerant to the end of the scent collecting device, a scent component having a lower boiling point can be reliably collected. In addition, when steam distillation is carried out in the presence of an inert gas such as nitrogen gas and / or an antioxidant such as vitamin C, it is preferable because deterioration due to heating of aroma components can be effectively prevented. is there. In steam distillation, a large amount of aroma is distilled off at the beginning of distillation, and thereafter, the distillation of aroma is gradually reduced. Where to end the distillation is determined in consideration of economics and the like with reference to the results of several times. As a result, the ratio of the recovered scent to roasted coffee beans is 1: 0.5 to 1: The recovered scent of about Bx 0.5 to 5 ° is obtained.

例えば、焙煎粉砕コーヒー豆を水と混合しスラリーとして、それを気−液向流接触法により香気回収する方法は、例えば、特公平7−22646号公報に記載の装置を用いて抽出する方法を採用することができる。この装置を用いて香気を回収する手段を具体的に説明すると、回転円錐と固定円錐が交互に組み合わせられた構造を有する気−液向流接触抽出装置の回転円錐上に、液状またはペースト状の嗜好性飲料用原料を上部から流下させると共に、下部から蒸気を上昇させ、該原料に本来的に存在している香気成分を回収する方法を例示することができる。この気−液向流接触抽出装置の操作条件としては、該装置の処理能力、原料の種類および濃度、香気の強度その他によって任意に選択することができる。コーヒースラリーのコーヒー豆と水の比率は、コーヒースラリーが流動性をもつ状態となる量であればいかなる比率も採用することができるがおおよそ、コーヒー豆1重量部に対し水5倍量〜30倍量を例示することができる。水が、この範囲を下回る場合、流動性が出にくく、また、水がこの範囲をはずれて多い場合、得られる留出液の香気が弱くなる傾向がある。   For example, a method in which roasted and ground coffee beans are mixed with water to form a slurry, and the flavor is recovered by a gas-liquid countercurrent contact method is, for example, a method of extraction using an apparatus described in Japanese Patent Publication No. 7-22646 Can be adopted. The means for recovering fragrance using this apparatus will be described in detail. On the rotating cone of the gas-liquid countercurrent contact extraction apparatus having a structure in which rotating cones and fixed cones are alternately combined, a liquid or paste-like structure is used. An example is a method in which a raw material for a palatable beverage is caused to flow down from the upper part and a vapor is raised from the lower part to recover an aroma component originally present in the raw material. The operating conditions of this gas-liquid countercurrent contact extraction apparatus can be arbitrarily selected depending on the processing capacity of the apparatus, the type and concentration of the raw material, the intensity of the aroma, and the like. The ratio of coffee beans to water in the coffee slurry can be any ratio as long as the coffee slurry is in a fluid state, but is approximately 5 to 30 times the amount of water with respect to 1 part by weight of the coffee beans. The amount can be exemplified. When water falls below this range, fluidity is difficult to occur, and when water is outside this range, the aroma of the resulting distillate tends to be weak.

気−液向流接触抽出装置の操作条件の一例を示せば、下記のごとくである。
原料供給速度:300〜700L/hr
蒸気流量:5〜50Kg/hr
蒸発量:3〜35Kg/hr
カラム底部温度:40〜100℃
カラム上部温度:40〜100℃
真空度:大気圧〜−100kPa(大気圧基準)
次に、天然原料に水を加えて抽出して抽出液を得る工程では、天然原料として上記の如き水蒸気蒸留を行った後の残渣を用いる場合と、上記の如き水蒸気蒸留とは全く別に、新たな天然原料を用いる場合の2通りの場合がある。しかしながら、手順は基本的に同じであり、上記の如き水蒸気蒸留を行った後の残渣を用いる場合で説明する。
An example of the operating conditions of the gas-liquid countercurrent contact extraction device is as follows.
Raw material supply speed: 300 to 700 L / hr
Steam flow rate: 5 to 50 kg / hr
Evaporation amount: 3 to 35 kg / hr
Column bottom temperature: 40-100 ° C
Column top temperature: 40-100 ° C
Degree of vacuum: atmospheric pressure to -100 kPa (based on atmospheric pressure)
Next, in the step of adding water to the natural raw material and extracting it to obtain an extract, the residue after the steam distillation as described above is used as the natural raw material, and the steam distillation as described above is completely separate. There are two cases of using natural raw materials. However, the procedure is basically the same, and the case will be described where the residue after the steam distillation as described above is used.

例えば、水蒸気蒸留残渣に対して、1〜5倍量の水を加え、5℃〜95℃の範囲の温度で0.5〜24時間の抽出を行い、濾過後、30℃以下に冷却し、Bx2〜10°程度の抽出液が得られる。   For example, 1 to 5 times the amount of water is added to the steam distillation residue, extraction is performed at a temperature in the range of 5 ° C to 95 ° C for 0.5 to 24 hours, and after filtration, the solution is cooled to 30 ° C or less. An extract of about Bx 2 to 10 ° is obtained.

