JPH01112965A - Extraction of flavoring component of cacao - Google Patents
Extraction of flavoring component of cacaoInfo
- Publication number
- JPH01112965A JPH01112965A JP62272048A JP27204887A JPH01112965A JP H01112965 A JPH01112965 A JP H01112965A JP 62272048 A JP62272048 A JP 62272048A JP 27204887 A JP27204887 A JP 27204887A JP H01112965 A JPH01112965 A JP H01112965A
- Authority
- JP
- Japan
- Prior art keywords
- cacao
- components
- carbon dioxide
- flavor
- dioxide gas
- Prior art date
- 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.)
- Pending
Links
- 244000299461 Theobroma cacao Species 0.000 title claims abstract description 64
- 235000005764 Theobroma cacao ssp. cacao Nutrition 0.000 title claims abstract description 43
- 235000005767 Theobroma cacao ssp. sphaerocarpum Nutrition 0.000 title claims abstract description 43
- 235000001046 cacaotero Nutrition 0.000 title claims abstract description 43
- 238000000605 extraction Methods 0.000 title claims description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 69
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000796 flavoring agent Substances 0.000 claims abstract description 46
- 235000019634 flavors Nutrition 0.000 claims abstract description 43
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 34
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 34
- 235000019441 ethanol Nutrition 0.000 claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 3
- 235000019219 chocolate Nutrition 0.000 abstract description 11
- 230000002542 deteriorative effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 29
- 239000000284 extract Substances 0.000 description 14
- 235000009470 Theobroma cacao Nutrition 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 244000046052 Phaseolus vulgaris Species 0.000 description 3
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 235000013355 food flavoring agent Nutrition 0.000 description 3
- 239000010903 husk Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 2
- 239000008370 chocolate flavor Substances 0.000 description 2
- 229940110456 cocoa butter Drugs 0.000 description 2
- 235000019868 cocoa butter Nutrition 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- YAPQBXQYLJRXSA-UHFFFAOYSA-N theobromine Chemical compound CN1C(=O)NC(=O)C2=C1N=CN2C YAPQBXQYLJRXSA-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- -1 and in such cases Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 229960004559 theobromine Drugs 0.000 description 1
Landscapes
- Seasonings (AREA)
- Fats And Perfumes (AREA)
- Confectionery (AREA)
Abstract
Description
【発明の詳細な説明】
のＩ
飲食品にチョコレートの香味を付与するには、カカオマ
ス、ココア、チョコレートなどのカカオ製品を加えるこ
とにより行われている。しかし、チョコレートの香味を
更に強くするには、香料を用いなければならない、この
ような場合、従来合成の香料を中心として調合した香料
が主に用いられている。[Detailed Description of the Invention] Part I: Adding a chocolate flavor to foods and beverages is accomplished by adding cacao products such as cacao mass, cocoa, and chocolate. However, in order to enhance the flavor of chocolate, it is necessary to use a flavoring agent, and in such cases, flavorants prepared mainly from conventionally synthesized flavoring agents are mainly used.
この発明は、カカオ成分から香味成分を抽出する方法に
間するものであり、カカオ成分から天然の香味成分を分
離、抽出し、それにより飲食品にチョコレートの望まし
い香味を付与するとき利用される。The present invention relates to a method for extracting flavor components from cacao components, and is used when separating and extracting natural flavor components from cacao components, thereby imparting a desirable chocolate flavor to foods and drinks.
従」ＬＱ」Ｌ庖
カカオ成分から香味成分を分離・抽出するには、水蒸気
蒸留や溶媒抽出が行われている。Steam distillation and solvent extraction are used to separate and extract flavor components from cacao components.
また、溶媒抽出に用いる溶媒も、例えば水（熱Ｉり、ア
ルコールなどの極性の大きなものを用いる場合と炭化水
素、エーテル、アセトンなどの極性の小さいものを用い
る場合とがある。Further, as for the solvent used for solvent extraction, for example, there are cases in which a highly polar solvent such as water (heated) or alcohol is used, and a case in which a less polar solvent such as a hydrocarbon, ether, or acetone is used.
