JP4826848B2 - Process for producing fractionated monkey oil - Google Patents
Process for producing fractionated monkey oil Download PDFInfo
- Publication number
- JP4826848B2 JP4826848B2 JP2009083515A JP2009083515A JP4826848B2 JP 4826848 B2 JP4826848 B2 JP 4826848B2 JP 2009083515 A JP2009083515 A JP 2009083515A JP 2009083515 A JP2009083515 A JP 2009083515A JP 4826848 B2 JP4826848 B2 JP 4826848B2
- Authority
- JP
- Japan
- Prior art keywords
- fat
- oil
- content
- weight
- monkey
- 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.)
- Expired - Fee Related
Links
Landscapes
- Fats And Perfumes (AREA)
- Edible Oils And Fats (AREA)
Description
本発明はカカオ代用脂として使用できるサル脂分別油の製造法、特に品質劣化の進んだ低品質のサル脂原油から、高品質のカカオ代用脂として使用できるサル脂分別油の製造法に関する。 The present invention relates to a method for producing a sebum fraction oil that can be used as a cacao substitute oil, and more particularly, to a method for producing a sebum fraction oil that can be used as a high quality cacao substitute oil from a low-quality saf oil crude oil whose quality has deteriorated.
従来からチョコレート用油脂の代表であるカカオ脂を代替しうる油脂として、対称型トリグリセリドの１、３ジ飽和−２不飽和トリグリセリド（以下ＳＵＳ、Ｓ：飽和脂肪酸 、Ｕ：不飽和脂肪酸）を主成分とした油脂であるカカオ代用脂が使用されている。対称型トリグリセリドを構成する代表的な飽和脂肪酸はパルミチン酸（Ｐ）、ステアリン酸 （Ｓｔ），アラキジン酸（Ａ）であり、不飽和脂肪酸はオレイン酸（Ｏ）である。主にＰＯＰはパーム油、チャイニーズタローの分別油から得られ、ＰＯＳｔはイリッペ油、 モーラー油など及びそれらの分別油から得られる。ＳｔＯＳｔはコクム油、マンゴ核油、シア脂、サル脂およびそれらの分別油から得られる。 As fats and oils that can replace cocoa butter, which is a representative fat for chocolate, symmetric triglycerides 1, 3 di-saturated-2 unsaturated triglycerides (hereinafter SUS, S: saturated fatty acids, U: unsaturated fatty acids) are the main components. The cacao substitute fat which is the fats and oils used is used. Typical saturated fatty acids constituting the symmetric triglyceride are palmitic acid (P), stearic acid (St), and arachidic acid (A), and the unsaturated fatty acid is oleic acid (O). POP is mainly obtained from palm oil and Chinese tallow fractionated oil, and POSt is obtained from iripe oil, mora oil and the like and fractionated oils thereof. StOSt is obtained from Kokum oil, mango kernel oil, shea fat, monkey fat and their fractionated oils.
サル脂は、ＳＯＳ（主成分はＳｔＯＳｔ、ＡＯＳｔ)を多く含むので、精製サル脂あるいはサル脂分別油はカカオ代用脂の原料油のひとつとしてますます重要な原料油脂である 。 Since monkey fat contains a large amount of SOS (main components are StOSt and AOSt), refined monkey fat or monkey fat fraction oil is an increasingly important raw oil and fat as one of the raw oils for cacao substitute fat.
サル脂は、サルシード脂とも呼ばれ、天然に生育するショリアロブスタというカン木の種子から主にヘキサンを用いて抽出される油脂で、ボルネオタロー型油脂と総称される油脂群のなかの一種である。ショリアロブスタ種子中の油脂は、加水分解酵素により加水分解されやすいため、種子集荷後は速やかに油脂の抽出を行うのが望ましいが、集荷地域の労働事情や交通事情のために必ずしも速やかな油脂の抽出がなされないのが実情である。そのため、入手したサル脂原油の中には加水分解が過度に進んだ、いわゆる低品質の原料油脂がしばしば見かけられる。一方、サル脂にはジヒドロキシステアリン酸を構成脂肪酸として含有するトリグリセリド（以下ＤＨＳ−ＴＧ）やエポキシステアリン酸を構成脂肪酸として含有するトリグリセリド（以下ＥＰ−ＴＧ）が存在すること、特にＤＨＳ−ＴＧが多く含まれることが知られている。低品質の原料油脂にはＤＨＳ−ＴＧが２〜１０重量％含まれ、該油脂を精製したサル脂や従来のサル脂分別油でも通常は１．０重量％以上含むため、かかる油脂は良好な品質のカカオ代用脂と言えないものになる。具体的には、チョコレート作製時のチョコレート生地粘度上昇を引き起こしテンパリングが困難になるとともに、離型性も不良となる。その結果、チョコレートの艶がなく、口溶けも不良となるという大きな問題がある。 Monkey fat, also called monkey seed fat, is an oil that is extracted mainly from corn tree seeds called Shoria Robusta, using hexane, and is a kind of oils and fats collectively called Borneo Tallow oil. is there. Since oils and fats in Shoria robusta seeds are easily hydrolyzed by hydrolytic enzymes, it is desirable to extract oils and fats immediately after seed collection. However, oils and fats are not always prompt due to labor and traffic conditions in the collection area. The fact is that no extraction is made. Therefore, so-called low-quality raw material fats and oils that are excessively hydrolyzed are often found in the obtained monkey fat crude oil. On the other hand, monkey fat contains triglyceride (hereinafter referred to as DHS-TG) containing dihydroxystearic acid as a constituent fatty acid and triglyceride (hereinafter referred to as EP-TG) containing epoxy stearic acid as a constituent fatty acid, especially DHS-TG. It is known to be included. The low-quality raw material fats and oils contain 2 to 10% by weight of DHS-TG, and the fats and oils obtained by purifying the fats and oils and the conventional fractionated monkey fats usually contain 1.0% by weight or more. It will not be a quality cacao substitute fat. Specifically, the chocolate dough viscosity is increased at the time of chocolate production, tempering becomes difficult, and releasability becomes poor. As a result, there is a big problem that the chocolate has no gloss and the melting of the mouth is poor.
低品質のサル脂原料油脂から、上記のようなＤＨＳ−ＴＧを除去して高品質のカカオ代用脂を得るべく下記のような試みがなされている。
非特許文献１は、サル脂の乾式分別又は極性溶剤のアセトン分別によるＤＨＳ−ＴＧおよびジグリセリド（以下DG）除去方法、あるいはサル脂中のＤＨＳ−ＴＧおよびDGを高濃度に分画する方法に関するものである。極性溶剤のアセトンを用いて分別し、結晶部のＤＨＳ−ＴＧおよびDGを減少させる方法と、シリカゲルカラムでＤＨＳ−ＴＧ及びDGを吸着、除去して減少させる方法が記載されているが、前者はＤＨＳ−ＴＧの除去が不十分で、後者は高価なシリカゲルカラムを用いる必要があり、さらにそのシリカゲルカラム再生のため多量の強極性溶剤を使用する必要があり、実用的な方法ではない。
Non-Patent Document 1 relates to a method for removing DHS-TG and diglyceride (hereinafter referred to as DG) by dry fractionation of monkey fat or acetone as a polar solvent, or a method of fractionating DHS-TG and DG in monkey fat at a high concentration. It is. The method of fractionating using acetone as a polar solvent to reduce DHS-TG and DG in the crystal part and the method of reducing by adsorbing and removing DHS-TG and DG on a silica gel column are described. The removal of DHS-TG is insufficient, and the latter requires the use of an expensive silica gel column, and a large amount of strong polar solvent must be used for regeneration of the silica gel column, which is not a practical method.
特許文献１は、サル脂の脱ガムやアルカリ脱酸による精製、及び非極性溶剤のヘキサン分別や活性剤分別によるＤＨＳ−ＴＧ，ＥＰ−ＴＧの除去方法であるが、ＳＵＳ含有量の低いサル脂分別油が得られたにすぎなかった。 Patent Document 1 is a method for removing DHS-TG and EP-TG by purification of monkey fat by degumming or alkali deoxidation, and hexane fractionation or activator fractionation of a nonpolar solvent, but monkey fat having a low SUS content. Only a fractionated oil was obtained.
