JP7168992B2 - Oil extraction method by aqueous medium method using tea saponin - Google Patents
Oil extraction method by aqueous medium method using tea saponin Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
Description
本発明は、茶サポニンを使用した水媒法による油抽出方法に関し、油処理の技術分野に属する。 TECHNICAL FIELD The present invention relates to an oil extraction method by an aqueous medium method using tea saponin, and belongs to the technical field of oil treatment.
水媒法の概念は、半世紀近くにわたって開発された圧搾法と浸出法以外の油抽出技術の分析と分類に基づいている。いわゆる水媒法とは、水を主媒体とする油抽出技術であり、、水溶性の食用物質（エタノールなど）、食品グレードの酵素、超音波、マイクロ波などを添加または添加せずに、油細胞壁および/または解乳化を破壊する食用油抽出技術である。このうち、エタノールによる水抽出法は、水媒法の開発の最新段階であり、その油抽出の基本原理は、エタノールの表面張力が水の表面張力よりも小さいことであり、エタノールの添加により、油水エマルジョンシステムの安定性が失われ、清澄油の収率の向上に役立つ。しかしながら、エタノール水抽出法には、エタノールの消費量が大きく、コストが高いという欠点もある。同様に、他の水媒法には、例えば、水酵素法で使用される酵素の量が多く、超音波とマイクロ波利用などにはエネルギー消費が大きいなどの欠点がある。 The hydroprocess concept is based on the analysis and classification of oil extraction techniques other than pressing and leaching that have been developed over nearly half a century. The so-called water-based method is an oil extraction technology that uses water as the main medium, and extracts oil with or without the addition of water-soluble edible substances (such as ethanol), food-grade enzymes, ultrasonic waves, microwaves, etc. An edible oil extraction technique that disrupts cell walls and/or demulsification. Of these, the water extraction method using ethanol is the latest stage in the development of the aqueous medium method. The basic principle of oil extraction is that the surface tension of ethanol is smaller than that of water. The stability of the oil-water emulsion system is lost, which helps improve the yield of clarified oil. However, the ethanol-water extraction method also has the disadvantages of high ethanol consumption and high cost. Similarly, other aqueous methods have drawbacks, such as high amounts of enzymes used in aqueous enzymatic methods, and high energy consumption, such as using ultrasound and microwaves.
本方法の第一目的は、水媒法により油を抽出する方法を提供することであり、該方法では、
水またはエタノールを含む水溶液を媒介とし、茶サポニンを含む抽出剤を使用して油を抽出し、抽出対象の材料を粉砕した後、５０～１００℃の抽出剤に０．５～３時間浸し、ｐＨを８～１０に調整し、続いて、遠心分離により、スラグ相、水相、油相およびエマルジョンを分離し；油相とエマルジョンを集めて解乳化し、清澄油を得ることを含む。
The primary object of the method is to provide a method for extracting oil by an aqueous method, the method comprising:
Using water or an aqueous solution containing ethanol as a medium, extracting the oil using an extractant containing tea saponin, pulverizing the material to be extracted, and soaking it in the extractant at 50-100 ° C for 0.5-3 hours, Adjusting the pH to 8-10 followed by centrifugation separates the slag phase, water phase, oil phase and emulsion; collecting and demulsifying the oil phase and emulsion to obtain a clear oil.
本発明の一実施形態では、前記方法は、
抽出対象の材料を粉砕した後、７０°Ｃの抽出剤に０．５時間浸漬し、ｐＨを９に調整し、続いて、遠心分離により、スラグ相、水相、油相およびエマルジョンを分離し、
油相とエマルジョンを集めて解乳化し、清澄油を得ることを含む。
In one embodiment of the invention, the method comprises:
After pulverizing the material to be extracted, it is immersed in an extractant at 70°C for 0.5 hours, the pH is adjusted to 9, followed by centrifugation to separate the slag phase, water phase, oil phase and emulsion. ,
It involves collecting and demulsifying the oil phase and emulsion to obtain a clear oil.
本発明の一実施形態では、前記茶サポニンは材料自体に含まれ、抽出プロセス中に水相に入るか、または追加で添加される。 In one embodiment of the invention, said tea saponins are included in the material itself, enter the aqueous phase during the extraction process, or are additionally added.
本発明の一実施形態では、前記材料は、油料作物の果実または種子を含む。 In one embodiment of the invention, said material comprises the fruit or seed of an oil crop.
本発明の一実施形態では、前記材料は、ツバキ種子油を抽出するためのツバキ種子である。 In one embodiment of the invention, said material is camellia seed for extracting camellia seed oil.
本発明の一実施形態では、前記界面活性剤は、油相と抽出剤の間の界面張力を２～８ｍＮ／ｍに制御することができる。 In one embodiment of the invention, said surfactant is capable of controlling the interfacial tension between the oil phase and the extractant to 2-8 mN/m.
本発明の一実施形態では、前記粉砕は、粒径１０～５０μｍまでの粉砕である。 In one embodiment of the invention, said grinding is to a particle size of 10-50 μm.
本発明の一実施形態では、前記解乳化は、凍結解乳化、酵素的解乳化またはエタノール溶液解乳化を含む。 In one embodiment of the invention, said demulsification comprises freeze demulsification, enzymatic demulsification or ethanol solution demulsification.
本発明の一実施形態では、前記方法の具体的なステップは、以下のとおりである、
（１）粒径が２０～４０μｍに粉砕された新鮮なツバキ種子材料に、抽出剤としての０～２００ｇ／Ｌの茶サポニンを含む水溶液に加えて、材料と溶液の比率を１：３～１０にし、均一に混合する、
（２）混合物を撹拌しながら５０～１００°Ｃに加熱し、ｐＨを８～１０に調整し、温度を０．５～３時間維持する、
（３）反応完了後、遠心分離により、スラグ相、水相、油相、およびエマルジョンを得る、
（４）その中の油相とエマルジョンを解乳化させる。
In one embodiment of the invention, the specific steps of said method are as follows:
(1) Fresh camellia seed material pulverized to a particle size of 20-40 μm is added to an aqueous solution containing 0-200 g/L of tea saponin as an extractant, and the ratio of material to solution is 1:3-10. and mix evenly,
(2) heating the mixture to 50-100° C. with stirring, adjusting the pH to 8-10 and maintaining the temperature for 0.5-3 hours;
(3) After completion of reaction, centrifugation to obtain slag phase, water phase, oil phase and emulsion;
(4) Demulsify the oil phase and emulsion therein.