濾過は、ろ紙、サラン、ネルを用い、不溶成分等の除去を行うが、その際、濾過助剤を併用しても良く、例えば、ケイソウ土、酸性白土、活性白土、タルク類、粘土、ゼオライト、粉末セルロース等を挙げることができるがこれらに限定されるものではない。さらに、濾過とは異なる手段として遠心分離で不純物の除去を行うことも効果的であり、単独、あるいは濾過と併用しても良い。   Filtration uses filter paper, saran, and nell to remove insoluble components. In this case, a filter aid may be used in combination, for example, diatomaceous earth, acidic clay, activated clay, talc, clay, zeolite. Examples thereof include, but are not limited to, powdered cellulose. Further, it is effective to remove impurities by centrifugation as a means different from filtration, and it may be used alone or in combination with filtration.

また、この水抽出時および/または水抽出後に酵素を用いても良い。例えば、アミラーゼ、セルラーゼ、マンナナーゼ、プロテアーゼ、リパーゼなどの酵素を作用させることもできる。また、場合により、水溶性有機溶媒の添加も効果的である。例えば、メタノール、エタノール、n−プロパノール、イソプロパノール、ブタノール、2−ブタノール、t−ブタノールなどのアルコール類;アセトンのようなケトン類;エチレングリコール、プロピレングリコール、グリセリン、1,3−ブチレングリコール、1,2−ブチレングリコール、ジプロピレングリコールなどの多価アルコール類などの一種もしくはそれらの複数種の混合物などを例示することができる。ただし、RO膜は高濃度の水溶性溶媒には弱いので、RO膜濃縮の際には溶媒をほとんど除去するか、膜に影響を与えない程度にする必要がある。   Moreover, you may use an enzyme at the time of this water extraction and / or after water extraction. For example, enzymes such as amylase, cellulase, mannanase, protease and lipase can be allowed to act. In some cases, addition of a water-soluble organic solvent is also effective. For example, alcohols such as methanol, ethanol, n-propanol, isopropanol, butanol, 2-butanol, t-butanol; ketones such as acetone; ethylene glycol, propylene glycol, glycerin, 1,3-butylene glycol, 1, Examples thereof include one kind of polyhydric alcohols such as 2-butylene glycol and dipropylene glycol or a mixture of plural kinds thereof. However, since the RO membrane is weak against high-concentration water-soluble solvents, it is necessary to remove almost all of the solvent or not to affect the membrane when the RO membrane is concentrated.

香気を含む留出液全量に対して上記抽出液の一部、または全量を混合し、RO膜濃縮を行う。その混合割合は、留出液を得るのに使用した天然原料の量(a)および抽出液を得るのに使用した天然原料の量(b)の比率、(a:b)で示せば、1:3〜10:1の範囲、好ましくは1:1〜5:1の範囲、より好ましくは1:1〜3:1の範囲を挙げることができる。留出液に由来する固形分に対して抽出液に由来する固形分の量が多いほど香気回収率は高くなり、香気濃縮物の香気は濃縮前の回収香の香気に近くなる。一方、香気濃縮率はRO膜濃縮の場合、通常、約Bx30°が濃縮の限界なので、香気の濃縮度を高くするためには、抽出物由来の香気成分以外の固形分の量が少ない方が好ましい。したがって、得られる香気濃縮物の香気の質、濃縮度を考慮して、回収香と抽出液の混合割合を決めるが、その比率を変えることにより、香気濃縮倍率が1.1〜10程度の香気濃縮物を得ることができる。得られる香気濃縮物は呈味成分などの不揮発性の水溶性成分も含むため、食品の風味をより一層改善する。   A part or all of the extract is mixed with the total amount of the distillate containing aroma, and RO membrane concentration is performed. The mixing ratio is the ratio of the amount (a) of the natural raw material used to obtain the distillate and the amount (b) of the natural raw material used to obtain the extract. : The range of 3-10: 1, Preferably it is the range of 1: 1-5: 1, More preferably, the range of 1: 1-3: 1 can be mentioned. The larger the amount of solid content derived from the extract than the solid content derived from the distillate, the higher the fragrance recovery rate, and the fragrance of the fragrance concentrate becomes closer to the fragrance of the recovered fragrance before concentration. On the other hand, in the case of RO membrane concentration, the concentration of fragrance is normally about Bx30 °, which is the limit of concentration. Therefore, in order to increase the concentration of fragrance, the amount of solids other than the fragrance component derived from the extract should be smaller. preferable. Therefore, the mixing ratio of the recovered fragrance and the extract is determined in consideration of the fragrance quality and concentration of the obtained fragrance concentrate. By changing the ratio, the fragrance having an odor concentration ratio of about 1.1 to 10 is determined. A concentrate can be obtained. Since the obtained fragrance concentrate also contains non-volatile water-soluble components such as a taste component, the flavor of the food is further improved.