特許文献２は、サル脂を分画して得られるＳＵＳ含有量が８０−９０重量％であるサル脂フラクションからなるハードバターに関するものである。ヘキサンなどの溶剤を使用して分別するものであり、一旦溶液を比較的弱く冷却して析出する高融点部の結晶を除去した後、再び低温にまで冷却し、析出する中融点フラクションの結晶を集める方法であるが、かかる方法では１段目の分別で残存したＤＨＳ−ＴＧは、２段目の分別で中融点部と共に結晶化するため、ＤＨＳ−ＴＧの除去が不十分という問題があった。 Patent Document 2 relates to a hard butter comprising a monkey fat fraction having a SUS content of 80 to 90% by weight obtained by fractionating monkey fat. The solvent is fractionated using a solvent such as hexane, and once the solution is cooled relatively weakly to remove precipitated high melting point crystals, the solution is cooled to a low temperature again, and the precipitated medium melting point fraction crystals are separated. In this method, DHS-TG remaining in the first-stage fractionation is crystallized together with the middle melting point portion in the second-stage fractionation, so that there is a problem that DHS-TG is not sufficiently removed. .
特許文献３は、サル脂を乾式分別又は非極性溶剤のヘキサン分別し、得た液状部を液状部に対して１００〜９００重量％の極性溶剤で溶剤分別することによるＤＨＳ−ＴＧの除去方法であるが、乾式分別又は非極性溶剤のヘキサン分別後に極性溶剤で分別するため、乾式分別と極性溶剤での溶剤分別の方式が異なる２種類の分別設備を必要とする、または非極性溶剤と極性溶剤の２種類の溶剤を使う必要があるため、いずれも生産効率に問題のある方法であった。 Patent Document 3 is a method of removing DHS-TG by subjecting monkey fat to dry fractionation or hexane fractionation of a nonpolar solvent, and subjecting the obtained liquid part to solvent fractionation with 100 to 900% by weight of polar solvent with respect to the liquid part. There are two types of separation equipment that differ in the methods of dry fractionation and solvent separation with polar solvents after separation by dry separation or hexane separation of nonpolar solvent, or nonpolar solvent and polar solvent Therefore, both of these methods were problematic in production efficiency.
上記の特許文献１〜３には、いずれもＤＨＳ−ＴＧの低減方法が記載されているが、カカオ代用脂の品質に同様に影響するジグリセリド（以下ＤＧ）、非対称型トリグリセリド（以下ＳＳＵ）画分の低減には言及していない。 The above Patent Documents 1 to 3 all describe methods for reducing DHS-TG, but the diglyceride (hereinafter referred to as DG) and asymmetric triglyceride (hereinafter referred to as SSU) fractions that similarly affect the quality of cacao substitute fat. It does not mention the reduction of.
特許文献４には、テンパリング阻害成分のひとつであるＳＳＵ画分を低減したカカオ代用脂が開示されており、高品質のカカオ代用脂を得るにはＳＳＵ画分の低減も重要である。 Patent Document 4 discloses a cacao substitute fat in which the SSU fraction, which is one of the tempering inhibiting components, is reduced. In order to obtain a high-quality cacao substitute fat, the reduction of the SSU fraction is also important.
上記文献から、高品質のサル脂分別油を得るにはＤＨＳ−ＴＧに限らず、ＤＧ、ＳＳＵ画分も併せて低減する必要があるが、従来の技術で低品質サル脂からかかる成分を効率的にしかも品質的に許容できる範囲まで低減するには限界があった。
従って、本発明の目的は、低品質のサル脂を原料として、高品質のカカオ代用脂として使用することができるようなＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分が十分に低減されたＳＵＳ含有量に富むサル脂分別油の製造法およびその分別油を提供することである。 Therefore, the object of the present invention is to provide a SUS content with sufficiently reduced DHS-TG, DG, and SSU fractions that can be used as a high-quality cocoa substitute fat using low-quality monkey fat as a raw material. It is to provide a method for producing a rich fraction of monkey oil and its fractionated oil.
本発明者らは、ＤＨＳ−ＴＧを低減すると同時に、ＤＧ、ＳＳＵ画分も併せて低減する方法を鋭意検討した結果、サル脂を精製し、極性溶剤を用いて分別するに際し、結晶化させるための晶析工程と晶析・ロ過後の結晶部の洗浄工程で用いる極性溶剤の総量を、サル脂精製油に対し１０００重量％以上とすることで、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分を除去、低減するとともにＳＵＳ含有量に富む結晶部を得ることにより、目的とする高品質のカカオ代用脂が得られることを見出し、本発明を完成した。 The inventors of the present invention have intensively studied a method for reducing DHS-TG and at the same time reducing DG and SSU fractions together. As a result, monkey fat is purified and crystallized when fractionated using a polar solvent. DHS-TG, DG, and SSU fractions are removed by setting the total amount of polar solvent used in the crystallization process and the washing process of the crystal part after crystallization and filtration to 1000% by weight or more with respect to refined monkey oil. It was found that the desired high-quality cacao substitute fat was obtained by obtaining a crystal part which was reduced and rich in SUS content, and the present invention was completed.
本発明は上記知見に基づいてなされたもので、本発明の第１は、サル脂を精製し、極性溶剤を用いて晶析及び結晶部の洗浄を行い、結晶部をハードバター成分として得る方法であって、当該晶析及び洗浄に用いる極性溶剤の総量がサル脂精製油１００重量％に対し１１００〜２１００重量％であることを特徴とし、ハードバター成分中のジヒドロキシステアリン酸を構成脂肪酸として含有するトリグリセリド」（ＤＨＳ−ＴＧ）含有量が０．４重量％以下、ジグリセリド（ＤＧ）含有量が０．５重量％以下、１，２ジ飽和−３不飽和トリグリセリド（ＳＳＵ）画分含有量が２重量％以下である、サル脂分別油の製造法である。第２は、ハードバター成分中の１，３ジ飽和−２不飽和トリグリセリド（ＳＵＳ）含有量が８５重量％以上である第１記載のサル脂分別油の製造法である。第３は、極性溶剤を用いて分別し、得られた結晶部を用いて再分別して結晶部をハードバター成分として得る第１または第２のサル脂分別油の製造法である。
The present invention has been made on the basis of the above findings. The first of the present invention is a method of purifying monkey fat, crystallization and washing of the crystal part using a polar solvent, and obtaining the crystal part as a hard butter component The total amount of the polar solvent used for the crystallization and washing is 1100 to 2100% by weight with respect to 100% by weight of the refined monkey fat, and contains dihydroxystearic acid in the hard butter component as a constituent fatty acid. "Triglyceride" (DHS-TG) content is 0.4 wt% or less, diglyceride (DG) content is 0.5 wt% or less, 1,2 di-saturated-3 unsaturated triglyceride (SSU) fraction content is This is a method for producing a sebum fraction oil that is 2% by weight or less. The second is a method for producing a sal fat fractionated oil according to the first aspect, wherein the content of 1,3 di-saturated-2 unsaturated triglyceride (SUS) in the hard butter component is 85% by weight or more. The third is a method for producing the first or second oil for fractionation of monkey fat, which is fractionated using a polar solvent and is re-fractionated using the obtained crystal part to obtain the crystal part as a hard butter component.
低品質のサル脂を原料として高品質のカカオ代用脂を得る方法を提供するものであり、該方法により品質の振れの大きい原料油脂であるサル脂をカカオ代用脂の原料として安定して使用することを可能とするものである。 The present invention provides a method for obtaining a high-quality cacao substitute fat using low-quality monkey fat as a raw material, and uses the monkey fat, which is a raw material fat with high quality fluctuation, as a raw material for cacao substitute fat. It is possible to do that.
以下、本発明のサル脂分別油の製造方法について説明する。本発明のサル脂分別油の製造方法は、ショリアロブスタの種子から抽出した原油を精製し、精製サル脂を極性溶剤を用いて分別するに際し、結晶化させるための晶析工程と晶析・ロ過後の結晶部の洗浄工程で用いる極性溶剤の総量を、サル脂精製油に対し１０００重量％以上とすることにより、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分を低減させるとともにＳＵＳ含有量が８５重量％以上の結晶部を得ることを特徴とする。 Hereafter, the manufacturing method of the monkey oil fractionation oil of this invention is demonstrated. The method for producing a sebum fraction oil according to the present invention includes a crystallization step and a crystallization step for refining crude oil extracted from Shoria robusta seeds, and crystallizing the refined safat using a polar solvent. The total amount of polar solvent used in the washing step of the crystal part after filtration is 1000% by weight or more with respect to the refined monkey fat, thereby reducing the DHS-TG, DG and SSU fractions and the SUS content is 85%. % Or more of the crystal part is obtained.