、■ Ｓ ゛ ９ 。１
チョコレートなどのカカオ成分の香味成分は、生のカカ
オ豆を発酵する際、糖類、タンパク質、脂肪、ポリフェ
ノール類又はこれらの分解生成物などが反応し合って生
じ、更に焙煎により複雑な反応が起こり、形成されるの
で、非常に多くの成分が関与しており、それぞれの成分
のバランスが重要である。,■S゛9. 1 The flavor components of cacao ingredients such as chocolate are produced when raw cacao beans are fermented, and sugars, proteins, fats, polyphenols, or their decomposition products react with each other, and further complex reactions occur during roasting. As it occurs and is formed, a large number of components are involved, and the balance of each component is important.
しかし、水蒸気蒸留や溶剤による抽出では、香味成分の
一部しか抽出できなかった。このような抽出物を用いて
飲食品にカカオの香味を付与しようとすれば、天然の望
ましい香味に近づけるため合成の香料で補わなければな
らなかった。However, only a portion of the flavor components could be extracted by steam distillation or solvent extraction. If such extracts were to be used to impart cacao flavor to foods and drinks, synthetic flavoring agents had to be used to approximate the desired natural flavor.
また、抽出のとき又は抽出液を濃縮するとき熱が加わる
ため揮発性の大きな成分の揮散や熱に弱い成分の変質な
ども見られた。Furthermore, since heat is applied during extraction or when concentrating the extract, volatilization of highly volatile components and deterioration of heat-sensitive components were observed.
一方、最近超臨界状態の炭酸ガスで抽出することが行わ
れるようになったが、カカオニブ、カカオマスなどのカ
カオ成分を超臨界状態の炭酸ガスで抽出すると、ココア
バターが同時に抽出されるため、更に溶媒などで抽出し
なければならず、問題の解決にならなかった。。On the other hand, extraction with supercritical carbon dioxide gas has recently started to be carried out, but when cacao components such as cacao nibs and cacao mass are extracted with supercritical carbon dioxide gas, cocoa butter is extracted at the same time. The problem had to be extracted using a solvent, etc., which did not solve the problem. .
この発明の発明者らは、カカオ成分からその望ましい香
味成分を抽出し、天然のカカオの香味をそのまま飲食品
に付与する方法を研究し、エチルアルコール又はエチル
アルコール水溶液を添加した超臨界状態の炭酸ガスで抽
出すると好ましい香味の成分が抽出されることを見いだ
し、この発明を完成させた。The inventors of this invention have researched a method of extracting the desired flavor components from cacao components and imparting the natural cacao flavor to food and drink products as they are, and have developed a supercritical state of carbonic acid with the addition of ethyl alcohol or an aqueous solution of ethyl alcohol. They discovered that a component with a desirable flavor can be extracted by extracting with gas, and completed this invention.
ｍ り
この発明では、カカオ成分を原料としてその香味成分を
抽出するに際し、２５℃、１気圧における容量に換算し
たとき１１に相当する量の炭酸ガスに対しエチルアルコ
ール又は３０％以上のエチルアルコール水溶液が０．１
〜３１の割合で加えられている超臨界状態の炭酸ガスを
用いて香味成分を抽出している。In this invention, when extracting the flavor components from cacao components as raw materials, ethyl alcohol or an aqueous solution of ethyl alcohol of 30% or more is added to the amount of carbon dioxide gas equivalent to 11 when converted to the volume at 25° C. and 1 atm. is 0.1
Flavor components are extracted using supercritical carbon dioxide gas added at a ratio of ~31%.
この発明のカカオ成分とは、カカオビーンズ又はその処
理物を指し、例えばカカオビーンズ、カカオニブ、カカ
オマス、カカオハスク、カカオジャーム、ココアケーキ
、ココアパウダー、ココアバター等が利用できる。The cacao component of this invention refers to cacao beans or processed products thereof, and examples of cacao beans, cacao nibs, cacao mass, cacao husk, cacao germ, cocoa cake, cocoa powder, cocoa butter, etc. can be used.