本発明の一実施形態では、前記方法は、油料作物の果実または種子を原料とする油脂を調製するために使用される。 In one embodiment of the invention, the method is used to prepare oils and fats derived from fruits or seeds of oil crops.
本発明の一実施形態では、前記方法は、ツバキの果実または種子の油脂を抽出するために使用される。 In one embodiment of the present invention, the method is used to extract oil from camellia fruit or seeds.
本発明の第二目的は、油脂を抽出するための茶サポニン含有抽出剤の適用を提供することであり、前記茶サポニン含有抽出剤は、茶サポニン濃度が１０～２００ｇ／Ｌの茶サポニン含有溶液である。 A second object of the present invention is to provide an application of a tea saponin-containing extractant for extracting fats and oils, wherein the tea saponin-containing extractant is a tea saponin-containing solution having a tea saponin concentration of 10 to 200 g/L. is.
本発明の第三目的は、ツバキ油を抽出する方法を提供することであり、
前記方法は、
水溶液を抽出剤として使用され、抽出対象の材料を粉砕した後、７０°Ｃの抽出剤に０．５時間浸漬し、ｐＨを９に調整し、続いて、遠心分離により、スラグ相、水相、油相およびエマルジョンを分離し、
油相とエマルジョンを集めて解乳化し、清澄油を得、
材料の次のバッチの抽出剤として水相を収集し、水相を繰り返し使用して少なくとも５回の油抽出を行う。サイクル数が増えると、水相中の茶サポニンの含有量は増加し続ける。
A third object of the present invention is to provide a method for extracting camellia oil,
The method includes:
An aqueous solution is used as an extractant, and after pulverizing the material to be extracted, it is immersed in the extractant at 70 ° C for 0.5 hours, the pH is adjusted to 9, and then separated by centrifugation into a slag phase, an aqueous phase. , to separate the oil phase and the emulsion,
collecting and demulsifying the oil phase and the emulsion to obtain a clarified oil;
Collect the aqueous phase as an extractant for the next batch of material and repeat the aqueous phase for at least 5 oil extractions. As the number of cycles increases, the content of tea saponins in the aqueous phase continues to increase.
本発明の一実施形態では、水相を繰り返し使用して５～１２回の油抽出を行う。 In one embodiment of the invention, 5 to 12 oil extractions are performed using repeated aqueous phases.
本発明の一実施形態では、前記方法の具体的なステップは、以下のとおりである、
（１）粒径が２０μｍに粉砕された新鮮なツバキ種子材料に水を加えて、反応材料と溶液の比率を１～５にする、
（２）混合物を撹拌しながら７０°Ｃに加熱し、ｐＨを９に調整し、温度を０．５時間維持する、
（３）遠心分離により、スラグ相、水相、油相、およびエマルジョンを得る、
（４）油相とエマルジョンを取り出して解乳化させ、清澄油を得、次の油抽出の抽出剤として水相を取り出し、不十分な部分は、１：５の比率まで水で補充され、ステップ（１）～（３）を繰り返す。
In one embodiment of the invention, the specific steps of said method are as follows:
(1) adding water to fresh camellia seed material pulverized to a particle size of 20 μm so that the ratio of reaction material to solution is 1-5;
(2) heating the mixture to 70° C. with stirring, adjusting the pH to 9 and maintaining the temperature for 0.5 hours;
(3) centrifugation to obtain a slag phase, an aqueous phase, an oil phase, and an emulsion;
(4) removing the oil phase and emulsion to demulsify to obtain a clear oil, removing the aqueous phase as an extractant for the next oil extraction, the insufficient part being supplemented with water to a ratio of 1:5, step (1) to (3) are repeated.
本発明の第四目的は、前記方法により調製されたツバキ種子油製品またはツバキ種子油含有の製品を提供することである。 A fourth object of the present invention is to provide a camellia seed oil product or product containing camellia seed oil prepared by said method.
有益な効果は、以下のとおりである、
１．本発明の油抽出プロセスはエタノールを使用する必要がなく、コストを節約することができるだけでなく、製造プロセス中の安全性を向上させることができ、防爆などの手段を必要としない。
The beneficial effects are:
1. The oil extraction process of the present invention does not need to use ethanol, which not only saves costs, but also improves safety during the production process, and does not require measures such as explosion protection.
２．本方法は、純水を出発抽出剤として使用する場合、水相を繰り返し使用することにより、油抽出率を約７５％から９２％以上に高めることができ、１５％のエタノール水溶液を出発抽出剤として使用する場合、水相を繰り返し使用することにより、油抽出率を元の８９％から９４％以上に増加することができる。 2. The method can increase the oil extraction rate from about 75% to more than 92% by repeated use of the aqueous phase when pure water is used as the starting extractant, and 15% ethanol aqueous solution is used as the starting extractant. , oil extraction can be increased from the original 89% to over 94% by repeated use of the aqueous phase.
３．本発明の抽出媒体は、水に加えて、ツバキ種子自身に含まれる茶サポニンまたは追加の茶サポニンを含む。茶サポニンは、抽出媒体の表面張力を低減させ、油作物から抽出媒体への油の溶解を促進することができる。抽出プロセスに、ツバキ種子自身に含まれる茶サポニンは水溶液（水相）に入り、水相の前のバッチは原料の次のバッチの抽出媒体として使用する。複数回繰り返した後、抽出媒体中の茶サポニンの含有量は連続的に増加し、油の抽出速度は連続的に増加し、同時に、水相中の茶サポニン、タンパク質および茶多糖類の含有量も連続的に増加する。純水を出発抽出剤として使用する場合、水相を１１回繰り返し使用した後、水相中の茶サポニンの含有量は、１回の抽出で４．２７％から１７．６３％に増加し、タンパク質の含有量は１回の抽出で３．１９％から１１．９８％に増加し、総糖は、１回の抽出で１．７４％から５．６０％に増加した。水相での茶サポニン、タンパク質、茶多糖類のリサイクルに非常に役立つ。 3. The extraction medium of the present invention contains, in addition to water, tea saponins contained in the camellia seeds themselves or additional tea saponins. Tea saponins can reduce the surface tension of the extraction medium and facilitate the dissolution of oil from oil crops into the extraction medium. During the extraction process, the tea saponins contained in the camellia seeds themselves enter an aqueous solution (aqueous phase) and the previous batch of aqueous phase is used as the extraction medium for the next batch of raw material. After repeating multiple times, the content of tea saponins in the extraction medium increased continuously, the extraction rate of oil increased continuously, and at the same time, the content of tea saponins, proteins and tea polysaccharides in the aqueous phase also increases continuously. When pure water is used as the starting extractant, the content of tea saponins in the aqueous phase increases from 4.27% to 17.63% in one extraction after 11 repeated uses of the aqueous phase, Protein content increased from 3.19% to 11.98% in one extraction and total sugars increased from 1.74% to 5.60% in one extraction. It is very useful for recycling tea saponins, proteins and tea polysaccharides in the aqueous phase.