サル脂原油の精製方法は一般的な方法であればよく、例えばサル脂原油に対して好ましくは０．１〜０．４重量％のリン酸を添加して脱ガム、アルカリによる脱酸、脱酸後の湯洗、減圧脱水、漂白、脱臭を行うのが一般的である。原油の品質によっては、かかる工程の一部を省略することができるが、低品質のサル脂原油の場合は脱ガム、アルカリによる脱酸、湯洗及び減圧脱水が必須で、かかる工程で処理することにより、原油中に含まれるＤＧ，ＥＰ−ＴＧ，ＤＨＳ−ＴＧを部分的に低減することができる。かかる工程なしでは、ＤＧ，ＥＰ−ＴＧ，ＤＨＳ−ＴＧの含有量が多すぎて、後の溶剤分別によってかかる成分を許容範囲まで低減することが困難となる。 The refining method of the sal fat crude oil may be a general method. For example, 0.1 to 0.4% by weight of phosphoric acid is preferably added to the sal fat crude oil for degumming, deoxidation with alkali, desorption. In general, washing with hot water after acid, dehydration under reduced pressure, bleaching, and deodorization are performed. Depending on the quality of the crude oil, part of this process can be omitted, but in the case of low-quality monkey oil crude oil, degumming, alkali deoxidation, hot water washing and dehydration under reduced pressure are essential. Thereby, DG, EP-TG, and DHS-TG contained in crude oil can be partially reduced. Without such a process, the content of DG, EP-TG, and DHS-TG is too high, and it becomes difficult to reduce such components to an acceptable range by subsequent solvent fractionation.
また、脱臭工程での脱臭条件も重要で、脱臭温度としては２３０〜２６０℃、好ましくは２３０〜２５０℃、最も好ましくは２３０〜２４０℃、脱臭時の真空度は５Ｔｏｒｒ以下、望ましくは２Ｔｏｒｒ以下が好ましい。脱臭温度が２５０℃を超えると、脱臭工程中にＳＵＳ画分の部分的な異性化が起こり、ＳＳＵ画分が生成する傾向にあり、好ましくない。また、脱臭温度が２３０℃未満である場合や真空度が５Ｔｏｒｒを超える場合は、油脂中の遊離脂肪酸の除去が不十分となるため好ましくない。 Deodorizing conditions in the deodorizing step are also important. The deodorizing temperature is 230 to 260 ° C., preferably 230 to 250 ° C., most preferably 230 to 240 ° C., and the degree of vacuum at the time of deodorizing is 5 Torr or less, desirably 2 Torr or less. preferable. When the deodorization temperature exceeds 250 ° C., partial isomerization of the SUS fraction occurs during the deodorization step, and an SSU fraction tends to be generated, which is not preferable. Moreover, when the deodorizing temperature is less than 230 ° C. or when the degree of vacuum exceeds 5 Torr, removal of free fatty acids in the oil and fat is not preferable.
低品質サル脂原油の場合は、既述のようにＤＨＳ−ＴＧを２〜１０重量％含み、上記のような方法で精製してもＤＨＳ−ＴＧが１〜４重量％残存し、ＤＧ、ＳＳＵ画分も許容できない範囲で含有するため、良質のハードバター成分とは言えない。かかる場合は、以下の本発明の方法で溶剤分別を行う必要がある。 In the case of low-quality monkey fat crude oil, it contains 2 to 10% by weight of DHS-TG as described above, and 1 to 4% by weight of DHS-TG remains even after refining by the above method. Since the fraction is contained in an unacceptable range, it cannot be said to be a good-quality hard butter component. In such a case, it is necessary to carry out solvent fractionation by the following method of the present invention.
５０〜７０℃に加熱し完全融解した精製サル脂に対し４００重量％以上、好ましくは４００〜３０００重量％の極性溶剤を混合し、冷媒による冷却装置及び攪拌装置の付いた晶析槽内で撹拌しながら０〜２０℃まで徐々に冷却する。晶析時間は、冷媒温度と極性溶剤の種類によって異なるが、 ０．５〜３時間程度である。晶析終了後、減圧ロ過などにより結晶部とロ液部にロ別する。ロ別した結晶部は、予め晶析温度〜晶析温度より１０℃低い温度まで冷却した新鮮な極性溶剤を分別原料油脂に対し、晶析工程と洗浄工程で用いる極性溶剤総量が１０００重量％以上となる量、好ましくは０〜２６００重量％混合して洗浄し、再度結晶部とロ液部にロ別する。こうして得られた結晶部は、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分が低減されＳＵＳ成分が濃縮されている。上記の晶析に用いる極性溶剤と洗浄に用いる極性溶剤の総量は、１０００重量％以上、好ましくは１０００〜３０００重量％、最も好ましくは１１００〜２１００重量％である。下限未満であると、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分の低減が不十分であり、上限を超えると極性溶剤の使用量が多すぎて分別の生産効率が低下するとともに分別後の脱溶剤工程での蒸留負荷が大きくなりすぎるため、いずれも好ましくない。 400 wt% or more, preferably 400 to 3000 wt% of a polar solvent is mixed with purified monkey fat heated to 50 to 70 ° C and completely melted, and stirred in a crystallization tank equipped with a cooling device and a stirring device using a refrigerant. While cooling, gradually cool to 0-20 ° C. The crystallization time varies depending on the refrigerant temperature and the type of polar solvent, but is about 0.5 to 3 hours. After crystallization is completed, the crystal part and the liquid part are separated by vacuum filtration or the like. The separated crystal part is a total of 1000% by weight or more of the polar solvent used in the crystallization step and the washing step with respect to the raw material oil separated from a fresh polar solvent that has been cooled to a temperature 10 ° C. lower than the crystallization temperature in advance. Then, the mixture is washed by mixing in an amount of 0 to 2600% by weight, and again separated into a crystal part and a liquid part. In the crystal part thus obtained, the DHS-TG, DG, and SSU fractions are reduced and the SUS component is concentrated. The total amount of the polar solvent used for crystallization and the polar solvent used for washing is 1000% by weight or more, preferably 1000 to 3000% by weight, and most preferably 1100 to 2100% by weight. If it is less than the lower limit, the reduction of DHS-TG, DG, and SSU fractions is insufficient, and if the upper limit is exceeded, the amount of polar solvent used is too much and the separation production efficiency decreases and the solvent removal step after the separation Neither of these is preferable because the distillation load in the tank becomes too large.
上記のサル脂精製油に対する極性溶剤総量を１０００重量％以上とする、サル脂精製油の分別法は大別して下記１）、２）の２通りの方法が適用できるが、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分のより効率的な低減には前者の方法が好適に利用できる。 The method for fractionating purified sal fat oil with the total amount of polar solvent based on the above refined fat oil being 1000% by weight or more can be broadly divided into the following two methods 1) and 2), but DHS-TG, DG, The former method can be suitably used for more efficient reduction of the SSU fraction.
１） ５０〜７０℃に加熱し完全融解した精製サル脂に対し４００〜９００重量％の極性溶剤を混合し、冷媒による冷却装置及び攪拌装置の付いた晶析槽内で撹拌しながら０〜２０℃まで徐々に冷却する。晶析終了後、減圧ロ過などにより結晶部とロ液部にロ別する。ロ別した結晶部は、予め晶析温度〜晶析温度より１０℃低い温度まで冷却した新鮮な極性溶剤を分別原料油脂に対し１００〜６００重量％混合して洗浄し、再度結晶部とロ液部にロ別する。こうして得られた結晶部を常法通り脱溶剤して得た結晶画分は、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分が低減されているが、低品質の精製サル脂の分別ではこの段階ではかかる成分の低減が不十分であり、さらに次の再分別に供する。 1) 400 to 900% by weight of a polar solvent is mixed with refined monkey fat heated to 50 to 70 ° C. and completely melted, and 0 to 20 with stirring in a crystallization tank equipped with a cooling device and a stirring device using a refrigerant. Cool gradually to ° C. After crystallization is completed, the crystal part and the liquid part are separated by vacuum filtration or the like. The separated crystal part is washed by mixing 100 to 600% by weight of a fresh polar solvent, which has been cooled to a temperature 10 ° C. lower than the crystallization temperature in advance, with respect to the fractionated raw oil and fat. Separated into parts. In the crystal fraction obtained by removing the solvent from the crystal part obtained in the usual manner, the DHS-TG, DG, and SSU fractions are reduced. Insufficient reduction of components, and further subjected to the next re-fractionation.