まず、カカオ成分は、香味成分を抽出するため超臨界状
態の炭酸ガスと接触させ、抽出する。すなわち、カカオ
成分を円筒状のカラムなどの抽出容器に詰め、その一端
から超臨界状態の炭酸ガスを注入し、多端から流出する
ようにする。First, cacao components are brought into contact with carbon dioxide gas in a supercritical state to extract flavor components. That is, cacao components are packed into an extraction container such as a cylindrical column, and supercritical carbon dioxide gas is injected from one end of the container and flows out from the other end.
これにより、抽出容器の中でカカオ成分と超臨界状態の
炭酸ガスが接触し、香味成分が超臨界状態の炭酸ガスに
より抽出される。As a result, the cacao component and the carbon dioxide gas in the supercritical state come into contact with each other in the extraction container, and the flavor components are extracted by the carbon dioxide gas in the supercritical state.
なお、抽出に用いる超臨界状態の炭酸ガスは、あらかじ
めエチルアルコール又はエチルアルコール水溶液を添加
しておく。Note that ethyl alcohol or an aqueous ethyl alcohol solution is added to the supercritical carbon dioxide gas used for extraction in advance.
超臨界状態の炭酸ガスにエチルアルコール又はエチルア
ルコール水溶液を添加するには、一定の流速で流れる超
臨界状態の炭酸ガスの流れに所定量のエチルアルコール
又はエチルアルコール水溶液を注入していくようにする
。To add ethyl alcohol or ethyl alcohol aqueous solution to supercritical carbon dioxide gas, inject a predetermined amount of ethyl alcohol or ethyl alcohol aqueous solution into the flow of supercritical carbon dioxide gas flowing at a constant flow rate. .
なお、エチルアルコール又はエチルアルコール水溶液を
加える量が少ない場合、脂肪や高級脂肪酸などが多く抽
出され、放置しておくと濁りや沈澱が生じる原因となる
。また、エチルアルコールやエチルアルコール水溶液の
量が多い場合、エステルなどの香りに関係する成分など
の抽出量が少なくなり、好ましい香味のものが得られな
いことがある。更に、炭酸ガス中のエチルアルコールの
量が多すぎると、抽出成分に多量のエチルアルコールが
混入し、香味成分が希釈されるおそれもあしたがって、
カカオ成分の望ましい香味成分を抽出するには、２５℃
、１気圧における容量に換算して１１に相当する量の炭
酸ガスに対しエチルアルコール又は３０％以上のエチル
アルコール水溶液を０．１〜３ｍｌの割合で加えた超臨
界状態の炭酸ガスを用いて抽出するようにする。Note that if the amount of ethyl alcohol or ethyl alcohol aqueous solution added is small, a large amount of fat, higher fatty acids, etc. will be extracted, which will cause turbidity and precipitation if left to stand. Furthermore, if the amount of ethyl alcohol or aqueous ethyl alcohol solution is large, the amount of components related to aroma such as esters extracted may be reduced, and a desired flavor may not be obtained. Furthermore, if the amount of ethyl alcohol in the carbon dioxide gas is too large, there is a risk that a large amount of ethyl alcohol will be mixed into the extracted components and the flavor components will be diluted.
To extract the desired flavor components of cacao, 25℃
Extraction using supercritical carbon dioxide gas, which is obtained by adding 0.1 to 3 ml of ethyl alcohol or an aqueous solution of 30% or more ethyl alcohol to an amount of carbon dioxide gas equivalent to 11 in terms of volume at 1 atm. I'll do what I do.