４．本発明の方法は、水相をリサイクルすることにより、抽出剤として使用される水の量を大幅に低減させ、コストを節約することに加えて、廃水の発生も低減させ、経済的利益を達成しながら省エネルギーと環境保護を達成し、それは複数の目的に役立つと言える。 4. By recycling the aqueous phase, the method of the present invention significantly reduces the amount of water used as an extractant, saving costs, as well as reducing wastewater generation, achieving economic benefits. While achieving energy saving and environmental protection, it can be said to serve multiple purposes.
１．油抽出率（清澄油の収量に等しい数値で）＝清澄油の品質／材料の脂肪含有量；定義：反応後の原料に含まれる総脂肪に対する清澄油の比率
２．原料およびスラグ相脂肪の測定：ソックスレー抽出法
３．水性脂肪の測定：Ｒｏｓｅ－Ｇｏｔｔｌｉｅｂ法
４．水相タンパク質の測定：フォリノール法
５．水相総糖の測定：フェノール硫酸法
６．水相茶サポニンの測定：バニリン硫酸比色法
７．スラグ相タンパク質の測定：ケルダール法
８．界面張力の測定：全自動表面張力試験機（ＤＣＡＴ２１）を使用した測定。
1. Oil Extraction Rate (in numbers equal to clarified oil yield) = clarified oil quality/fat content of material; definition: ratio of clarified oil to total fat contained in raw material after reaction. Measurement of raw material and slag phase fat: Soxhlet extraction method3. Determination of aqueous fat: Rose-Gottlieb method4. Aqueous phase protein measurement: Folinol method5. Measurement of aqueous phase total sugar: Phenol-sulfuric acid method6. Determination of Aqueous Phase Tea Saponins: Vanillin Sulfate Colorimetric Method7. Measurement of slag phase protein: Kjeldahl method8. Measurement of interfacial tension: measurement using a fully automatic surface tension tester (DCAT21).
実施例１ 異なる抽出剤の繰り返し使用による抽出効果の比較
（１）新たに粉砕したツバキ種子材料（粒径２０μｍに粉砕）２００ｇを取り、１Ｌの脱イオン水を加えて（反応材料と溶液の比率を１：５にして）均一に混合した、
（２）撹拌しながら７０°Ｃで３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、１時間保温した、
（３）反応後、混合物を５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した、
(４）その中の油相とエマルジョンを取り出して－２０°Ｃの冷蔵庫に２４時間入れ、５０°Ｃの水浴で凍結および解乳化して、清澄油の収率を計算し、その中のスラグ相を取り出して乾燥させ、粉砕後にその脂肪などの含有量を測定し、その中の水相を取り出して次の油抽出の反応液として使用し、反応溶液が不十分な場合は、水を１Ｌまで補充した。スラグ相の脂肪含有量が安定するまでステップ（１）～（３）を繰り返し、同時にその脂肪および他の物質の含有量を測定した。
Example 1 Comparison of extraction effect by repeated use of different extraction agents (1) Take 200 g of freshly ground camellia seed material (ground to a particle size of 20 μm), add 1 L of deionized water (ratio of reaction material to solution to 1:5) was uniformly mixed,
(2) Soak the material at 70°C for 30 minutes with stirring, adjust to pH = 9.0 with 20% NaOH and incubate for 1 hour;
(3) After the reaction, the mixture was centrifuged at 5000 rpm for 15 minutes, and the liquid in the reaction solution was separated into four parts: slag phase, water phase, oil phase and emulsion;
(4) Take out the oil phase and emulsion in it and put it in a refrigerator at -20°C for 24 hours, freeze and demulsify it in a water bath at 50°C, calculate the yield of clarified oil, and slag in it The phase is taken out and dried, and the content of fat etc. is measured after pulverization, and the aqueous phase in it is taken out and used as the reaction solution for the next oil extraction. supplemented up to Steps (1)-(3) were repeated until the fat content of the slag phase stabilized, while its fat and other substance contents were measured.
水相の繰り返し使用中の油回収率、スラグ相の油含量、水相の油含量変化を図1に示すとおりである。総脂肪に対する清澄油の比率は最初の７５．７６％から約９１．２１％に増加することができ、総脂肪に対する水相の油の比率は５．３９％から約２０．５５％に増加することができ、総脂肪に対するスラグ相の脂肪含有量は３．７２％から約２．３７％に減少した。 Fig. 1 shows the oil recovery rate during repeated use of the aqueous phase, the oil content in the slag phase, and the change in oil content in the aqueous phase. The ratio of clarified oil to total fat can be increased from an initial 75.76% to about 91.21%, and the ratio of water phase oil to total fat increases from 5.39% to about 20.55%. and the fat content of the slag phase decreased from 3.72% to about 2.37% relative to total fat.
図２に示すとおり、水相の繰り返し使用により、スラグ相の脂肪含有量を最初の９．００％から約３．１０％に減少することができる。 As shown in Figure 2, repeated use of the water phase can reduce the fat content of the slag phase from the initial 9.00% to about 3.10%.
図３に示すとおり、水相の繰り返し使用により、水相の脂肪含有量を最初の０．６４％から約２．２５％に増加することができ、これは明らかであり、後期遊離油の回収および他の付随物の回収に使用することができる。 As shown in Figure 3, repeated use of the aqueous phase can increase the fat content of the aqueous phase from the initial 0.64% to about 2.25%, which is evident and the late free oil recovery. and other accompaniment recovery.