上記で得られた結晶画分を５０〜７０℃に加熱し完全に融解してから、該結晶画分に対し４００〜９００重量％の極性溶剤を混合し、冷媒による冷却装置及び攪拌装置の付いた晶析槽内で撹拌しながら０〜２０℃まで徐々に冷却する。晶析終了後、減圧ロ過などにより結晶部とロ液部にロ別する。ロ別した結晶部は、予め晶析温度〜晶析温度より１０℃低い温度まで冷却した新鮮な極性溶剤を分別原料油脂に対し１００〜６００重量％混合して洗浄し、再度結晶部とロ液部にロ別する。晶析終了後、減圧ロ過などにより結晶部とロ液部にロ別する。この再分別により得られた結晶部は、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分がさらに一段と低減されＳＵＳ成分もさらに濃縮されており、常法通り脱溶剤、精製して高品質のカカオ代用脂になりうるものである。なお、この再分別に供する結晶部は１段目の分別で得られた極性溶剤を含むものでも差し支えなく、その場合は３０〜５０℃に加熱し完全融解してから極性溶剤と混合して、分別すればよい。 The crystal fraction obtained above is heated to 50 to 70 ° C. and completely melted, and then 400 to 900% by weight of a polar solvent is mixed with the crystal fraction, and a cooling device and a stirring device with a refrigerant are attached. The mixture is gradually cooled to 0 to 20 ° C. with stirring in the crystallization tank. After crystallization is completed, the crystal part and the liquid part are separated by vacuum filtration or the like. The separated crystal part is washed by mixing 100 to 600% by weight of a fresh polar solvent, which has been cooled to a temperature 10 ° C. lower than the crystallization temperature in advance, with respect to the fractionated raw oil and fat. Separated into parts. After crystallization is completed, the crystal part and the liquid part are separated by vacuum filtration or the like. In the crystal part obtained by this re-fractionation, the DHS-TG, DG, and SSU fractions are further reduced and the SUS component is further concentrated. Solvent removal and purification are performed as usual to obtain high-quality cocoa substitute fat. It can be. In addition, the crystal part to be subjected to this re-fractionation may contain the polar solvent obtained in the first-stage fractionation, in which case it is heated to 30 to 50 ° C. and completely melted and then mixed with the polar solvent, What is necessary is just to separate.
上記の２段階の分別で用いる極性溶剤の総量が、サル脂精製油に対して１０００重量％以上とするのが
ＤＨＳ−ＴＧ，ＤＧ，ＳＳＵ画分を許容範囲内に低減するために重要である。
In order to reduce the DHS-TG, DG, and SSU fractions within an allowable range, it is important that the total amount of the polar solvent used in the above two-stage fractionation is 1000% by weight or more based on the refined monkey fat. .
上記の２段階の分別法ではなく、１段階の分別法の場合は下記の手順を適用することができる。
２） ５０〜７０℃に加熱し完全融解した精製サル脂に対し４００〜３０００重量％の極性溶剤を混合し、冷媒による冷却装置及び攪拌装置の付いた晶析槽内で撹拌しながら０〜２０℃まで徐々に冷却する。晶析終了後、減圧ロ過などにより結晶部とロ液部にロ別する。ロ別した結晶部は、予め晶析温度〜晶析温度より１０℃低い温度まで冷却した新鮮な極性溶剤を分別原料油脂に対し０〜２６００重量％混合して洗浄し、再度結晶部とロ液部にロ別する。上記の晶析及び結晶部の洗浄に用いる極性溶剤の総量は、やはりサル脂精製油に対して１０００重量％以上とする必要がある。得られた結晶部から常法通り脱溶剤、精製して得られる結晶画分は、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分が十分に低減され、ＳＵＳ成分も十分に濃縮されており、高品質のカカオ代用脂になりうるものである。
In the case of a one-stage fractionation method instead of the above-described two-stage fractionation method, the following procedure can be applied.
2) 400 to 3000% by weight of a polar solvent is mixed with purified monkey fat heated to 50 to 70 ° C. and completely melted, and 0 to 20 while stirring in a crystallization tank equipped with a cooling device and a stirring device using a refrigerant. Cool gradually to ° C. After crystallization is completed, the crystal part and the liquid part are separated by vacuum filtration or the like. The separated crystal part is washed by mixing 0 to 2600% by weight of a fresh polar solvent, which has been cooled to a temperature lower than the crystallization temperature by 10 ° C. in advance, with respect to the fractionated raw material fat. Separated into parts. The total amount of the polar solvent used for the crystallization and washing of the crystal part needs to be 1000% by weight or more based on the refined monkey fat. The crystal fraction obtained by solvent removal and purification from the obtained crystal part as usual, DHS-TG, DG, SSU fraction is sufficiently reduced, SUS component is also sufficiently concentrated, high quality It can be used as a cacao substitute fat.
本発明に用いる極性溶剤としてはアセトン、メチルエチルケトン、ジエチルケトン、エチルアルコール、n‐ブチルアルコール等が例示できる。なかでもアセトンが好適に利用できる。なお、極性溶剤中の水分は２重量％以下、好ましくは１重量％以下であるのが望ましい。水分が２重量％を超えると、油脂の溶解度が低下して溶剤に対する油脂分を高くすることが困難となるので好ましくない。 Examples of the polar solvent used in the present invention include acetone, methyl ethyl ketone, diethyl ketone, ethyl alcohol, and n-butyl alcohol. Of these, acetone can be preferably used. The water content in the polar solvent is 2% by weight or less, preferably 1% by weight or less. If the water content exceeds 2% by weight, the solubility of fats and oils decreases and it becomes difficult to increase the fats and oils content in the solvent.
本発明の、サル脂精製油に対して１０００重量％以上の極性溶剤を用いて分別して得られるサル脂分別油は、ＤＨＳ−ＴＧ含有量が０．４重量％以下、ＤＧ含有量が０．５重量％以下、ＳＳＵ画分含有量２重量％以下であるのが好ましい。 In the present invention, the oil for fractionated sal fat obtained by fractionating 1000% by weight or more of the refined oil for fat with fat has a DHS-TG content of 0.4% by weight or less and a content of DG of 0. The content is preferably 5% by weight or less and the SSU fraction content is 2% by weight or less.
本発明で得られるサル脂分別油のＤＨＳ−ＴＧ含有量は、上記のように０．４重量％以下、好ましくは０．３重量％以下、さらに好ましくは０．２重量％以下である。ＤＨＳ−ＴＧが０．４重量％を超えると、チョコレートに使用したとき、テンパリング工程でのチョコレート生地粘度上昇が顕著になり、チョコレート型流し、冷却後の型離れが低下するため好ましくない。 As described above, the DHS-TG content of the oil for fractionated monkey fat obtained in the present invention is 0.4% by weight or less, preferably 0.3% by weight or less, and more preferably 0.2% by weight or less. When DHS-TG exceeds 0.4% by weight, when used for chocolate, the increase in the chocolate dough viscosity in the tempering step becomes significant, and the chocolate mold flows and the mold release after cooling decreases, which is not preferable.
なお、本発明で得られるサル脂分別油に含まれるＤＨＳ−ＴＧは、９，１０−ジヒドロキシステアロイル−ジステアリン（ＳｔＤＳｔ）、９，１０−ジヒドロキシステアロイル−ステアロイル−アラキジン（ＳｔＤＡ）、９，１０−ジヒドロキシステアロイル−ステアロイル−パルミチン（ＳｔＤＰ）の３成分からなり、かかる３成分の合計量が０．４重量％以下であるが、好ましくはＳｔＤＳｔ含有量が０．２重量％以下、ＳｔＤＡ含有量が０．１重量％以下、ＳｔＤＰ含有量が０．１重量％以下である。 In addition, DHS-TG contained in the sebum fraction oil obtained in the present invention is 9,10-dihydroxystearoyl-distearin (StDSt), 9,10-dihydroxystearoyl-stearoyl-arachidine (StDA), 9,10-dihydroxy. It is composed of three components, stearoyl-stearoyl-palmitin (StDP), and the total amount of these three components is 0.4% by weight or less. Preferably, the StDSt content is 0.2% by weight or less, and the StDA content is 0.00. 1 wt% or less, and StDP content is 0.1 wt% or less.