なお、香味成分を抽出した超臨界状態の炭酸ガスは、ト
ラップなどに導き、そこで圧力を下げ、炭酸ガスと抽出
成分とに分離する。このとき、数回にわたって段階的に
圧力を下げ、それぞれの圧力のとき分離する抽出成分を
分取することにより、香味の異なる複数の抽出成分を得
ることもできる。Note that the supercritical carbon dioxide gas from which flavor components have been extracted is led to a trap or the like, where the pressure is lowered and separated into carbon dioxide gas and extracted components. At this time, it is also possible to obtain a plurality of extract components with different flavors by lowering the pressure stepwise several times and collecting the extract components separated at each pressure.
なお、このようにして分離した香味成分を抽出原料とし
て、シリカゲルなどに吸着させるなどして更に超臨界状
態の炭酸ガスにより抽出し、香味成分を分離・濃縮する
ことも可能である。It is also possible to separate and concentrate the flavor components by using the flavor components separated in this way as extraction raw materials, adsorbing them onto silica gel, etc., and then extracting them with carbon dioxide gas in a supercritical state.
１１立１１
本発明では、超臨界状態の炭酸ガスで抽出するので、圧
力を下げるだけで抽出媒体である炭酸ガスが揮散して抽
出成分が得られ、操作中熱やその他の溶媒を用いる必要
がない。したがって、抽出成分が熱で変質する心配がな
く、しかも酸素に比べ活性の小さい炭酸ガスを用いるた
め操作中空気中の酸素により酸化される心配もない。そ
の上、エチルアルコール又はエチルアルコール水溶液を
添加することにより、超臨界状態の炭酸ガスの極性をカ
カオ成分から香味成分をそのまま抽出するのによい状態
として抽出を行うため、天然のカカオ成分の香味を変質
することなくそのまま抽出することができる。11 11 In the present invention, since extraction is performed using carbon dioxide gas in a supercritical state, the carbon dioxide gas, which is the extraction medium, can be volatilized and the extracted components can be obtained by simply lowering the pressure, and there is no need to use heat or other solvents during the operation. do not have. Therefore, there is no fear that the extracted components will be altered by heat, and since carbon dioxide gas, which is less active than oxygen, is used, there is no fear that the extracted components will be oxidized by oxygen in the air during operation. Furthermore, by adding ethyl alcohol or an aqueous ethyl alcohol solution, the polarity of carbon dioxide gas in a supercritical state is adjusted to a state suitable for extracting the flavor components from the cocoa components as they are. It can be extracted as is without deterioration.
すなわち、本発明により抽出した香味成分は、カカオ成
分の香味を損なうことなくそのままで得られ、しかも濃
縮された香味の優れたものが得られる。That is, the flavor components extracted according to the present invention can be obtained as they are without impairing the flavor of the cacao component, and moreover, can be obtained in a concentrated form with excellent flavor.
大」１例 次に、本発明を実施例により説明する。Large” 1 case Next, the present invention will be explained by examples.
実施例１
０−ストしたカカオニブ９７．９ｇ を３０１１ｗ×
２５０ａｕａの抽出容器に充填した０次いで、抽出塔の
下端から超臨界状態（１７０にｇ／ ｃｍ２．３８℃）
の炭酸ガスをｌ気圧に換算して ２．２１ ／ｗｉｎ、
の割合で流し、抽出した。このとき９０％エチルアルコ
ール水溶液を０．Ｅ３ｓｌ／ｗｉｎ、の割合で加えた。Example 1 97.9g of 0-starved cacao nibs was added to 3011w×
A 250aua extraction vessel was filled with 0.000g, then from the bottom of the extraction column to a supercritical state (170g/cm2.38°C).
Converting carbon dioxide to 1 atm: 2.21 /win,
It was extracted at a ratio of At this time, add 0.0% 90% ethyl alcohol aqueous solution. It was added at a ratio of E3sl/win.