スラグ相のタンパク質含有量の変化を図４に示すとおりであり、水相の繰り返し使用により、スラグ相のタンパク質含有量は８．９２％から約１０．１９％に増加することができる。油抽出プロセス中、原料に含まれるタンパク質は水相に蓄積され、水相のタンパク質を連続的に増加させ、水相に入るタンパク質は、タンパク質濃度が増加するにつれて溶解度が低減し、それによりスラグ相のタンパク質が高まる。 The change in protein content of the slag phase is shown in Figure 4, with repeated use of the water phase the protein content of the slag phase can be increased from 8.92% to about 10.19%. During the oil extraction process, the protein contained in the raw material accumulates in the water phase, continuously increasing the protein in the water phase, and the protein entering the water phase decreases in solubility as the protein concentration increases, thereby causing the slag phase of protein is increased.
水相中のその他の物質の組成を測定した結果、図５に示すとおり、水相の繰り返し使用により、タンパク質、茶サポニン（ＴＳ）、および総糖含有量が連続的に蓄積された。タンパク質含有量は３．１９％から１１．９８％に、茶サポニンは４．２７％から１７．６３％に、総糖は１．７４％から５．６０％に増加することができる。 The composition of the other substances in the aqueous phase was determined, resulting in continuous accumulation of protein, tea saponin (TS), and total sugar content with repeated use of the aqueous phase, as shown in FIG. Protein content can be increased from 3.19% to 11.98%, tea saponins from 4.27% to 17.63% and total sugars from 1.74% to 5.60%.
抽出前後のシステムの界面張力を測定した結果、水を抽出剤として１回抽出した後、界面張力が７．５７ｍＮ／ｍから５．３２ｍＮ／ｍに減少したことが示された。 Measurement of the interfacial tension of the system before and after extraction showed that the interfacial tension decreased from 7.57 mN/m to 5.32 mN/m after one extraction with water as the extractant.
また、本発明者らは、抽出剤としてタンパク質のみまたは糖のみを含む水溶液を使用し、実施例１の方法で油抽出を実施した結果、油抽出率は大きく増加しなかった。 In addition, the present inventors used an aqueous solution containing only protein or only sugar as an extractant, and performed oil extraction by the method of Example 1. As a result, the oil extraction rate did not increase significantly.
実施例２ 異なる水相抽出剤の抽出効果の比較
４つのグループの粒径２０μｍの新たに粉砕したツバキ種子材料２０ｇを取り、第一グループに４０ｇ／Ｌの濃度の茶サポニン溶液１Ｌを加え、第二グループに１Ｌの脱イオン水を加え、第三グループに１５％のエタノール水溶液１Ｌを加え、第四グループに実施例１で１回繰り返し使用した抽出物１ Ｌを加え、ツバキ種子材料と各溶液を材料と溶液１：５の比率に応じて完全に混合した後、反応器に入れた。
Example 2 Comparison of the extraction effect of different aqueous phase extraction agents Take 20 g of freshly ground camellia seed material with a particle size of 20 μm in four groups, add 1 L of tea saponin solution with a concentration of 40 g/L to the first group, Add 1 L of deionized water to the second group, add 1 L of 15% ethanol aqueous solution to the third group, add 1 L of the extract used repeatedly in Example 1 to the fourth group, and add Camellia seed material and each solution. was thoroughly mixed according to the ratio of material and solution 1:5 and then put into the reactor.
抽出ステップは、実施例１のステップ（２）～（３）と同様に実施した。 The extraction steps were performed in the same manner as steps (2)-(3) of Example 1.
油相とエマルジョンを取り出し、－２０°Ｃの冷蔵庫に２４時間入れ、５０°Ｃの水浴で凍結および解乳化し、清澄油の収率を計算した。そのスラグ相を取り出して乾燥させ、粉砕後にその中の脂肪などの含有量を測定した。 The oil phase and emulsion were removed, placed in a −20° C. refrigerator for 24 hours, frozen and demulsified in a 50° C. water bath, and the yield of clarified oil was calculated. The slag phase was taken out and dried, and the content of fat etc. therein was measured after pulverization.
抽出剤システムの界面張力を測定した結果、油相と抽出剤間の界面張力は、４０ｇ／Ｌ茶サポニン溶液（５．７５ｍＮ／ｍ）、脱イオン水（８．２０ｍＮ／ｍ）、１５％エタノール水溶液（２．１２ｍＮ／ｍ）、１回繰り返し使用した抽出溶液（７．９６ｍＮ／ｍ）であった。 As a result of measuring the interfacial tension of the extractant system, the interfacial tension between the oil phase and the extractant is 40 g/L tea saponin solution (5.75 mN/m), deionized water (8.20 mN/m), 15% ethanol Aqueous solution (2.12 mN/m), extraction solution (7.96 mN/m) used repeatedly.
４つのグループの材料の反応後の油抽出率を測定した結果、４％茶サポニンを使用した油抽出率は８１．６８％で、脱イオン水を使用した油抽出率は７５．４５％で、１５％のエタノール水溶液を使用した油抽出率は８９．３９％で、１回繰り返し使用した抽出液で抽出した油抽出率は８０．９６％であった。 After measuring the oil extraction rate of the four groups of materials after reaction, the oil extraction rate using 4% tea saponin was 81.68%, the oil extraction rate using deionized water was 75.45%, The oil extraction rate using the 15% ethanol aqueous solution was 89.39%, and the oil extraction rate extracted with the extraction liquid used repeatedly was 80.96%.