本発明で用いるRO膜は、その材質、分子構造など特に限定はないが、例えば、市販品であるSU−720(食塩阻止率99.4%)、SU−720F(食塩阻止率99.4%)、SU−720L(食塩阻止率99.0%)、SU−820(食塩阻止率99.75%)、SU−820L(食塩阻止率99.7%)、以上、東レ株式会社製RO膜;低圧スパイラル型ROエレメントNTR−759HR(食塩阻止率99%)、低圧スパイラル型ROエレメントLF10シリーズ(食塩阻止率98.5%)、低圧スパイラル型ROエレメントES10(食塩阻止率99.5%)、低圧スパイラル型ROエレメントES15−D(食塩阻止率99.5%)、低圧スパイラル型ROエレメントES20−D(食塩阻止率99.7%)、低圧スパイラル型ROエレメントES15−U(食塩阻止率93%)、NTR70HG S2F(食塩阻止率99%)、NTR759HG S2F(食塩阻止率99%)、以上、日東電工社製RO膜;フィルムテックSW30−HR320(食塩阻止率99.4%)、フィルムテックSW30−HR380(食塩阻止率99.4%)、フィルムテックSW30−XLE400i(食塩阻止率99.6%)、以上、ムロマチテクノス社製RO膜等を挙げることができる。特に食塩阻止率99%以上の膜は香気バランスの良い天然濃縮エキスが得られるので好ましい。   The RO membrane used in the present invention is not particularly limited in its material, molecular structure and the like. For example, commercially available products are SU-720 (salt blocking rate 99.4%), SU-720F (salt blocking rate 99.4%). ), SU-720L (salt blocking rate 99.0%), SU-820 (salt blocking rate 99.75%), SU-820L (salt blocking rate 99.7%), and above, RO membrane manufactured by Toray Industries, Inc .; Low pressure spiral RO element NTR-759HR (salt rejection 99%), low pressure spiral RO element LF10 series (salt rejection 98.5%), low pressure spiral RO element ES10 (salt rejection 99.5%), low pressure Spiral RO element ES15-D (salt rejection 99.5%), low pressure spiral RO element ES20-D (salt rejection 99.7%), low pressure spiral RO element ES15-U (salt blocking rate of 93%), NTR70HG S2F (salt blocking rate of 99%), NTR759HG S2F (salt blocking rate of 99%), RO membrane manufactured by Nitto Denko Corporation; Filmtec SW30-HR320 (salt blocking) Rate 99.4%), film tech SW30-HR380 (salt blocking rate 99.4%), film tech SW30-XLE400i (salt blocking rate 99.6%), and more, RO membranes manufactured by Muromachi Technos, Inc. it can. In particular, a membrane having a salt rejection of 99% or more is preferable because a natural concentrated extract having a good aroma balance can be obtained.

食塩阻止率は逆浸透膜の透過性を表す数値であり、水中でNaイオンとClイオンに解離している食塩の透過しにくさを示し、食塩阻止率99%のように表示され、一般に市販品では食塩阻止率90〜99.8%程度のものがある。また、実際の逆浸透膜を含む濃縮装置は、着脱可能な円筒状の膜モジュール、膜モジュールに濃縮しようとする液を循環して供給するポンプ部、コントロール部などからなる装置である場合が多いが、形式はどんなものでも良い。   The salt rejection is a numerical value representing the permeability of the reverse osmosis membrane and indicates the difficulty of permeation of the salt dissociated into Na ions and Cl ions in water. It is displayed as a salt rejection of 99% and is generally commercially available. Some products have a salt rejection of 90-99.8%. In addition, a concentration device including an actual reverse osmosis membrane is often a device comprising a detachable cylindrical membrane module, a pump unit that circulates and supplies a liquid to be concentrated to the membrane module, a control unit, and the like. However, any format is acceptable.

RO膜による濃縮は0.1〜50MPaの操作圧力で行う。また、操作温度は濃縮を行う天然原料によって適宜選択するが、例えば、5〜50℃程度の温度範囲で行う。一般に温度が高い方が水の透過速度が大きくなるが、含有する成分の溶解性、安定性、逆浸透膜への吸着性なども原料により異なるので、好ましい温度を検討してから実際の操作を行う。RO膜濃縮の進行に伴って水が膜を通過し、除去される結果、濃縮液の固形分濃度が上昇し、濃縮液の粘性が高くなり、通常、約Bx30°程度まで濃縮すると、濃縮液は膜、ポンプおよびこれらを連結するパイプ内を循環することが困難になり、実質的に水の通過が止まる。このレベルまで濃縮するか、あるいはそれ以前の任意の段階で濃縮を終了する。   Concentration with the RO membrane is performed at an operating pressure of 0.1 to 50 MPa. The operating temperature is appropriately selected depending on the natural raw material to be concentrated, and is, for example, in a temperature range of about 5 to 50 ° C. In general, the higher the temperature, the greater the permeation rate of water, but the solubility and stability of the components contained, and the adsorptivity to the reverse osmosis membrane also differ depending on the raw materials. Do. As the RO membrane concentration progresses, water passes through the membrane and is removed. As a result, the concentration of the solid content of the concentrate increases, and the viscosity of the concentrate increases. Makes it difficult to circulate through the membrane, the pump and the pipe connecting them, and the passage of water is substantially stopped. Concentrate to this level or terminate the enrichment at any previous stage.

上記した方法により得られる本発明の天然香気濃縮物は、そのまま水溶液の形態として使用することもできるが、所望により該エキスにデキストリン、加工澱粉、サイクロデキストリン、アラビアガム等の賦形剤を添加又は添加しないで、ペースト状とすることもでき、さらにまた、噴霧乾燥、真空乾燥、凍結乾燥などの適宜な乾燥手段を採用して乾燥することにより粉末状とすることもできる。   The natural fragrance concentrate of the present invention obtained by the method described above can be used as it is in the form of an aqueous solution, but if desired, an excipient such as dextrin, modified starch, cyclodextrin, gum arabic or the like is added to the extract. Without addition, it can be made into a paste, and it can also be made into a powder by drying using an appropriate drying means such as spray drying, vacuum drying or freeze drying.