抽出塔の上端から流出した香味成分を抽出した炭酸ガス
をトラップに導き、そこで圧力を下げ、気体となった炭
酸ガスと液状の抽出成分とを分離した。分離した炭酸ガ
スは加圧ポンプにより加圧し、再利用した。５時閏の抽
出操作で５４．４ｇ のカカオ香味成分を得た。The carbon dioxide gas that extracted the flavor components flowing out from the upper end of the extraction tower was led to a trap, where the pressure was lowered and the gaseous carbon dioxide gas and the liquid extracted components were separated. The separated carbon dioxide gas was pressurized with a pressure pump and reused. 54.4 g of cacao flavor components were obtained by the 5-hour extraction operation.
このカカオ香味成分は、カカオの好ましい香りがした。This cocoa flavor component had a pleasant aroma of cocoa.
実施例２
あらかじめ１６０ Ｋｇ／ ｃｓ＋２．３８℃の超臨界
状態の炭酸ガス（１気圧に換算して２．８１ ／ｗｉｎ
、）及びエチルアルコール（０，４ｍｌ／ｗｉｎ、）を
流しておいたシリカゲル（メルク社製５１６０、粒度２
５〜４０μｍ）を充填した２ ０ ｅｕ＋Ｘ ３０ ｃ
ｍＱカラムの一端に実施例１で得たカカオ成分抽出物の
５ｇを供給し、更に前と同じ組成のエチルアルコールを
加えた超臨界状態の炭酸ガスを流し、カラムの他端で流
出する成分を検出したところ第１図に示すように多数の
成分に分かれて流出した。Example 2 Carbon dioxide gas in a supercritical state at 160 Kg/cs + 2.38°C (2.81/win when converted to 1 atm)
, ) and ethyl alcohol (0.4 ml/win, ) were poured over silica gel (manufactured by Merck & Co., Ltd. 5160, particle size 2).
20 eu+X30 c filled with 5~40μm)
5 g of the cacao component extract obtained in Example 1 was supplied to one end of the mQ column, and supercritical carbon dioxide gas with ethyl alcohol of the same composition as before was flowed, and the components flowing out at the other end of the column were When detected, it was separated into many components and leaked out, as shown in Figure 1.
この ２．５分から１４分までの間に流出した成分を分
取してカカオ成分の香味成分を得た。この香味成分は、
実施例１に比べ香味が濃縮され、更に良好な香りがした
。The components flowing out between 2.5 minutes and 14 minutes were fractionated to obtain the flavor component of the cacao component. This flavor ingredient is
The flavor was more concentrated than in Example 1, and the fragrance was even better.
実施例３
実施例１に記載のカラムと同じ大きさのカラムにカカオ
ハスク ６１．９ｇを充填し、カラムの上端から１７０
Ｋｇ／ｃＩ１１２の超臨界状態の炭酸ガス（１気圧に換
算して ３．０１ ／ｎ＋ｉｎ、）及び９０％エチルア
ルコール水溶液（０，８ｍｌ／ ｗｉｎ、）を流入し、
２時間抽出を行い、 ６１．９ ｇのカカオ成分抽出物
を得た。Example 3 A column of the same size as that described in Example 1 was packed with 61.9 g of cocoa husk, and 170 g of cacao husk was packed from the top of the column.
Supercritical carbon dioxide gas of Kg/cI 112 (3.01/n+in, converted to 1 atm) and 90% ethyl alcohol aqueous solution (0.8 ml/win) were introduced,
Extraction was performed for 2 hours to obtain 61.9 g of cocoa component extract.
このカカオ成分抽出物は、大変良好なチョコレートの香
りがした。This cacao component extract had a very good chocolate aroma.
このカカオ成分抽出物を添加して調整したチョコレート
とカカオ成分抽出物を加えずに同様に調整したチョコレ
ートと比較する官能検査を１０名のパネラ−により行っ
た結果、１０名ともカカオ成分抽出物を加えたチョコレ
ートの方が風味が優れているとした。A sensory test was conducted by 10 panelists to compare chocolate prepared with the addition of this cacao extract to chocolate prepared in the same manner without the addition of the cacao extract. The added chocolate had a better flavor.