実施例３ 異なる茶サポニン溶液の抽出効果の比較
粉砕したツバキ種子は、茶サポニン溶液の異なる濃度（０～１００ｇ／Ｌ）で油抽出し、それぞれ、脱イオン水、１０ｇ／Ｌの茶サポニン溶液、４０ｇ／Ｌの茶サポニン溶液、および１００ｇ／Ｌの茶サポニン溶液を用いて抽出し、具体的な抽出ステップは以下のとおりである、
（１）新たに粉砕したツバキ種子材料（粒径２０μｍに粉砕）２００ｇを取り、１Ｌの上記脱イオン水または茶サポニン溶液を加えて（反応材料と溶液の比率を１：５にして）均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した、
抽出剤システムの界面張力を測定した結果、油相と抽出剤間の界面張力は、それぞれ、脱イオン水（８．２０ｍＮ／ｍ）、１０ｇ／Ｌ茶サポニン溶液（７．８５ｍＮ／ｍ）、４０ｇ／Ｌ茶サポニン溶液（５．７５ｍＮ／ｍ）、１００ｇ／Ｌ茶サポニン溶液（５．４３ｍＮ／ｍ）であった。
Example 3 Comparison of extraction effect of different tea saponin solutions Crushed camellia seeds were oil-extracted with different concentrations of tea saponin solution (0-100 g/L), deionized water, 10 g/L tea saponin solution, 40 g/L tea saponin solution and 100 g/L tea saponin solution are used for extraction, and the specific extraction steps are as follows:
(1) Take 200 g of freshly ground camellia seed material (ground to a particle size of 20 μm), add 1 L of the above deionized water or tea saponin solution (with a ratio of reaction material and solution of 1:5) and uniformly mixed,
(2) Heated to 70°C with stirring, soaked the material for 30 minutes, adjusted to pH=9.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion;
As a result of measuring the interfacial tension of the extractant system, the interfacial tension between the oil phase and the extractant is deionized water (8.20 mN/m), 10 g/L tea saponin solution (7.85 mN/m), 40 g /L tea saponin solution (5.75 mN/m) and 100 g/L tea saponin solution (5.43 mN/m).
反応後の油抽出率は、それぞれ、純水グループで７５．４５％、１０ｇ／Ｌ茶サポニングループで７６．４７％、４０ｇ／Ｌ茶サポニングループで８２．６８％、１００ｇ／Ｌ茶サポニングループで８１．４４％であった。 The oil extraction rates after the reaction were 75.45% for the pure water group, 76.47% for the 10 g/L tea saponin group, 82.68% for the 40 g/L tea saponin group, and 82.68% for the 100 g/L tea saponin group, respectively. It was 81.44%.
実施例４ 異なる抽出剤の抽出効果の比較
それぞれ、脱イオン水、５０ｇ／ＬのＴｗｅｅｎ２０、体積分率１５％のエタノール、４０ｇ／Ｌの茶サポニン水溶液、１００ｇ／Ｌのラウリル硫酸ナトリウム水溶液の油抽出効果を試行する。具体的なプロセスは以下のとおりである、
（１）漢方薬粉砕機で粒径約２０μｍに新たに粉砕したツバキ種子材料を５つのグループに分けて各グループ２００ｇとし、第一グループには１Ｌの脱イオン水を加え、第二グループには１Ｌの１０％Ｔｗｅｅｎ２０水溶液を加え、第三グループに体積分率１５％のエタノール水溶液を加え、第四グループに濃度が４％の茶サポニン溶液１Ｌを加え、第五グループには濃度が１０％のラウリル硫酸ナトリウム溶液１Ｌを加え（反応材料と溶液の比率を１：５にして）、均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した、
その中の油相とエマルジョンを取り出し、－２０°Ｃの冷蔵庫に２４時間入れ、かつ５０°Ｃの水浴で凍結および解乳化し、清澄油の収率を計算した。その中のスラグ相を取り出して乾燥させ、粉砕後に脂肪などの含有量を測定した。
Example 4 Comparison of extraction effect of different extractants Oil extraction of deionized water, 50 g/L Tween20, 15% volume fraction ethanol, 40 g/L tea saponin aqueous solution, 100 g/L sodium lauryl sulfate aqueous solution respectively try the effect. The specific process is as follows:
(1) Freshly pulverized camellia seed material to a particle size of about 20 μm with a herbal medicine grinder, divided into 5 groups, each group 200 g, adding 1 L of deionized water to the first group, and adding 1 L to the second group. 10
(2) Heated to 70°C with stirring, soaked the material for 30 minutes, adjusted to pH=9.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion;
The oil phase and emulsion therein were taken out, placed in a -20°C refrigerator for 24 hours, and frozen and demulsified in a 50°C water bath to calculate the yield of clarified oil. The slag phase therein was taken out and dried, and the content of fat and the like was measured after pulverization.
抽出剤システムの界面張力を測定した結果、油相と抽出剤間の界面張力は、脱イオン水（８．２０ｍＮ／ｍ）、５０ｇ／ＬＴｗｅｅｎ２０（４．８ ｍＮ／ｍ）、１５％のエタノール水溶液（２．１２ｍＮ／ｍ）、４０ｇ／Ｌの茶サポニン溶液（５．７５ｍＮ／ｍ）、１００ｇ／Ｌのラウリル硫酸ナトリウム水溶液（１６．２ｍＮ／ｍ）であった。 As a result of measuring the interfacial tension of the extractant system, the interfacial tension between the oil phase and the extractant is deionized water (8.20 mN/m), 50 g/LTween20 (4.8 mN/m), 15% ethanol aqueous solution (2.12 mN/m), 40 g/L tea saponin solution (5.75 mN/m), and 100 g/L sodium lauryl sulfate aqueous solution (16.2 mN/m).