本発明の天然香気濃縮物は、所望により、他の方法で得られる天然抽出エキス、香料、抗酸化剤、色素、ビタミンなどの任意の食品素材または添加剤を添加することもできる。   If desired, the natural fragrance concentrate of the present invention may be added with any food material or additive such as natural extract, fragrance, antioxidant, pigment and vitamin obtained by other methods.

かくして、本発明によれば、例えば、清涼飲料、炭酸飲料、乳飲料、機能性飲料などの飲料類;キャンディー、クッキー、ケーキ、ゼリーなどの菓子類などに天然濃縮物の適当量を添加することにより、天然原料の持つ、バランスのよい、良好な天然風味が付与された飲食品を提供することができる。また、本発明によれば、例えば、シャンプー類、ヘアクリーム類、その他の毛髪化粧料基剤;オシロイ、口紅、その他の化粧用基剤や化粧用洗剤類基剤;洗濯用洗剤類、消毒用洗剤類、防臭洗剤類、その他各種の保健・衛生用洗剤類;歯磨き、ティシュー、トイレトペーパーなどの各種保健・衛生材料類;医薬品類などに天然濃縮物の適当量を添加することにより、天然感の向上した、嗜好性の高い消費財を提供することができる。
以下、本発明を実施例および比較例によりさらに具体的に説明する。
Thus, according to the present invention, for example, an appropriate amount of natural concentrate is added to beverages such as soft drinks, carbonated drinks, milk drinks and functional drinks; confectionery such as candies, cookies, cakes and jellies. Thus, it is possible to provide a food / beverage product with a good natural flavor with a good balance that the natural raw material has. In addition, according to the present invention, for example, shampoos, hair creams, other hair cosmetic bases; osiroy, lipstick, other cosmetic bases and cosmetic detergent bases; laundry detergents, disinfectants Detergents, deodorant detergents, and other various health and hygiene detergents; various health and hygiene materials such as toothpaste, tissue, and toilet paper; natural by adding an appropriate amount of natural concentrate to pharmaceuticals It is possible to provide consumer goods with improved taste and high palatability.
Hereinafter, the present invention will be described more specifically with reference to Examples and Comparative Examples.

実施例1
市販の焙煎コーヒー豆であるブラジルサントス#2(L値16.5)10kgを内径27cm、高さ57cmの三連のステンレス製カラムのそれぞれに充填し、100〜105℃で2.5時間、水蒸気蒸留を行い、留出液54kg(参考品1、pH3.28)を得た。次にそれぞれのカラムに90℃の軟水30kgを加え、90〜95℃で30分間保持した後、1時間放置し、蒸留残渣の抽出を行い、濾過することにより抽出液81kg(Bx8.48°)を得た。上記の留出液9kgに抽出液13.5kgを加え、重曹にてpH5.01としたものをRO膜濃縮機NTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理後、遠沈処理(20℃、800×G、5分間)を行い、Bx20°に調整し、200メッシュ濾過を行い、濃縮液5.7kg(本発明品1、Bx20°、対留出液濃縮倍率:1.58)を得た。
Example 1
10 kg of commercially available roasted coffee beans, Brazil Santos # 2 (L value 16.5), are packed into each of three stainless steel columns with an inner diameter of 27 cm and a height of 57 cm, at 100 to 105 ° C. for 2.5 hours, Steam distillation was performed to obtain 54 kg of a distillate (Reference product 1, pH 3.28). Next, 30 kg of soft water of 90 ° C. was added to each column, held at 90-95 ° C. for 30 minutes, and then left for 1 hour to extract the distillation residue and filtered to obtain 81 kg of extract (B × 8.48 °). Got. An extract of 13.5 kg was added to 9 kg of the above distillate, and the pH was adjusted to 5.01 with sodium bicarbonate. Using RO membrane concentrator NTR-759HG S2F (manufactured by Nitto Denko), operating pressure of 4 MPa for about 3 hours. After the treatment, centrifugation (20 ° C., 800 × G, 5 minutes) is performed, Bx is adjusted to 20 °, 200-mesh filtration is performed, and 5.7 kg of concentrated liquid (present product 1, B × 20 °, anti-distillate) Concentration magnification: 1.58) was obtained.

実施例2
実施例1で得られた留出液9kgに抽出液6.75kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液2.86kg(本発明品2、Bx20°、対留出液濃縮倍率:3.15)を得た。
Example 2
6.75 kg of the extract was added to 9 kg of the distillate obtained in Example 1, and the pH was adjusted to 5.01 with sodium bicarbonate. Then, RO membrane concentration was performed, and soft water was added to adjust to Bx20 ° to obtain a concentrate. 2.86 kg (Product 2 of the present invention, Bx20 °, distillate concentration rate: 3.15) was obtained.

実施例3
実施例1で得られた留出液9kgに抽出液4.5kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液1.9kg(本発明品3、Bx20°、対留出液濃縮倍率:4.74)を得た。
Example 3
After adding 4.5 kg of the extract to 9 kg of the distillate obtained in Example 1 and adjusting the pH to 5.01 with sodium bicarbonate, RO membrane concentration was performed, and soft water was added to adjust the Bx to 20 ° to obtain a concentrate. 1.9 kg (Product 3 of the present invention, Bx20 °, concentration of distillate solution: 4.74) was obtained.