実施例４
あらかじめ１９０にｇ／ ｃｍ２．３８℃の超臨界状態
の炭酸ガス（１気圧に換算して２．８１ ／ｍｉｎ、）
及びエチルアルコール（０，３ｍｌ／ ｗｉｎ、）を流
しておいたシリカゲル（メルク社ｉ！５ｉ６０、粒度２
５−４０μｍ）を充填した２ ０ ｍｍＸ ３０ ｃｍ
のカラムの一端に実施例３で得たカカオ成分抽出物の１
０ｇを供給し、更に前と同じ組成のエチルアルコールを
加えた超臨界状態の炭酸ガスを流し、カラムの他端で流
出する成分を検出したところ第２図に示すように多数の
成分に分かれて流出した。Example 4 Carbon dioxide in a supercritical state at 190 g/cm2.38°C (2.81/min, converted to 1 atm)
Silica gel (Merck i!5i60, particle size 2
20 mm x 30 cm filled with 5-40 μm)
1 of the cocoa component extract obtained in Example 3 was placed at one end of the column.
0g was supplied, and supercritical carbon dioxide gas containing ethyl alcohol of the same composition as before was flowed. When the components flowing out at the other end of the column were detected, they were separated into many components as shown in Figure 2. It leaked out.
この２分から１６分までの間に流出した成分を分取して
カカオ成分の香味成分を得た。この香味成分は、実施例
１に比べ香味が濃縮され、更に良好な香りがした。The components that flowed out between 2 minutes and 16 minutes were fractionated to obtain the flavor component of the cacao component. This flavor component had a more concentrated flavor than Example 1, and had a better aroma.
実施例５
実施例４で１８分間抽出した後のシリカゲルにまだ吸着
しているカカオ成分抽出物を ３７．５％エチルアルコ
ール水溶液２５０１で溶出した。この溶出したカカオ成
分抽出物は、チョコレートの香りと色をしており、 ｏ
、ｏｏａ％のカフェインと ０．５４％のテオブロミン
を有した透明な溶液であった。Example 5 The cocoa component extract still adsorbed on the silica gel after extraction for 18 minutes in Example 4 was eluted with 37.5% ethyl alcohol aqueous solution 2501. This eluted cacao component extract has the aroma and color of chocolate, and o
It was a clear solution with .00% caffeine and 0.54% theobromine.
このカカオ成分抽出物を水で１００倍に希釈し、砂糖７
部及びクエン酸 ０．０１部を加えチョコレートドリン
クとした。Dilute this cacao component extract 100 times with water and add 70% sugar.
1 part and 0.01 part of citric acid were added to prepare a chocolate drink.
このチョコレートドリンクは、大変風味が良かった。This chocolate drink had great flavor.
第１図は実施例２において抽出カラムから流出する成分
を２００から２５０ｎｍの波長の光の吸収を検出したと
きのチャート、図面の横軸は時間、縦軸は波長、高さは
吸光度である。また第２図は実施例４の流出成分のチャ
ート、横軸、縦軸、高さは第１図に同じ。
特許出願人 森永製菓株式会社
手続補正書（方式）
１、事件の表示
昭和６２年特許願第２７２０４８号
２、発明の名称
カカオ香味成分の抽出方法
１、補正をする者
事件との関係 特許出願人
（発送臼 昭和６３年 １ 月２６日）５、補正の対象
図面
６、補正の内容
第１図、第２図（トレーシングペーパーを用いて黒色で
描いた図面とした。）
、−一一一崎にFIG. 1 is a chart showing the detection of absorption of light with a wavelength of 200 to 250 nm in components flowing out of the extraction column in Example 2. The horizontal axis of the drawing is time, the vertical axis is wavelength, and the height is absorbance. Further, FIG. 2 is a chart of the outflow components of Example 4, and the horizontal axis, vertical axis, and height are the same as in FIG. 1. Patent Applicant Morinaga & Co., Ltd. Procedural Amendment (Method) 1. Indication of the case Patent Application No. 272048 of 1988 2. Name of the invention Method for extracting cacao flavor components 1. Person making the amendment Relationship with the case Patent applicant (Delivery date January 26, 1988) 5. Drawings to be amended 6. Details of amendments Figures 1 and 2 (Drawings drawn in black using tracing paper) -111 On the slope
Claims (1)
、２５℃、１気圧における容量に換算したとき１ｌに相
当する量の炭酸ガスに対しエチルアルコール又は３０％
以上のエチルアルコール水溶液が０．１〜３ｍｌの割合
で加えられている超臨界状態の炭酸ガスを用いて抽出す