５つのグループの原料を反応させた後の油抽出の結果を図６に示すとおり、比較後、Ｔｗｅｅｎ２０、エタノール、茶サポニンを加えた後、透明なオイルの収率が純水よりも著しく高いが、１０％のラウリル硫酸ナトリウム水溶液を加えた油抽出効果が著しく低い。そのうち、Ｔｗｅｅｎ２０と茶サポニングループの清澄油の収率は、それぞれ８０．８４％と８２．２１％に達し、１５％のエタノール水溶液の油抽出効果に近く、１００ｇ／Ｌのラウリル硫酸ナトリウムの清澄油の収率はわずか５５．４７％であった。
The results of oil extraction after reacting five groups of raw materials are shown in Fig. 6. After comparison, after adding
エマルジョン中の残留脂肪の比率は、異なる抽出剤間で異なり、同じ原材料で調製されたエマルジョン中の総脂肪に対する残留脂肪の比率は、１０％ラウリル硫酸ナトリウム（２５．８０％）＞純水グループ（１２．９９％）＞１０％のＴｗｅｅｎ２０グループ（８．８６％）＞４％の茶サポニングループ（６．７１％）＞１５％のエタノールグループ（６．２８％）であった。
The ratio of residual fat in emulsions differs between different extractants, and the ratio of residual fat to total fat in emulsions prepared with the same raw materials is 10% sodium lauryl sulfate (25.80%) >pure water group ( 12.99%) > 10
Ｔｗｅｅｎ２０と茶サポニンは両方とも、ＨＬＢ値が約１５～１７の非イオン性界面活性剤であり、ラウリル硫酸ナトリウムは、ＨＬＢ値が約４０のアニオン性界面活性剤である。Ｔｗｅｅｎ２０と茶サポニンを抽出剤とする抽出プロセス中の乳濁液含有量が少なく、清澄油の収率がより高かった。天然の非イオン性界面活性剤として、茶サポニンはツバキ種子油の抽出プロセスの水相に豊富であり、理想的な天然抽出剤である。
Both
実施例５
８００ｇの原料を使用して油抽出反応を増幅し、そのフローは以下のとおりである、
（１）漢方薬粉砕機で粒径約２０μｍに新たに粉砕したツバキ種子材料８００ｇを取り、４Ｌの脱イオン水を加えて（反応材料と溶液の比率を１：５にして）均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離する、
（４）その中の油相とエマルジョンを取り出し、－２０°Ｃの冷蔵庫に２４時間入れ、かつ５０°Ｃの水浴で凍結および解乳化し、清澄油の収率を計算した。その中のスラグ相を取り出して乾燥させ、粉砕後に脂肪などの含有量を測定した。その中の水相を取り出して次の油抽出の反応液として使用し、反応溶液が不十分な場合は、水を補充する。スラグ相の脂肪含有量が安定するまで、すなわち、得られたスラグ相中の脂肪含有量の変化が１％以内に安定した場合、ステップ（１）～（３）を繰り返し、同時にその脂肪および他の物質の含有量を測定した。かつ、水相中の茶サポニン、総糖、タンパク質の濃度を測定した。
Example 5
Using 800g of raw material to amplify the oil extraction reaction, the flow is as follows:
(1) Take 800 g of camellia seed material freshly pulverized to a particle size of about 20 μm by a Chinese herbal medicine grinder, add 4 L of deionized water (with a ratio of reaction material and solution of 1:5) and mix evenly;
(2) Heated to 70°C with stirring, soaked the material for 30 minutes, adjusted to pH=9.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, centrifuge at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion;
(4) The oil phase and emulsion therein were taken out, placed in a -20°C refrigerator for 24 hours, and frozen and demulsified in a 50°C water bath, and the yield of clarified oil was calculated. The slag phase therein was taken out and dried, and the content of fat and the like was measured after pulverization. The aqueous phase therein is taken out and used as the reaction solution for the next oil extraction, and if the reaction solution is insufficient, water is added. Steps (1)-(3) are repeated until the fat content of the slag phase stabilizes, i.e. when the change in fat content in the resulting slag phase stabilizes within 1%, simultaneously was measured. In addition, the concentrations of tea saponin, total sugar and protein in the aqueous phase were measured.
清澄油の収率が安定する傾向がある場合（８回目の繰り返し使用後）、水相の一部が取り出され、付随物と脂肪の分離として使用することができる。 When the yield of clarified oil tends to stabilize (after the 8th iteration), a portion of the aqueous phase can be removed and used as a seperate of the attendant and fat.
水相の繰り返し使用中の清澄油の収率、スラグ相の油含量、および水相の油含量と付随物の変化を図７～８に示すとおりである。 The change in yield of clarified oil, slag phase oil content, and water phase oil content and concomitant during repeated use of the water phase is shown in Figures 7-8.
図７から、反応を増幅し、８００ｇの原材料を使用して水相で１２回繰り返し油抽出した後、清澄油の収率およびスラグ相と水相中の脂肪の分布法則が小規模抽出と同じ傾向を示すことが分かった。清澄油の収率は７５．６２％から９２．０６％に増加し、スラグ相中の総脂肪に対する脂肪の比率は１１．９０％から３．３８％に減少し、水相中の総脂肪に対する脂肪の比率は３．２１％から１０．８７％に増加した。また、水相の繰り返し使用により、油抽出プロセス中に生成されたエマルジョンの量が連続的に減少することにより、清澄油の含有量が増加した。
From FIG. 7, it can be seen that after amplifying the reaction and using 800 g of raw material to repeat oil extraction in the
図８から、水相中の付随物が蓄積し続ける過程にあることが分かった。そのうち、茶サポニンの含有量は４．４５％から約１６％に増加することができ、タンパク質濃度は３．５％から１０．９１％に増加することができ、総糖濃度は２．６７％から６．９７％に増加ことができ、いずれも小規模抽出の法則と一致した。 From FIG. 8, it was found that the accompanying substances in the aqueous phase were in the process of continuing to accumulate. Among them, the content of tea saponins can be increased from 4.45% to about 16%, the protein concentration can be increased from 3.5% to 10.91%, and the total sugar concentration is 2.67%. to 6.97%, all consistent with the law of small scale sampling.
実施例２と比較して、増幅後の抽出効果は、タンパク質、茶サポニン含有量および総糖含有量に関して元の濃度の約２倍の増加があった。 Compared to Example 2, the extraction effect after amplification was about double the original concentration with respect to protein, tea saponin content and total sugar content.
実施例６
（１）新たに粉砕したツバキ種子材料（粒径２０μｍに粉砕）２００ｇを取り、１Ｌの体積分率１５％のエタノール水溶液を加えて（反応材料と溶液の比率を１：５にして）均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した、
（４）その中の油相とエマルジョンを取り出し、－２０°Ｃの冷蔵庫に２４時間入れ、かつ５０°Ｃの水浴で凍結および解乳化し、清澄油の収率を計算した。その中のスラグ相を取り出して乾燥させ、粉砕後に脂肪などの含有量を測定し、その中の水相を取り出して次の油抽出の反応液として使用し、反応溶液が不十分な場合は、水を１Ｌまで補充した。スラグ相の脂肪含有量が安定するまでステップ（１）～（３）を繰り返し、同時にその脂肪および他の物質の含有量を測定した。
Example 6
(1) Take 200 g of freshly pulverized camellia seed material (pulverized to a particle size of 20 μm), add 1 L of ethanol aqueous solution with a volume fraction of 15% (with a ratio of reaction material and solution of 1:5) to homogenize mixed,
(2) Heated to 70°C with stirring, soaked the material for 30 minutes, adjusted to pH=9.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion;
(4) The oil phase and emulsion therein were taken out, placed in a -20°C refrigerator for 24 hours, and frozen and demulsified in a 50°C water bath, and the yield of clarified oil was calculated. The slag phase in it is taken out and dried, the content of fat etc. is measured after pulverization, the water phase in it is taken out and used as the reaction liquid for the next oil extraction, if the reaction solution is insufficient, Topped up with water to 1L. Steps (1)-(3) were repeated until the fat content of the slag phase stabilized, while its fat and other substance contents were measured.