実施例4
実施例1で得られた留出液9kgに抽出液3.38kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液1.43kg(本発明品4、Bx20°、対留出液濃縮倍率:6.29)を得た。
Example 4
After adding 3.38 kg of extract to 9 kg of the distillate obtained in Example 1 and adjusting the pH to 5.01 with sodium bicarbonate, RO membrane concentration was performed, and soft water was added to adjust to Bx20 ° to obtain a concentrate. 1.43 kg (Product 4 of the present invention, Bx20 °, concentration ratio of distillate was 6.29) was obtained.

実施例5
実施例1と同じ、焙煎したブラジルサントス#2(L値16.5)10kgを用意し、新たに実施例1と同じカラムに充填し、90℃の軟水30kgを加え、90〜95℃で30分間保持した後、1時間放置し、抽出を行い、濾過することにより抽出液27.5kg(Bx8.52°)を得た。上記の抽出液13.5kgに実施例1の留出液9kgを加え、重曹にてpH5.01としたものをRO膜濃縮機NTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理後、遠沈処理(20℃、800×G、5分間)を行い、Bx20°に調整し、200メッシュ濾過を行い、濃縮液5.96kg(本発明品5、Bx20°、対留出液濃縮倍率:1.51)を得た。
Example 5
Prepare 10 kg of roasted Brazil Santos # 2 (L value 16.5), which is the same as in Example 1, and newly fill the same column as in Example 1, add 30 kg of soft water at 90 ° C, and at 90-95 ° C. After maintaining for 30 minutes, the mixture was allowed to stand for 1 hour, extracted, and filtered to obtain 27.5 kg of extract (Bx8.52 °). 9 kg of the distillate of Example 1 was added to 13.5 kg of the above extract and the pH was adjusted to 5.01 with sodium bicarbonate using an RO membrane concentrator NTR-759HG S2F (manufactured by Nitto Denko Corporation) at an operating pressure of 4 MPa. After the treatment for about 3 hours, a centrifuge treatment (20 ° C., 800 × G, 5 minutes) is performed, the pressure is adjusted to B × 20 °, 200 mesh filtration is performed, and 5.96 kg of the concentrated liquid (present product 5, B × 20 °, Concentration ratio of distillate was 1.51).

比較例1
実施例1の留出液9kg(pH3.28)に重曹を加え、pH5.01とし、RO膜濃縮機NTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理を行い、濃縮留出液3kgを得た。次に実施例1の抽出液13.5kg(Bx8.48°)をNTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理を行い、濃縮抽出液4.3kg(Bx26.6°)を得た。
濃縮留出液および濃縮抽出液を混合し、軟水を加え、Bx20°に調整し、90℃達温殺菌後、30℃以下に冷却後、200メッシュ濾過を行い、濃縮液5.7kg(比較品1、Bx20°、対留出液濃縮倍率:2.09)を得た。
(官能評価)
本発明品1〜5および比較品1は対留出液濃縮倍率に従い、希釈し、これら希釈品と参考品1を訓練された10名のパネラーにより官能評価を行った。香気強度およびコーヒー感の2項目に関して参考品1の風味を10として各パネラーが評価を行い、その平均値を示すとともに、香気強度およびコーヒー感の値を平均して総合評価とした。その結果を表1に示す。
(香気分析)
参考品1、本発明品1〜5および比較品1をガスクロマトグラフィーにより分析した。分析結果を酸、エステル、アルデヒド、アルコール、フラン、フェノール、ケトン、窒素化合物、硫黄化合物およびその他の化合物に分け、香気成分量の変化を比較した。参考品1に比べ比較品1で減少が大きかったのは、酸、フラン、窒素化合物、硫黄化合物であり、それら成分の濃縮後の存在量を、濃縮前を100とした時の数値で表した。また、ガスクロマトグラフィーの香気成分量(ppm)を合計して香気量(ppm)とした。なお、本発明品1〜5および比較品1は対留出液濃縮倍率にしたがって換算して参考品1と比較した。その結果を表1に示す。
Comparative Example 1
Sodium bicarbonate was added to 9 kg (pH 3.28) of the distillate of Example 1 to adjust the pH to 5.01, and the RO membrane concentrator NTR-759HG S2F (manufactured by Nitto Denko Corporation) was used for about 3 hours of treatment at an operating pressure of 4 MPa. And 3 kg of concentrated distillate was obtained. Next, 13.5 kg (Bx8.48 °) of the extract of Example 1 was treated with NTR-759HG S2F (manufactured by Nitto Denko Corporation) at an operating pressure of 4 MPa for about 3 hours, and 4.3 kg of concentrated extract ( Bx26.6 °) was obtained.
Concentrated distillate and concentrated extract are mixed, soft water is added, adjusted to Bx20 °, sterilized at 90 ° C, cooled to below 30 ° C, filtered through 200 mesh, and concentrated solution 5.7kg (comparative product) 1, Bx20 °, distillate concentration rate: 2.09).
(sensory evaluation)
The inventive products 1 to 5 and the comparative product 1 were diluted according to the concentration ratio of the distillate and the sensory evaluation was performed by 10 panelists who were trained on the diluted product and the reference product 1. Each panelist evaluated the flavor of the reference product 1 as 10 with respect to two items of fragrance intensity and coffee feeling, showed the average value, and averaged the values of fragrance intensity and coffee feeling to make a comprehensive evaluation. The results are shown in Table 1.
(Aroma analysis)
Reference product 1, invention products 1 to 5 and comparative product 1 were analyzed by gas chromatography. The analysis results were divided into acids, esters, aldehydes, alcohols, furans, phenols, ketones, nitrogen compounds, sulfur compounds and other compounds, and changes in the amount of aroma components were compared. It was acid, furan, nitrogen compound, sulfur compound that the decrease was large in comparison product 1 compared to reference product 1, and the abundance after concentration of these components was expressed as a numerical value when 100 before concentration. . Moreover, the amount of fragrance components (ppm) of gas chromatography was added to obtain the amount of fragrance (ppm). In addition, this invention products 1-5 and the comparative product 1 were converted according to the distillate concentration ratio, and compared with the reference product 1. The results are shown in Table 1.