ることを特徴とするカカオ香味成分の抽出方法。When extracting the flavor components from cacao components as raw materials, ethyl alcohol or 30%
A method for extracting cacao flavor components, characterized in that the extraction is carried out using supercritical carbon dioxide gas to which the above ethyl alcohol aqueous solution is added at a ratio of 0.1 to 3 ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62272048A JPH01112965A (en) | 1987-10-28 | 1987-10-28 | Extraction of flavoring component of cacao |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62272048A JPH01112965A (en) | 1987-10-28 | 1987-10-28 | Extraction of flavoring component of cacao |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01112965A true JPH01112965A (en) | 1989-05-01 |
Family
ID=17508383
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62272048A Pending JPH01112965A (en) | 1987-10-28 | 1987-10-28 | Extraction of flavoring component of cacao |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01112965A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02235998A (en) * | 1989-03-09 | 1990-09-18 | T Hasegawa Co Ltd | Manufacture of roast seed flavor |
| JPH0322956A (en) * | 1989-04-25 | 1991-01-31 | T Hasegawa Co Ltd | Production of flavor from animal or plant fatty oil |
| JPH06125710A (en) * | 1992-09-01 | 1994-05-10 | Lotte Co Ltd | Cacao husk extract capable of improving concentration and its production and concentration-improved chocolate with the same applied thereto |
| WO1995010946A1 (en) * | 1993-10-20 | 1995-04-27 | Cadbury Schweppes Plc | Process for manufacture of reduced fat and reduced calorie chocolate |
| US6090427A (en) * | 1998-09-21 | 2000-07-18 | Nestec Sa | Natural cocoa aroma/flavor compositions and methods for preparing same |
| CN107460042A (en) * | 2016-06-04 | 2017-12-12 | 潘峰 | A kind of cacao essence preparation method |
| JP6259047B1 (en) * | 2016-11-07 | 2018-01-10 | 森永製菓株式会社 | Chocolate production method |
-
1987
- 1987-10-28 JP JP62272048A patent/JPH01112965A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02235998A (en) * | 1989-03-09 | 1990-09-18 | T Hasegawa Co Ltd | Manufacture of roast seed flavor |
| JPH0322956A (en) * | 1989-04-25 | 1991-01-31 | T Hasegawa Co Ltd | Production of flavor from animal or plant fatty oil |
| JPH06125710A (en) * | 1992-09-01 | 1994-05-10 | Lotte Co Ltd | Cacao husk extract capable of improving concentration and its production and concentration-improved chocolate with the same applied thereto |
| WO1995010946A1 (en) * | 1993-10-20 | 1995-04-27 | Cadbury Schweppes Plc | Process for manufacture of reduced fat and reduced calorie chocolate |
| US6090427A (en) * | 1998-09-21 | 2000-07-18 | Nestec Sa | Natural cocoa aroma/flavor compositions and methods for preparing same |
| SG97810A1 (en) * | 1998-09-21 | 2003-08-20 | Nestle Sa | Natural cocoa aroma/flavor compositions and methods for preparing same |
| CN107460042A (en) * | 2016-06-04 | 2017-12-12 | 潘峰 | A kind of cacao essence preparation method |
| JP6259047B1 (en) * | 2016-11-07 | 2018-01-10 | 森永製菓株式会社 | Chocolate production method |
| JP2018074909A (en) * | 2016-11-07 | 2018-05-17 | 森永製菓株式会社 | Production method of chocolate |
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