また、ＤＧ含有量もさらに好ましくは０．２重量％以下であり、０．５重量％を超えると、やはりチョコレートのテンパリング工程でのチョコレート生地粘度上昇が顕著になり、チョコレート型流し、冷却後の型離れが低下するため好ましくない。 In addition, the DG content is more preferably 0.2% by weight or less, and if it exceeds 0.5% by weight, the increase in the chocolate dough viscosity in the tempering process of chocolate becomes remarkable, the chocolate mold flows, and after cooling This is not preferable because mold release is reduced.
さらに、ＳＳＵ画分含有量も２重量％を超えると、同様に油脂の結晶性が低下するためチョコレートテンパリング作業性が低下し、耐熱保型性やスナップ性、口溶けの低下が生じるため好ましくない。 Furthermore, if the SSU fraction content exceeds 2% by weight, the crystallinity of the oil and fat is similarly lowered, so that the chocolate tempering workability is lowered, and the heat-resistant shape retention, snapping property, and melting in the mouth are lowered, which is not preferable.
本発明の、サル脂精製油に対して１０００重量％以上の極性溶剤を用いて分別して得られるサル脂分別油は、ＳＵＳ含有量が８５重量％以上であるのが好ましい。ＳＵＳ含有量が８５重量％未満であると、サル脂分別油を使用したチョコレートのスナップ性や耐熱保型性が低下し、シャープな口溶けが得られなくなるので好ましくない。 In the present invention, it is preferable that the fraction obtained by fractionation of the sal fat refined oil using a polar solvent of 1000% by weight or more has a SUS content of 85% by weight or more. If the SUS content is less than 85% by weight, the snapping property and heat-resisting shape retention property of chocolate using the sebum fraction oil will be lowered, and it will not be possible to obtain a sharp mouth melt, which is not preferable.
本発明で得られるサル脂分別油をカカオ代用脂として使用する場合、サル脂分別油のみでもカカオバター代用脂として使用可能であるが、カカオ脂、パーム脂、イリッペ油、シア脂、マンゴ核油、およびこれらの分別油、エステル交換油等の油脂を本発明のサル脂分別油に配合しても良い。
また、本発明のサル脂分別油はカカオ代用脂としてチョコレートに使用する以外にも製菓製パン用、カレー等のルー用、フライ用等の油脂として使用可能である。
When using the sebum fraction oil obtained in the present invention as a cacao substitute oil, it can be used as a cacao butter substitute oil alone, but cacao fat, palm fat, iripe oil, shea fat, mango kernel oil And oils such as these fractionated oils and transesterified oils may be blended in the monkey fat fractionated oil of the present invention.
Moreover, the oil for fractionation of monkey fat of the present invention can be used as fats and oils for confectionery bread, curry and other frying, frying, etc. in addition to being used for chocolate as a cacao substitute fat.
以下に実施例および比較例を挙げて本発明を詳細に説明する。なお、以下の例中、特に断りのない限り、「％」は「重量％」を意味する。 Hereinafter, the present invention will be described in detail with reference to Examples and Comparative Examples. In the following examples, “%” means “% by weight” unless otherwise specified.
＜実施例１＞
ショリアロブスタの種子から得られたサル脂原油（ＤＨＳ−ＴＧ５．２％含有）に対して、リン酸を０．２％添加して脱ガムした。脱ガム油を常法通り、アルカリ脱酸し、次いで常法通り白土を使用した 漂白処理と脱臭処理（脱臭温度２５０〜２６０℃、真空度２Ｔｏｒｒ以下）を行い、精製サル脂を得た。得られた精製サル脂は、高速液体クロマトグラフィー（ＨＰＬＣ）で分析した結果、ＤＨＳ−ＴＧ２．３％，ＤＧ３．３ ％、ＳＵＳ画分６２．０％を含有していた。また、薄層クロマトグラフィー（ＴＬＣ）展開法で分析した結果、ＳＳＵ画分含有量は３．８％であった。
<Example 1>
To monkey oil crude oil (containing DHS-TG 5.2%) obtained from Shoria robusta seeds, 0.2% of phosphoric acid was added and degummed. The degummed oil was subjected to alkaline deoxidation as usual, and then subjected to bleaching treatment and deodorization treatment using a white clay (deodorization temperature 250 to 260 ° C., vacuum degree 2 Torr or less) as usual to obtain purified monkey fat. As a result of analysis by high performance liquid chromatography (HPLC), the obtained purified monkey fat contained DHS-TG 2.3%, DG 3.3%, and SUS fraction 62.0%. Moreover, as a result of analyzing by the thin layer chromatography (TLC) expansion | deployment method, SSU fraction content was 3.8%.
この精製サル脂を６０℃に加熱し完全融解し、精製サル脂に対し５６７重量％のアセトン（水分０．９％）を混合した。混合液を４０℃に調温してから、撹拌しながら２℃／分で１３℃まで冷却し、１３±０．５℃で０．５時間、撹拌して晶析させた。そして減圧下吸引ロ過して結晶部とロ液部に分離した。結晶部を１０℃に冷却した原料油脂の２００重量％の新鮮なアセトンで洗浄し、再度減圧下吸引ロ過して結晶部とロ液部に分離した。洗浄ロ液は先に分離したロ液部に加えた。得られた結晶部、ロ液部を脱溶剤した 。結晶部から得られた結晶画分の収率は６２．８％、ロ液部から得られたロ液画分の収率は３７．２％であった。この結晶画分は、ＨＰＬＣで分析した結果、ＤＨＳ−ＴＧ１．８％（ＳｔＤＳｔ：１．０％、ＳｔＤＡ：０．５％、ＳｔＤＰ：０．３％）、ＤＧ１．３％、ＳＵＳ画分８２．６％を含有していた。ＴＬＣ展開法で分析した結果、ＳＳＵ画分含有量は２．２％であった。
This purified monkey fat was heated to 60 ° C. and completely melted, and 567 wt% acetone (water content 0.9%) was mixed with the purified monkey fat. After the temperature of the mixture was adjusted to 40 ° C., the mixture was cooled to 13 ° C. at 2 ° C./min with stirring and crystallized by stirring at 13 ± 0.5 ° C. for 0.5 hour. Then, suction filtration was performed under reduced pressure to separate the crystal part and the liquid part. The crystal part was washed with 200% by weight fresh acetone of raw oil and fat cooled to 10 ° C., and suction filtered again under reduced pressure to separate the crystal part and the liquid part. The washing solution was added to the previously separated solution. The obtained crystal part and the filtrate part were desolvated. The yield of the crystal fraction obtained from the crystal part was 62.8%, and the yield of the filtrate fraction obtained from the filtrate part was 37.2%. As a result of analyzing by HPLC, this crystal fraction was found to be DHS-TG 1.8% (StDSt: 1.0%, StDA: 0.5%, StDP: 0.3%), DG1.3%, SUS fraction 82. Contained 6%. As a result of analysis by the TLC development method, the SSU fraction content was 2.2%.
続いて、上記で得られた結晶画分を６０℃に加熱し完全融解し、その結晶画分に対しアセトン（水分０．９％）５６７重量％（対原料油脂３５６重量％）を混合した。混合液を４０℃に調温してから、撹拌しながら２℃／分で１８℃まで冷却し、１８±０．５℃で０．５時間、撹拌して晶析させた。そして減圧下吸引ロ過して結晶部とロ液部に分離した。結晶部を１５℃に冷却 した対結晶画分２００重量％（対原料油脂１２６重量％）の新鮮なアセトンで洗浄し、再度減圧下吸引ロ過して結晶部とロ液部に分離した。洗浄ロ液は先に分離したロ液部に加えた。得られた結晶部、ロ液部を脱溶剤した。結晶部から得られた結晶画分の収率は対分別原料油脂で４２．７％、ロ液部から得られたロ液画分の収率は対分別原料油脂で２０．１％であった。 Subsequently, the crystal fraction obtained above was heated to 60 ° C. and completely melted, and 567% by weight of acetone (water content 0.9%) (based on raw material fat / oil 356% by weight) was mixed with the crystal fraction. After the temperature of the mixture was adjusted to 40 ° C., the mixture was cooled to 18 ° C. at 2 ° C./min with stirring, and stirred for crystallization for 0.5 hours at 18 ± 0.5 ° C. Then, suction filtration was performed under reduced pressure to separate the crystal part and the liquid part. The crystal part was cooled to 15 ° C., washed with fresh acetone of 200% by weight of the fraction of the crystal (126% by weight of the raw material fat), and again filtered under reduced pressure to separate the crystal part and the liquid part. The washing solution was added to the previously separated solution. The obtained crystal part and filtrate part were desolvated. The yield of the crystal fraction obtained from the crystal part was 42.7% with respect to the fractionated raw material oil and fat, and the yield of the filtrate fraction obtained from the filtrate part was 20.1% with respect to the fractionated raw material fat. .