Figure 0005455331
Figure 0005455331

表1に示すように、本発明品1〜5はいずれも比較品1に比べ、香気強度、香気バランスが高く、総合評価も高かった。特に本発明品1、2および5は濃縮前の参考品1の香気バランスが保持されており、非常に良好であった。また、香気量(ppm)は本発明品1〜5のいずれの場合も比較品1に比べ高い数値であった。比較品1では酸、フラン、窒素化合物、硫黄化合物の存在量は参考品1を100とする値が、77、65、74、30であったが、本発明品1〜5のいずれの場合も比較品1に比べ高い数値であった。これらの成分はコーヒーの重要な香気成分であり、これら成分の数値が高いことは香気バランスの改善を支持する結果であった。特に、硫黄化合物は微量でもコーヒー香気に大きな影響を与える成分であるが、本発明品1〜5の数値は85〜105と非常に高く、比較品1の30に比べ、香気の回収に関し格段の改善効果が見られた。   As shown in Table 1, the inventive products 1 to 5 all had higher fragrance strength and fragrance balance and higher overall evaluation than Comparative Product 1. In particular, the inventive products 1, 2 and 5 were very good because the aroma balance of the reference product 1 before concentration was maintained. Further, the amount of fragrance (ppm) was higher than that of the comparative product 1 in any of the inventive products 1 to 5. In Comparative Product 1, the abundance of acid, furan, nitrogen compound, and sulfur compound was 77, 65, 74, 30 with reference product 1 being 100, but in any case of Invention Products 1-5 The value was higher than that of Comparative Product 1. These components are important aroma components of coffee, and the high value of these components is a result supporting improvement of the aroma balance. In particular, the sulfur compound is a component that greatly affects the coffee aroma even in a small amount, but the numerical values of the products 1 to 5 of the present invention are very high as 85 to 105, which is much higher than that of the comparative product 1 in terms of aroma recovery. Improvement effect was seen.

実施例6
市販の煎茶5kgを内径27cm、高さ57cmの三連のステンレス製カラムのそれぞれに充填し、100〜105℃で2〜3時間、水蒸気蒸留を行い、留出液30kg(参考品2、pH4.56)を得た。次にそれぞれのカラムに50℃軟水15kgを加え、50〜55℃で30分間の抽出を行い、濾過することにより抽出液36kg(Bx7.48°)を得た。上記の留出液7.5kgに抽出液9kgを加え、重曹にてpH5.01としたものをRO膜濃縮機NTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理後、遠沈処理(20℃、800×G、5分間)を行い、Bx20°に調整し、200メッシュ濾過を行い、濃縮液3.35kg(本発明品6、Bx20°、対留出液濃縮倍率:2.24)を得た。
Example 6
5 kg of commercially available sencha was packed in each of three stainless steel columns having an inner diameter of 27 cm and a height of 57 cm, and subjected to steam distillation at 100 to 105 ° C. for 2 to 3 hours, and 30 kg of distillate (reference product 2, pH 4. 56) was obtained. Next, 15 kg of 50 ° C. soft water was added to each column, extraction was performed at 50 to 55 ° C. for 30 minutes, and filtration was performed to obtain 36 kg (B × 7.48 °) of an extract. 9 kg of the extract was added to 7.5 kg of the above distillate, and the pH was adjusted to 5.01 with sodium bicarbonate using an RO membrane concentrator NTR-759HG S2F (manufactured by Nitto Denko) for about 3 hours at an operating pressure of 4 MPa. After the treatment, centrifuge treatment (20 ° C, 800 × G, 5 minutes) is performed, Bx is adjusted to 20 °, 200 mesh filtration is performed, and 3.35 kg of concentrated solution (Product 6 of the present invention, Bx20 °, anti-distillate) Concentration magnification: 2.24) was obtained.

実施例7
実施例6で得られた留出液4.5kgに抽出液6.75kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液2.51kg(本発明品7、Bx20°、対留出液濃縮倍率:1.79)を得た。
Example 7
By adding 6.75 kg of the extract to 4.5 kg of the distillate obtained in Example 6 and adjusting the pH to 5.01 with sodium bicarbonate, RO membrane concentration is performed, and soft water is added to adjust to Bx20 °. 2.51 kg of concentrated liquid (Invention product 7, Bx20 °, concentration ratio of distillate liquid: 1.79) was obtained.

実施例8
実施例6で得られた留出液4.5kgに抽出液4.5kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液1.67kg(本発明品8、Bx20°、対留出液濃縮倍率:2.69)を得た。
Example 8
By adding 4.5 kg of the extract to 4.5 kg of the distillate obtained in Example 6 and adjusting to pH 5.01 with sodium bicarbonate, RO membrane concentration is performed, and soft water is added to adjust to Bx20 °. 1.67 kg of concentrated liquid (Product 8 of the present invention, Bx20 °, concentration ratio of distillate liquid: 2.69) was obtained.