結果を図９に示すとおり、体積分率１５％のエタノール水溶液で油を抽出し、かつ水相を１１回繰り返し使用すると、油抽出率は８９．７６％から約９４．１０％に増加し、スラグ相中の脂肪の残存率は２．９２％から２．０８％に減少したが、水相中の脂肪の残存率は４．３９％から１７．３１％に増加した。 The results are shown in FIG. 9, when the oil is extracted with an ethanol aqueous solution with a volume fraction of 15% and the aqueous phase is repeatedly used 11 times, the oil extraction rate increases from 89.76% to about 94.10%, The fat retention in the slag phase decreased from 2.92% to 2.08%, while the fat retention in the water phase increased from 4.39% to 17.31%.
実施例７
（１）新たに粉砕したツバキ種子材料（粒径２０～４０μｍに粉砕）５００ｇを取り、１．５Ｌの純水を加えて（反応材料と溶液の比率を１：３にして）均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した。
反応後の油抽出率は６５．５４％であった。
Example 7
(1) Take 500 g of freshly pulverized camellia seed material (pulverized to a particle size of 20 to 40 μm), add 1.5 L of pure water (the ratio of reaction material and solution is 1:3) and mix uniformly. ,
(2) Heated to 70°C with stirring, soaked the material for 30 minutes, adjusted to pH=9.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, it was centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion.
The oil extraction rate after the reaction was 65.54%.
実施例８
（１）新たに粉砕したツバキ種子材料（粒径２０～４０μｍに粉砕）５００ｇを取り、１．５Ｌの純水を加えて（反応材料と溶液の比率を１：３にして）均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、２時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した。
反応後の油抽出率は６７．３６％であった。
Example 8
(1) Take 500 g of freshly pulverized camellia seed material (pulverized to a particle size of 20 to 40 μm), add 1.5 L of pure water (the ratio of reaction material and solution is 1:3) and mix uniformly. ,
(2) Heated to 70°C with stirring, soaked the material for 30 minutes, adjusted to pH = 9.0 with 20% NaOH and left to react for 2 hours;
(3) After the reaction, it was centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion.
The oil extraction rate after the reaction was 67.36%.
実施例９
（１）新たに粉砕したツバキ種子材料（粒径２０～４０μｍに粉砕）１Ｋｇを取り、それぞれ１０Ｌの純水を加えて（反応材料と溶液の比率を１：１０にして）均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝９．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した。
反応後の油抽出率は８０．０２％であった。
Example 9
(1) Take 1 kg of freshly pulverized camellia seed material (pulverized to a particle size of 20 to 40 μm), add 10 L of pure water to each (with a ratio of reaction material and solution of 1:10) and mix uniformly;
(2) Heated to 70°C with stirring, soaked the material for 30 minutes, adjusted to pH=9.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, it was centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion.
The oil extraction rate after the reaction was 80.02%.
実施例１０
（１）新たに粉砕したツバキ種子材料（粒径２０～４０μｍに粉砕）１Ｋｇを取り、それぞれ１０Ｌの純水を加えて（反応材料と溶液の比率を１：１０にして）均一に混合した、
（２）撹拌しながら７０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝１０．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した。
反応後の油抽出率は８２．３３％であった。
Example 10
(1) Take 1 kg of freshly pulverized camellia seed material (pulverized to a particle size of 20 to 40 μm), add 10 L of pure water to each (with a ratio of reaction material and solution of 1:10) and mix uniformly;
(2) Heated to 70°C with stirring, soaked material for 30 minutes, adjusted to pH = 10.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, it was centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion.
The oil extraction rate after the reaction was 82.33%.
実施例１１
（１）新たに粉砕したツバキ種子材料（粒径２０～４０μｍに粉砕）１Ｋｇを取り、それぞれ１０Ｌの純水を加えて（反応材料と溶液の比率を１：１０にして）均一に混合した、
（２）撹拌しながら９０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝１０．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した。
反応後の油抽出率は８４．０２％であった。
Example 11
(1) Take 1 kg of freshly pulverized camellia seed material (pulverized to a particle size of 20 to 40 μm), add 10 L of pure water to each (with a ratio of reaction material and solution of 1:10) and mix uniformly;
(2) Heated to 90°C with stirring, soaked the material for 30 minutes, adjusted to pH = 10.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, it was centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion.
The oil extraction rate after the reaction was 84.02%.
実施例１２
（１）新たに粉砕したツバキ種子材料（粒径２０～４０μｍに粉砕）１Ｋｇを取り、それぞれ１０Ｌの純水を加えて（反応材料と溶液の比率を１：１０にして）均一に混合した、
（２）撹拌しながら５０°Ｃに加熱し、３０分間材料を浸漬し、２０％のＮａＯＨでｐＨ＝１０．０に調整し、１時間反応し続けた、
（３）反応後、５０００ｒｐｍで１５分間遠心分離し、反応溶液中の液体をスラグ相、水相、油相およびエマルジョンの４つの部分に分離した。
反応後の油抽出率は７５．４５％であった。
Example 12
(1) Take 1 kg of freshly pulverized camellia seed material (pulverized to a particle size of 20 to 40 μm), add 10 L of pure water to each (with a ratio of reaction material and solution of 1:10) and mix uniformly;
(2) Heated to 50°C with stirring, soaked the material for 30 minutes, adjusted to pH = 10.0 with 20% NaOH and left to react for 1 hour;
(3) After the reaction, it was centrifuged at 5000 rpm for 15 minutes to separate the liquid in the reaction solution into four parts: slag phase, water phase, oil phase and emulsion.
The oil extraction rate after the reaction was 75.45%.