再分別により得られたサル脂分別油は、ＨＰＬＣで分析した結果、ＤＨＳ−ＴＧ０．２％（ＳｔＤＳｔ：０．２％、ＳｔＤＡ：０．０％、ＳｔＤＰ：０．０％）、ＤＧ０ ．０％、ＳＵＳ含有量９３．２％を含有していた。ＴＬＣ展開法で分析した結果、ＳＳＵ画分含有量は１．４％であった。 As a result of HPLC analysis, the fractionated monkey oil obtained by re-fractionation was found to have DHS-TG 0.2% (StDSt: 0.2%, StDA: 0.0%, StDP: 0.0%), DG0. It contained 0% and a SUS content of 93.2%. As a result of analysis by the TLC development method, the SSU fraction content was 1.4%.
＜実施例２＞
実施例１で調製した精製サル脂を６０℃に加熱し完全融解し、精製サル脂に対し５６７重量部とアセトン（水分０．９％）を混合した。混合液を４０℃に調温してから、撹拌しながら２℃／分で１３℃まで冷却し、１３±０．５℃で０．５時間、撹拌して晶析させた。そして減圧下吸引ロ過して結晶部とロ液部に分離した。結晶部を１３℃に冷却 した原料油脂の７６７重量％の新鮮なアセトンで洗浄し、再度減圧下吸引ロ過して結晶部とロ液部に分離した。洗浄ロ液は先に分離したロ液部に加えた。得られた結晶部、ロ液部を脱溶剤した。結晶部の収率は４３．２％、ロ液部の収率は５６．８％であった。
<Example 2>
The purified monkey fat prepared in Example 1 was heated to 60 ° C. and completely melted, and 567 parts by weight and acetone (water content 0.9%) were mixed with the purified monkey fat. After the temperature of the mixture was adjusted to 40 ° C., the mixture was cooled to 13 ° C. at 2 ° C./min with stirring and crystallized by stirring at 13 ± 0.5 ° C. for 0.5 hour. Then, suction filtration was performed under reduced pressure to separate the crystal part and the liquid part. The crystal part was washed with 767% by weight fresh acetone of the raw oil and fat cooled to 13 ° C., and again suctioned under reduced pressure to separate the crystal part and the liquid part. The washing solution was added to the previously separated solution. The obtained crystal part and filtrate part were desolvated. The yield of the crystal part was 43.2%, and the yield of the filtrate part was 56.8%.
得られたサル脂分別油は、ＨＰＬＣで分析した結果、ＤＨＳ−ＴＧ０．３％（ＳｔＤＳｔ：０．２％、ＳｔＤＡ：０．０％、ＳｔＤＰ：０．１％）、ＤＧ０ ．０％、ＳＵＳ含有量９２．５％を含有していた。ＴＬＣ展開法で分析した結果、ＳＳＵ画分含有量は１．８％であった。 As a result of analyzing by HPLC, the obtained oil fraction for monkey fat was DHS-TG 0.3% (StDSt: 0.2%, StDA: 0.0%, StDP: 0.1%), DG0. It contained 0% and a SUS content of 92.5%. As a result of analysis by the TLC development method, the SSU fraction content was 1.8%.
＜実施例３＞
実施例１で調製した精製サル脂を６０℃に加熱し完全融解し、精製サル脂に対し１２３３重量％のアセトン（水分０．９％）を混合した。混合液を４０℃に調温してから、撹拌しながら２℃／分で１０℃まで冷却し、１０±０．５℃で０．５時間、撹拌して晶析させた。そして減圧下吸引ロ過して結晶部とロ液部に分離した。結晶部を７℃に冷却した原料油脂の２００重量％の新鮮なアセトンで洗浄し、再度減圧下吸引ロ過して結晶部とロ液部に分離した。洗浄ロ液は先に分離したロ液部に加えた。得られた結晶部、ロ液部を脱溶剤した。結晶部の収率は４２．２％、ロ液部の収率は５７．８％であった。
<Example 3>
The purified monkey fat prepared in Example 1 was heated to 60 ° C. and completely melted, and 1233 wt% acetone (water content 0.9%) was mixed with the purified monkey fat. After the temperature of the mixture was adjusted to 40 ° C., the mixture was cooled to 10 ° C. at 2 ° C./min with stirring, and stirred at 10 ± 0.5 ° C. for 0.5 hour for crystallization. Then, suction filtration was performed under reduced pressure to separate the crystal part and the liquid part. The crystal part was washed with 200% by weight fresh acetone of raw oil and fat cooled to 7 ° C., and suction filtered again under reduced pressure to separate the crystal part and the liquid part. The washing solution was added to the previously separated solution. The obtained crystal part and filtrate part were desolvated. The yield of the crystal part was 42.2%, and the yield of the filtrate part was 57.8%.
得られたサル脂分別油は、ＨＰＬＣで分析した結果、ＤＨＳ−ＴＧ０．３％（ＳｔＤＳｔ：０．２％、ＳｔＤＡ：０．０％、ＳｔＤＰ：０．１％）、ＤＧ０ ．０％、ＳＵＳ含有量９３．８％を含有していた。ＴＬＣ展開法で分析した結果、ＳＳＵ画分含有量は１．７％であった。 As a result of analyzing by HPLC, the obtained oil fraction for monkey fat was DHS-TG 0.3% (StDSt: 0.2%, StDA: 0.0%, StDP: 0.1%), DG0. It contained 0% and a SUS content of 93.8%. As a result of analysis by the TLC development method, the SSU fraction content was 1.7%.
＜比較例１＞
実施例１で調製した精製サル脂を６０℃に加熱し完全融解し、精製サル脂に対し５６７重量％のアセトン（水分０．９％）を混合した。混合液を４０℃に調温してから、撹拌しながら２℃／分で１６℃まで冷却し、１６±０．５℃で０．５時間、撹拌して晶析させた。そして減圧下吸引ロ過して結晶部とロ液部に分離した。結晶部を１３℃に冷却した原料油脂の２００重量％２倍重量部の新鮮なアセトンで洗浄し、再度減圧下吸引ロ過して結晶部とロ液部に分離した。洗浄ロ液は先に分離したロ液部に加えた。得られた結晶部、ロ液部を脱溶剤した。結晶部の収率は４８．０％、ロ液部の収率は５２．０％であった。
<Comparative Example 1>
The purified monkey fat prepared in Example 1 was heated to 60 ° C. and completely melted, and 567 wt% acetone (water content 0.9%) was mixed with the purified monkey fat. After the temperature of the mixture was adjusted to 40 ° C., the mixture was cooled to 16 ° C. at 2 ° C./min with stirring, and stirred for crystallization for 0.5 hours at 16 ± 0.5 ° C. Then, suction filtration was performed under reduced pressure to separate the crystal part and the liquid part. The crystal part was washed with 200 parts by weight of fresh acetone that had been cooled to 13 ° C. and 2 parts by weight of fresh acetone, and suctioned again under reduced pressure to separate the crystal part and the liquid part. The washing solution was added to the previously separated solution. The obtained crystal part and filtrate part were desolvated. The yield of the crystal part was 48.0%, and the yield of the filtrate part was 52.0%.
得られたサル脂分別油は、ＨＰＬＣで分析した結果、ＤＨＳ−ＴＧ１．２％（ＳｔＤＳｔ：０．６％、ＳｔＤＡ：０．３％、ＳｔＤＰ：０．３％）、ＤＧ０．９％、ＳＵＳ画分８３．２％を含有していた。ＴＬＣ展開法で分析した結果、ＳＳＵ画分含有量は２．３％であった。 As a result of HPLC analysis, the obtained oil fraction for monkey fat was DHS-TG 1.2% (StDSt: 0.6%, StDA: 0.3%, StDP: 0.3%), DG 0.9%, SUS Contained 83.2% fraction. As a result of analysis by the TLC development method, the SSU fraction content was 2.3%.