実施例9
実施例6で得られた留出液4.5kgに抽出液3.38kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液1.25kg(本発明品8、Bx20°、対留出液濃縮倍率:3.6)を得た。
Example 9
By adding 3.38 kg of the extract to 4.5 kg of the distillate obtained in Example 6 and adjusting to pH 5.01 with sodium bicarbonate, RO membrane concentration is performed, and soft water is added to adjust to Bx20 °. Concentrated liquid 1.25 kg (Product 8 of the present invention, B × 20 °, concentration ratio of distillate liquid: 3.6) was obtained.

比較例2
実施例6で得られた留出液7.5kgに重曹を加え、pH5.01とし、RO膜濃縮機NTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理を行い、濃縮留出液1kgを得た。次に実施例6の抽出液9kg(Bx7.48°)をNTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理を行い、濃縮抽出液2.5kg(Bx26.8°)を得た。
Comparative Example 2
Sodium bicarbonate was added to 7.5 kg of the distillate obtained in Example 6 to adjust the pH to 5.01, and the RO membrane concentrator NTR-759HG S2F (manufactured by Nitto Denko Corporation) was used for about 3 hours of treatment at an operating pressure of 4 MPa. 1 kg of concentrated distillate was obtained. Next, 9 kg (Bx7.48 °) of the extract of Example 6 was treated with NTR-759HG S2F (manufactured by Nitto Denko Corporation) at an operating pressure of 4 MPa for about 3 hours, and 2.5 kg (Bx26. 8 °).

濃縮留出液および濃縮抽出液を混合し、軟水を加え、Bx20°に調整後、90℃達温殺菌後、30℃以下に冷却し、200メッシュ濾過を行い、濃縮液3.4kg(比較品2、Bx20°、対留出液濃縮倍率:3.0)を得た。
(官能評価)
本発明品6〜9および比較品2は対留出液濃縮倍率に従い、希釈し、これら希釈品と参考品2を訓練された10名のパネラーにより官能評価を行った。その結果を表2に示す。
Concentrated distillate and concentrated extract are mixed, soft water is added, adjusted to Bx20 °, sterilized at 90 ° C, cooled to 30 ° C or lower, filtered through 200 mesh, and 3.4 kg of concentrated solution (comparative product) 2, Bx20 °, distillate concentration rate: 3.0).
(sensory evaluation)
The inventive products 6 to 9 and the comparative product 2 were diluted according to the concentration ratio of the distillate, and sensory evaluation of these diluted products and the reference product 2 was performed by 10 trained panelists. The results are shown in Table 2.

Figure 0005455331
Figure 0005455331

表2に示すように、本発明品6〜9の香気香味は、比較品2と比べ、香気強度、香気バランスが高く、総合評価も高いとともに、良好な煎茶感を有していた。特に本発明品5および6は濃縮前の参考品2と同程度の香気バランスが保持されており、非常に良好であった。   As shown in Table 2, the fragrance flavors of the inventive products 6 to 9 had higher fragrance strength and fragrance balance, higher overall evaluation, and good sencha feeling compared to Comparative Product 2. In particular, the products 5 and 6 of the present invention were very good because the same fragrance balance as that of the reference product 2 before concentration was maintained.

実施例10
市販の鰹節研磨粉(鰹節の整形時に、まわりをグラインダーで削ることにより、生成する粉、G粉とも呼ばれる)5kgを内径27cm、高さ57cmのステンレス製カラムのそれぞれに充填し、100〜105℃で2〜3時間、水蒸気蒸留を行い、留出液30kg(参考品3、pH4.65)を得た。次にそれぞれのカラムに95℃軟水50kgを加え、90〜95℃で30分間の抽出を行い、濾過することにより抽出液123kg(Bx2.0°)を得た。上記の留出液5kgに重曹を加え、pH 5.01としたものに、抽出液20.5kgを添加混合し、RO膜濃縮機NTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理後、遠沈処理(20℃、800×G、5分間)を行い、Bx20°に調整し、200メッシュ濾過を行い、濃縮液2.0kg(本発明品10、Bx20°)を得た。
Example 10
5 kg of commercially available bonito polishing powder (which is also called G powder, which is generated by grinding around with a grinder when shaping the bonito) is packed into each of a stainless steel column having an inner diameter of 27 cm and a height of 57 cm. Then, steam distillation was performed for 2 to 3 hours to obtain 30 kg of a distillate (Reference product 3, pH 4.65). Next, 50 kg of 95 ° C. soft water was added to each column, extraction was performed at 90 to 95 ° C. for 30 minutes, and filtration was performed to obtain 123 kg (B × 2.0 °) of an extract. Sodium bicarbonate was added to 5 kg of the above distillate to adjust the pH to 5.01, 20.5 kg of the extract was added and mixed, and RO membrane concentrator NTR-759HG S2F (manufactured by Nitto Denko Corporation) was used, and the operating pressure was 4 MPa. After about 3 hours of treatment, centrifuge treatment (20 ° C., 800 × G, 5 minutes) is performed, Bx is adjusted to 20 °, 200 mesh filtration is performed, and 2.0 kg of concentrated solution (Product 10 of the present invention, B × 20 °). )

実施例11
実施例10で得られた留出液5kgに抽出液10.25kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液1.01kg(本発明品11、Bx20°)を得た。
Example 11
After adding 10.25 kg of the extract to 5 kg of the distillate obtained in Example 10 and adjusting the pH to 5.01 with sodium bicarbonate, RO membrane concentration was performed, and soft water was added to adjust to Bx20 ° to obtain a concentrate. 1.01 kg (Invention product 11, Bx20 °) was obtained.