実施例１３ ツバキ科の他の種子に対する油抽出
具体的な実施形態と前の実施例との違いは、材料がツバキ種子、茶種子、および茶花種子であることである。油抽出率を表1に示す。
比較例１
スパン－２０を使用して油抽出し、抽出ステップは実施例４と同じであり、結果は、抽出率が５１．６％であることを示した。
Comparative example 1
The oil was extracted using Span-20, the extraction step was the same as in Example 4, and the results showed that the extraction rate was 51.6%.
本発明を上記の好ましい実施形態に開示したが、本発明はこれに限定されるものではなく、本発明の精神および範囲から逸脱することなく、様々な修正および変更を行うことができ、したがって、本発明の保護範囲は、特許請求の範囲によって決定されるべきである。 Although the present invention has been disclosed in the preferred embodiments set forth above, the invention is not so limited and various modifications and changes can be made without departing from the spirit and scope of the invention; The protection scope of the present invention should be determined by the claims.
Claims (13)
水またはエタノールを含む水溶液を媒介とし、１０～２００ｇ／Ｌの茶サポニンが添加された抽出剤を使用して油を抽出することを含み、
抽出対象の材料を粉砕した後、５０～１００℃の抽出剤に０．５～３時間浸し、ｐＨを８～１０に調整し、続いて、遠心分離により、スラグ相、水相、油相およびエマルジョンを分離し、油相とエマルジョンを集めて解乳化し、清澄油を得ることを特徴とする、
水媒法による油抽出方法。 An oil extraction method by an aqueous medium method,
extracting the oil using an extractant with water or an aqueous solution containing ethanol as a medium and to which 10-200 g/L of tea saponin is added;
After grinding the material to be extracted, it is soaked in an extractant at 50-100° C. for 0.5-3 hours, the pH is adjusted to 8-10, and then centrifuged to separate the slag phase, water phase, oil phase and Separating the emulsion, collecting and demulsifying the oil phase and the emulsion to obtain a clear oil,
Oil extraction method by aqueous method.
請求項１に記載の方法。 characterized in that the material comprises fruits or seeds of oil crops,
The method of claim 1.
請求項２に記載の方法。 The material is camellia seed for extracting camellia seed oil,
3. The method of claim 2.
請求項１に記載の方法。 characterized by controlling the interfacial tension between the oil phase and the extractant to 13 mN / m or less,
The method of claim 1 .
請求項１に記載の方法。 The demulsification process adopts a method including freeze demulsification, enzymatic demulsification or ethanol solution demulsification,
The method of claim 1 .
（１）新たに粉砕したツバキ種子材料に、抽出剤としての１０～２００ｇ／Ｌの茶サポニンが添加された水溶液を加えて、均一に混合する、
（２）混合物を撹拌しながら５０～１００°Ｃに加熱し、ｐＨを８～１０に調整し、０．５～３時間保温する、
（３）反応完了後、遠心分離により、スラグ相、水相、油相、およびエマルジョンを得る、
（４）油相とエマルジョンを解乳化させる、ことを特徴とする、
請求項１～５のいずれか一項に記載の方法。 The specific steps of the method are as follows:
(1) An aqueous solution containing 10-200 g/L of tea saponin as an extractant is added to freshly pulverized camellia seed material and mixed uniformly.
(2) heating the mixture to 50-100°C with stirring, adjusting the pH to 8-10 and keeping it warm for 0.5-3 hours;
(3) After completion of reaction, centrifugation to obtain slag phase, water phase, oil phase and emulsion;
(4) demulsifying the oil phase and the emulsion,
The method according to any one of claims 1-5 .
水媒体法による油抽出効率の改善を補助するための茶サポニンの使用。 Oil extraction is performed using a solution to which tea saponin with a concentration of 10 to 200 g / L is added,
Use of tea saponins to help improve oil extraction efficiency by aqueous methods.
油相とエマルジョンを集めて解乳化し、清澄油を得、
次のバッチの材料の抽出剤として水相を収集し、水相を少なくとも３回繰り返し使用し、このプロセス中、原料中の茶サポニンは連続的に水相に入り、水相中の茶サポニンの濃度を連続的に増加させる、ことを特徴とする、
ツバキ油の抽出方法。 Using an aqueous solution containing 10-200 g/L of tea saponin as a medium, the material to be extracted is pulverized and then immersed in an extractant at 50-100°C for 0.5-3 hours to adjust the pH to 8-10. , followed by centrifugation to separate the slag phase, water phase, oil phase and emulsion,
collecting and demulsifying the oil phase and the emulsion to obtain a clarified oil;
The aqueous phase is collected as an extractant for the next batch of material, and the aqueous phase is repeatedly used at least three times. characterized by continuously increasing the concentration,
Extraction method of camellia oil.
請求項８に記載の方法。 The aqueous phase is repeatedly used to perform oil extraction 3 to 12 times,
9. The method of claim 8 .
（１）粒径が２０μｍの新たに粉砕したツバキ種子材料に水を加えて、反応材料と溶液の比率を１：５にする、
（２）混合物を撹拌しながら７０°Ｃに加熱し、ｐＨを９に調整し、０．５時間維持する、
（３）遠心分離により、スラグ相、水相、油相、およびエマルジョンを得る、
（４）その中の油相とエマルジョンを取り出して解乳化させ、清澄油を得て、次の油抽出の抽出剤として水相を取り出し、不十分な部分は、１：３～１０の比率まで水で補充され、ステップ（１）～（３）を繰り返す、ことを特徴とする、
請求項８または９に記載の方法。 The specific steps of the method are as follows:
(1) adding water to a freshly ground camellia seed material with a particle size of 20 μm to a ratio of reaction material to solution of 1:5;
(2) Heat the mixture to 70° C. with stirring, adjust the pH to 9 and maintain for 0.5 hours.
(3) centrifugation to obtain a slag phase, an aqueous phase, an oil phase, and an emulsion;
(4) Remove the oil phase and emulsion therein to demulsify to obtain a clear oil, remove the aqueous phase as an extractant for the next oil extraction, and the insufficient part up to a ratio of 1:3-10. replenished with water and repeating steps (1) to (3),
10. A method according to claim 8 or 9 .
請求項１１に記載の使用。 The camellia fruits or seeds include at least one of camellia seeds, tea seeds, and tea flower seeds,
Use according to claim 11 .
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