精製サル脂、実施例１、比較例１のサル脂分別油のＤＨＳ−ＴＧ含有量、ＳｔＤＳｔ含有量、ＳｔＤＡ含有量、ＳｔＤＰ含有量、ＤＧ含有量、ＳＳＵ画分含有量、固体脂含量の分析結果を表１に示す。なお、これらの測定方法は以下に準ずる。 Analysis of DHS-TG content, StDSt content, StDA content, StDP content, DG content, SSU fraction content, solid fat content of the refined monkey fat, Example 1, comparative oil of monkey fat of Comparative Example 1 The results are shown in Table 1. These measuring methods are based on the following.
＜測定方法＞
（１）ＤＨＳ−ＴＧ含有量、ＳｔＤＳｔ含有量、ＳｔＤＡ含有量、ＳｔＤＰ含有量、ＤＧ含有量：ＨＰＬＣ（カラム：ＯＤＳ−ＡおよびＬｉｃｈｒｏｓｏｒｂ直列２本カラム、溶離液： アセトン／アセトニトリル＝８０／２０、流量：０．９ｍｌ／分、カラム温度：２５℃、検出機：示差屈折計）で測定した。
<Measurement method>
(1) DHS-TG content, StDSt content, StDA content, StDP content, DG content: HPLC (column: ODS-A and Librosorb in-line two columns, eluent: acetone / acetonitrile = 80/20, Flow rate: 0.9 ml / min, column temperature: 25 ° C., detector: differential refractometer).
（２）ＳＳＵ画分含有量：ＴＬＣ展開法（ＴＬＣプレート：ＨＰＴＬＣ−Ｋｉｅｓｅｌｇｅｌ１６０ Ｆ２５４、展開溶媒：ベンゼン／ヘキサン／ジエチルエーテル＝７５／２ ５／２、発色：臭素→塩化スルフリル）で測定した。なお、ＳＳＵ画分含有量は次式で算出したものである。
ＳＳＵ画分含有量（％）＝｛ＳＳＵ画分含有量／（ＳＳＵ画分含有量＋ＳＵＳ画分含有量）｝×１００
(2) SSU fraction content: Measured by TLC development method (TLC plate: HPTLC-Kieselgel 160 F254, developing solvent: benzene / hexane / diethyl ether = 75/2 5/2, color development: bromine → sulfuryl chloride). The SSU fraction content is calculated by the following formula.
SSU fraction content (%) = {SSU fraction content / (SSU fraction content + SUS fraction content)} × 100
（３）固体脂含量：基準油脂分析試験法暫定法１−１９９６、固体脂含量ＮＭＲ法に基づいて測定した。エージングは２６℃／４０時間とした。 (3) Solid fat content: measured based on provisional method 1-196 for standard fat analysis test, solid fat content NMR method. Aging was performed at 26 ° C./40 hours.
（４）融点：基準油脂分析試験法２．２．４．３−１９９６，軟化点（環球法）に基づいて測定した。エージングは２５℃／２４時間とした。 (4) Melting point: Measured based on the standard fat and oil analysis test method 2.2.4.3-1996, softening point (ring ball method). Aging was performed at 25 ° C./24 hours.
＜表１＞
＊ ２段目晶析、２段目洗浄に使用した溶剤量は対２段目分別原料油脂（1段目で得られた結晶部）の量、で対分別原料油脂ではそれぞれ３５６％、１２６％に相当する。
<Table 1>
* The amount of solvent used for second-stage crystallization and second-stage washing is the amount of the second-stage fractionated raw oil and fat (crystal parts obtained in the first stage), and for the fractionated raw-material fat and oil, 356% and 126%, respectively. It corresponds to.
表１にあるように、分別に使用した極性溶剤総使用量が１２００〜１５００重量％であった実施例１〜３は、比較例１に比べて、ＤＨＳ−ＴＧ含有量％、ＤＧ含有量％、ＳＳＵ画分含有量％が低い値を示し、ＳＵＳ含有量は逆に高い値を示す。そのため実施例１〜３は、比較例１との対比で、固体脂含量、融点とも高く、明らかに高品質のカカオ代用脂になりうるものであった。比較例１は、ＤＨＳ−ＴＧ、ＤＧ、ＳＳＵ画分のいずれも十分に低減されておらず、ＳＵＳ含有量もやや低いものであり、良質のカカオ代用脂になりうるものではなかった。 As shown in Table 1, Examples 1 to 3, in which the total amount of polar solvents used separately were 1200 to 1500% by weight, compared to Comparative Example 1, were DHS-TG content% and DG content%. , SSU fraction content% shows a low value, SUS content shows a high value on the contrary. Therefore, Examples 1-3 were high in solid fat content and melting point in comparison with Comparative Example 1, and could obviously be high-quality cocoa substitute fats. In Comparative Example 1, none of the DHS-TG, DG, and SSU fractions were sufficiently reduced, the SUS content was slightly low, and it could not be a high-quality cocoa substitute fat.
＜実施例４＞
実施例１で得たサル脂分別油４７重量部と、常法で調整したパーム中融点部油（ヨウ素価３４．５、融点３１．６℃、ＰＯＰ含有量６８．０％）５３重量部を配合してカカオ脂近似のカカオ代用脂を調製し、冷却曲線、固体脂含量、融点を測定し、カカオ代用脂としての機能を評価した。
<Example 4>
47 parts by weight of the oil for fractionation of monkey fat obtained in Example 1 and 53 parts by weight of oil having a middle melting point of palm oil (iodine value 34.5, melting point 31.6 ° C., POP content 68.0%) prepared by a conventional method A cacao substitute fat similar to cacao fat was prepared by blending, and the cooling curve, solid fat content and melting point were measured, and the function as a cacao substitute fat was evaluated.
＜比較例２＞
比較例１で得たサル脂分別油４７重量部と、常法で調整したパーム中融点部油（ヨウ素価３４．５、融点３１．６℃、ＰＯＰ含有量６８．０％）５３重量部を配合してカカオ脂 近似のカカオ代用脂を調製し、冷却曲線、固体脂含量、融点を測定し、カカオ代用脂としての機能を評価した。
<Comparative example 2>
47 parts by weight of the oil for fractionated sal fat obtained in Comparative Example 1 and 53 parts by weight of oil having a middle melting point of palm oil (iodine value 34.5, melting point 31.6 ° C., POP content 68.0%) prepared by a conventional method A cacao substitute fat similar to cacao butter was prepared and the cooling curve, solid fat content and melting point were measured, and the function as a cacao substitute fat was evaluated.
実施例４、比較例２の冷却曲線、固体脂含量、融点の結果を表２に示す。なお、これらの測定法は以下に準ずる。 Table 2 shows the results of the cooling curves, solid fat contents, and melting points of Example 4 and Comparative Example 2. In addition, these measuring methods apply to the following.