実施例12
実施例10で得られた留出液5kgに抽出液6.83kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液0.68kg(本発明品12、Bx20°)を得た。
Example 12
After adding 6.83 kg of the extract to 5 kg of the distillate obtained in Example 10 and adjusting the pH to 5.01 with sodium bicarbonate, RO membrane concentration was performed, and soft water was added to adjust to Bx20 ° to obtain a concentrate. 0.68 kg (Invention product 12, Bx20 °) was obtained.

実施例13
実施例10で得られた留出液10kgに抽出液5.13kgを加え、重曹にてpH5.01とした後、RO膜濃縮を行い、軟水を加えてBx20°に調整することにより、濃縮液0.52kg(本発明品12、Bx20°)を得た。
Example 13
After adding 5.13 kg of the extract to 10 kg of the distillate obtained in Example 10 and adjusting the pH to 5.01 with sodium bicarbonate, RO membrane concentration is performed, and soft water is added to adjust the Bx to 20 ° to obtain a concentrate. 0.52 kg (Invention product 12, Bx20 °) was obtained.

比較例3
実施例10で得られた留出液5kgに重曹を加え、pH5.01とし、RO膜濃縮機NTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理を行い、濃縮留出液1.3kgを得た。次に実施例10の抽出液10.25kg(Bx7.48°)をNTR−759HG S2F(日東電工社製)を用い、操作圧4MPaで約3時間の処理を行い、濃縮抽出液3.14kg(Bx24.3°)を得た。
Comparative Example 3
Sodium bicarbonate was added to 5 kg of the distillate obtained in Example 10 to adjust the pH to 5.01, and the RO membrane concentrator NTR-759HG S2F (manufactured by Nitto Denko) was used, and the treatment was performed at an operating pressure of 4 MPa for about 3 hours. 1.3 kg of concentrated distillate was obtained. Next, the extract of Example 10 (10.25 kg (Bx7.48 °)) was treated with NTR-759HG S2F (manufactured by Nitto Denko Corporation) at an operating pressure of 4 MPa for about 3 hours, and 3.14 kg of concentrated extract ( Bx24.3 °) was obtained.

濃縮留出液および濃縮抽出液を混合し、軟水を加え、Bx20°に調整後、90℃達温殺菌後、30℃以下に冷却し、200メッシュ濾過を行い、濃縮液3.8kg(比較品2、Bx20°)を得た。
(官能評価)
本発明品10〜13および比較品3は対留出液濃縮倍率に従い、希釈し、これら希釈品と参考品3を訓練された10名のパネラーにより官能評価を行った。その結果を表3に示す。
Concentrated distillate and concentrated extract are mixed, soft water is added, adjusted to Bx20 °, sterilized at 90 ° C, cooled to 30 ° C or lower, filtered through 200 mesh, and concentrated solution 3.8kg (comparative product) 2, Bx20 °).
(sensory evaluation)
The inventive products 10 to 13 and the comparative product 3 were diluted according to the concentration ratio of the distillate, and sensory evaluation was performed by 10 panelists who were trained on the diluted product and the reference product 3. The results are shown in Table 3.

Figure 0005455331
Figure 0005455331

表3に示すように、本発明品10〜13の香気香味は、比較品3と比べ、香気強度、香気バランスが高く、総合評価も高いとともに、鰹節の有する上品な風味を有していた。特に本発明品10および11は濃縮前の参考品3と同程度の香気バランスが保持されており、非常に良好であった。   As shown in Table 3, the fragrance flavors of the inventive products 10 to 13 were higher in fragrance strength and fragrance balance, higher in overall evaluation than the comparative product 3, and had an elegant flavor possessed by bonito. In particular, the products 10 and 11 of the present invention were very good because the same fragrance balance as that of the reference product 3 before concentration was maintained.

Claims (2)

下記工程:
(A)焙煎コーヒー豆を水蒸気蒸留して香気を含む留出液を得る工程、
(B)工程(A)で発生した水蒸気蒸留残渣に水を加えて抽出して抽出液を得る工程、
(C)(A)の留出液に(B)の抽出液の一部または全量を混合後、該混合物をpH5.01に調整し、逆浸透膜を用いて濃縮することを特徴とするコーヒー香気濃縮物の製造方法。
The following process:
(A) A step of steam-distilling roasted coffee beans to obtain a distillate containing aroma,
(B) A step of adding water to the steam distillation residue generated in step (A) and extracting it to obtain an extract,
(C) A coffee characterized by mixing part or all of the extract of (B) with the distillate of (A) , adjusting the mixture to pH 5.01, and concentrating using a reverse osmosis membrane. A method for producing an aroma concentrate.
コーヒー香気濃縮物中の硫黄化合物の存在量が濃縮前の85〜107%である請求項1に記載のコーヒー香気濃縮物の製造方法 The method for producing a coffee aroma concentrate according to claim 1, wherein the abundance of the sulfur compound in the coffee aroma concentrate is 85 to 107% before the concentration .
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