＜測定方法＞
（１）冷却曲線：英国基準分析法（Ｂｒｉｔｉｓｈ Ｓｔａｎｄａｒｄ Ｍｅｔｈｏｄｓ ｏｆ Ｆａｔｓ ａｎｄ ｆａｔｔｙ ｏｉｌｓ，Pａｒｔ １．Ｐｈｙｓｉｃａｌ methods，Ｓｅｃｔｉｏｎ １．１３，Ｄｅｔｅｒｍｉｎａｔｉｏｎ ｏｆ ｃｏｏｌｉｎｇ ｃｕｒｖｅ）に基づき、測定した。すなわち、サル脂分別油を ６０℃、３０分以上で加熱融解し、７５ｇを１００ｍｌ容試験管にいれ、１６．０℃の恒温水槽で撹拌しながら冷却したときの変化を、縦軸を温度とし、横軸を経過時間としてグラフにしたものであり、サル脂分別油を冷却・結晶化したときの温度変化を示したものである。冷却曲線は、溶解した油脂が冷却されるに従い油脂の温度が下がるが、結晶化が起こると結晶化熱により油脂温度が上昇しはじめ、やがて最高温度に達すると再び下降するような温度変化をグラフにしたものである。結晶化熱により、油脂温度が上昇しはじめる温度を最下点温度（Ｔｍｉｎ）、最高温度を最高点温度（Ｔｍａｘ）として、ＴｍａｘとＴｍｉｎの差（ΔＴ）が大きいほど、結晶化特性が良いとされ、チョコレートテンパリング後の離型性がよくなる傾向のため、カカオ代用脂としてより好ましい。カカオ代用脂の中でも、Ｃｏｃｏａ Ｂｕｔｔｅｒ Ｅｑｕｉｖａｌｅｎｔ（ＣＢＥ）と呼ばれるカカオ脂近似の物理的性質を持つような高品質カカオ代用脂の場合は、ΔＴが４．５℃以上をひとつの目安としている。
<Measurement method>
(1) Cooling curve: measured based on British Standard Methods of Fats and Fatty Oils, Part 1. Physical methods, Section 1.13, Determining of cooling curve. That is to say, when the oil fraction of monkey sebum is heated and melted at 60 ° C. for 30 minutes or longer, 75 g is placed in a 100 ml test tube and cooled with stirring in a 16.0 ° C. constant temperature water bath, and the vertical axis is the temperature. The graph shows the elapsed time on the horizontal axis, and shows the temperature change when the monkey oil fraction is cooled and crystallized. The cooling curve is a graph showing the temperature change in which the temperature of the oil and fat decreases as the dissolved oil and fat cools, but when the crystallization occurs, the temperature of the oil and fat starts to increase due to the heat of crystallization, and then decreases again when the maximum temperature is reached. It is a thing. The temperature at which the oil and fat temperature starts to rise due to crystallization heat is the lowest point temperature (Tmin), the highest temperature is the highest point temperature (Tmax), and the larger the difference (ΔT) between Tmax and Tmin, the better the crystallization characteristics. In view of the tendency to improve releasability after chocolate tempering, it is more preferable as a cacao substitute fat. Among the cocoa substitute fats, in the case of a high quality cocoa substitute fat having a physical property of cacao fat approximation called Cocoa Butter Equivalent (CBE), ΔT is set to 4.5 ° C. or more as one standard.
（２）固体脂含量：基準油脂分析試験法暫定法１−１９９６、固体脂含量ＮＭＲ法に基づいて測定した。エージングは２６℃／４０時間とした。 (2) Solid fat content: measured based on provisional method 1-196 for standard fat analysis method, solid fat content NMR method. Aging was performed at 26 ° C./40 hours.
（３））融点：基準油脂分析試験法２．２．４．３−１９９６，軟化点（環球法）に基づいて測定した。エージングは２５℃／２４時間とした。 (3)) Melting point: Measured based on the standard fat and oil analysis test method 2.2.4.3-1996, softening point (ring-ball method). Aging was performed at 25 ° C./24 hours.
＜表２＞
表２にあるように、実施例４は比較例２に比べて冷却曲線ΔＴが大きく、固体脂含量も高い値を示した。この結果から、本発明の実施例１で製造したサル脂分別油を使用した実施例４は比較例２に対比して、明らかに高品質のカカオ代用脂であった。
As shown in Table 2, Example 4 showed a larger cooling curve ΔT and higher solid fat content than Comparative Example 2. From this result, Example 4 using the salfat fractionated oil produced in Example 1 of the present invention was clearly a high-quality cacao substitute fat in comparison with Comparative Example 2.
本発明は低品質サル脂の品質改良法に関し、詳しくはサル脂分別油をカカオ代用脂として利用したとき良好な結晶化特性を示すように、サル脂分別油を品質改良する方法に関する。 The present invention relates to a method for improving the quality of low-quality monkey fat, and more particularly to a method for improving the quality of monkey oil fraction so as to exhibit good crystallization characteristics when the monkey fat fraction is used as a cocoa substitute fat.
Claims (3)
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009083515A JP4826848B2 (en) | 2009-03-30 | 2009-03-30 | Process for producing fractionated monkey oil |
| MYPI2010001230A MY147413A (en) | 2009-03-30 | 2010-03-19 | Production method for franctionated sal fat |
| SG201001961-0A SG165267A1 (en) | 2009-03-30 | 2010-03-22 | Production method for fractionated sal fat |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009083515A JP4826848B2 (en) | 2009-03-30 | 2009-03-30 | Process for producing fractionated monkey oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2010235711A JP2010235711A (en) | 2010-10-21 |
| JP4826848B2 true JP4826848B2 (en) | 2011-11-30 |
Family
ID=43090351
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2009083515A Expired - Fee Related JP4826848B2 (en) | 2009-03-30 | 2009-03-30 | Process for producing fractionated monkey oil |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP4826848B2 (en) |
| MY (1) | MY147413A (en) |
| SG (1) | SG165267A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MY191291A (en) * | 2016-12-20 | 2022-06-14 | Nisshin Oillio Group Ltd | Method for manufacturing fats and oils |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4475702B2 (en) * | 1999-08-18 | 2010-06-09 | 株式会社Ａｄｅｋａ | Process for producing fractionated monkey oil |
| JP2004298041A (en) * | 2003-03-31 | 2004-10-28 | Fuji Oil Co Ltd | Method for producing chocolate and hard butter |
| TWI441915B (en) * | 2007-09-07 | 2014-06-21 | Nisshin Oillio Group Ltd | Method of fractionating 1, 3-disaturated-2-unsaturated triglyceride |
-
2009
- 2009-03-30 JP JP2009083515A patent/JP4826848B2/en not_active Expired - Fee Related
-
2010
- 2010-03-19 MY MYPI2010001230A patent/MY147413A/en unknown
- 2010-03-22 SG SG201001961-0A patent/SG165267A1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| MY147413A (en) | 2012-12-14 |
| SG165267A1 (en) | 2010-10-28 |
| JP2010235711A (en) | 2010-10-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2490550B1 (en) | High melting point sunflower fat for confectionary | |
| JP6163530B2 (en) | Method for producing hard butter similar to cocoa butter | |
| US9803159B2 (en) | Method of making oil-and-fat | |
| JP2013507119A (en) | Cocoa butter substitute oil and fat for chocolate and chocolate composition containing the same | |
| JP2013507118A (en) | Chocolate by enzymatic transesterification and method for producing confectionery fats and oils | |
| JPWO2011122278A1 (en) | Extraction method of shea fat | |
| EP0130487A2 (en) | Cacao butter substitutes and chocolates containing the same | |
| JP4826848B2 (en) | Process for producing fractionated monkey oil | |
| US7767241B2 (en) | Dry fractionation method for fat | |
| JP2004298041A (en) | Method for producing chocolate and hard butter | |
| JP4475702B2 (en) | Process for producing fractionated monkey oil | |
| JP5576513B2 (en) | Oil and fat manufacturing method | |
| JPS60395B2 (en) | Palm oil separation method | |
| JP2000109879A (en) | Process for fractionation of cocoa butter | |
| JP2014162859A (en) | Method for dry-fractionating oil and fat | |
| JP2016077175A (en) | Manufacturing method of hard butter | |
| JP4534986B2 (en) | Method for dry separation of fats and oils | |
| JP4397116B2 (en) | Cocoa butter ole infrastructure | |
| US20140206891A1 (en) | Method for producing triacylglycerol oil | |
| JPS63479B2 (en) | ||
| JP5724872B2 (en) | Chocolates with excellent bloom inhibitors and bloom resistance | |
| JPS629289B2 (en) | ||
| JP2017184666A (en) | Manufacturing method of hard butter | |
| JP2013523910A (en) | Dry fractionation method for transesterified oil / fat composition (Dryfractionation methodforesterified oil and fat composition) | |
| WO2022050338A1 (en) | Non-tempered-type hard butter composition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20110304 |
|
| A871 | Explanation of circumstances concerning accelerated examination |
Free format text: JAPANESE INTERMEDIATE CODE: A871 Effective date: 20110304 |
|
| A975 | Report on accelerated examination |
Free format text: JAPANESE INTERMEDIATE CODE: A971005 Effective date: 20110329 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20110502 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20110629 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20110719 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20110722 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20110817 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20110830 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140922 Year of fee payment: 3 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 4826848 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140922 Year of fee payment: 3 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| R371 | Transfer withdrawn |
Free format text: JAPANESE INTERMEDIATE CODE: R371 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| LAPS | Cancellation because of no payment of annual fees |