TWI657747B - Peach extract and method for producing the same - Google Patents
Peach extract and method for producing the same Download PDFInfo
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Abstract
本發明之課題在提供具有得自桃的活性氧清除能之桃萃取物、及安全性優異的製造方法。 An object of the present invention is to provide a peach extract having active oxygen scavenging energy derived from peach, and a method for producing the peach extract having excellent safety.
其係將疏果桃(幼桃)、熟桃、或者疏果桃或熟桃經除去種子及果汁而得之含纖維成分的桃加工殘渣之桃原料,經過乙醇、或乙醇/己烷混合液萃取,再以製得之一次萃取液經己烷/水分段萃取而獲得之具有活性氧清除能的桃萃取物,亦為含神經醯胺(神經鞘糖脂質)、多酚之桃萃取物,以及其製造方法。本發明製得之桃萃取物,可利用在食品、化妝品或準藥品,及該等之加工品上。 It is a peach raw material obtained from sparse peaches (young peaches), ripe peaches, or sparse peaches or ripe peaches by removing the seeds and fruit juice, and containing fiber-containing peach processing residues, after passing through ethanol or an ethanol / hexane mixture Peach extract with active oxygen scavenging energy obtained by one-stage extraction with hexane / water, and a peach extract containing ceramide (sphingomyelin) and polyphenols , And its manufacturing method. The peach extract prepared by the present invention can be used in food, cosmetics or quasi-drugs, and processed products thereof.
Description
本發明係有關一種具有活性氧清除能,且含神經鞘糖脂質(神經醯胺成分)之桃萃取物、及其製造方法。 The present invention relates to a peach extract having active oxygen scavenging ability and containing sphingomyelin (neuraminyl component), and a method for producing the same.
最近,在安全性方面所進行的來自天然成分之素材的研究,已提出各種具有有效之生理活性的植物萃取物。 Recently, research on materials derived from natural ingredients in terms of safety has proposed various plant extracts having effective physiological activity.
本案發明人等亦關注於植物油脂,特別是在製造以米糠作為原料之食用米糠油之過程中產生的副產品所含之可用微量成分,進行檢討之結果,確立米源神經醯胺之萃取製造法,而可提供天然來源之米源神經醯胺(神經鞘糖脂質)。 The inventors of this case are also concerned about vegetable oils and fats, and in particular the usable trace ingredients contained in the by-products produced during the production of edible rice bran oil using rice bran as a raw material. The results of the review have established the extraction and manufacturing method of rice-derived nerve ceramide. It can provide rice-derived ceramide (sphingomyelin) of natural origin.
本發明人等所提供之米源神經醯胺,係來自於天然素材之神經醯胺,其安全性高,且其純度極高,因此目前已廣泛地利用作為食品、化妝品或準藥品,及該等之加工品之素材。 The rice-derived neuraminamine provided by the present inventors is a neuraminamine derived from natural materials, which has high safety and extremely high purity. Therefore, it has been widely used as food, cosmetics or quasi drugs, and the And other processed materials.
神經醯胺係神經鞘脂質之一種,為長鏈胺 基醇之神經胺醇與脂肪酸經由醯胺鍵結的化合物群之統稱。該神經醯胺,已知係以高濃度存在於細胞膜中,特別,以皮膚之角質細胞間脂質主成分存在,而擔任防止水分由皮膚內部蒸發之保濕能力的屏障功能。 Neuraminamine is a kind of sphingomyelin, which is a long-chain amine. A group of compounds in which ceramide and fatty acids are bonded via amidine. This neuraminamine is known to exist in cell membranes at high concentrations, and in particular, to be the main component of interkeratinocyte lipids of the skin, and to serve as a barrier function to prevent moisture from evaporating from the skin.
然而,已有報告指出,由於年齡增長亦會同時使角質細胞間脂質中的神經醯胺減少,使保濕能力降低,因此成為皮膚乾燥、皺紋、或皮膚粗糙之原因。 However, it has been reported that as age increases, neuraminamine in the keratinocyte lipids is also reduced, which reduces the ability to moisturize, which can cause dry skin, wrinkles, or rough skin.
同時,不只皮膚老化,由於異位性皮膚炎所引起之皮膚乾燥、皮膚粗糙的主要原因係報告指出為神經醯胺之不足。亦即,報告指出異位性皮膚炎中之乾燥皮膚之特徵係原本之神經醯胺較少,隨著皮膚之屏障功能的降低,水分容易由皮膚內部向外流失,而使皮膚粗乾而乾燥,致使抗原及化學物質易於進入皮膚內部,結果引起過敏反應,呈現搔癢及發炎等之各種症狀。 At the same time, not only the skin is aging, but the main causes of dry skin and rough skin due to atopic dermatitis are reported as the deficiency of neuraminamine. That is, the report points out that the characteristic of dry skin in atopic dermatitis is that the original neuraminamine is less. As the barrier function of the skin is reduced, moisture is easily lost from the skin to the outside, making the skin rough and dry As a result, antigens and chemicals can easily enter the skin, resulting in allergic reactions, showing various symptoms such as itching and inflammation.
因此,皮膚中神經醯胺之含量,成為皮膚健康狀態的指標之一,一般指出不足之神經醯胺的補充具有皮膚的保濕效果、或對美白效果有效,因而使神經醯胺成為化妝品之原料的需求增加,同時,甚至廣泛地利用作為緩和異位性皮膚炎症狀之機能性食品。 Therefore, the content of ceramide in the skin has become one of the indicators of skin health. Generally, it is pointed out that the supplement of inadequate ceramide has the moisturizing effect of the skin, or is effective for whitening, so that ceramide becomes the raw material of cosmetics At the same time, demand has increased, and at the same time, functional foods have been widely used to alleviate the symptoms of atopic skin inflammation.
此外,神經醯胺亦確定具有活化免疫作用、抗腫瘤效果等,因此今後將不斷地增加其需求。 In addition, Neuramin is also known to have activating immune effects and anti-tumor effects, so its demand will continue to increase in the future.
再者,目前為止,對來自各種果實或蔬菜等植物的神經醯胺成分進行各式各樣之研究(專利文獻1)。其中,由於桃據稱含多量之神經醯胺,而提出由桃萃 取神經醯胺的技術(專利文獻2)。 In addition, various studies have been conducted on neural amine components from plants such as various fruits and vegetables (Patent Document 1). Among them, because peach is said to contain a large amount of ceramides, Technique for taking Neuraminamine (Patent Document 2).
在桃所含之成分方面,不只其神經醯胺之萃取,亦對桃果實本身進行生理活性之檢討,亦曾報告桃果實所含之多酚、桃本身的活性氧清除能等之檢討(非專利文獻1至3)。 In terms of the ingredients contained in peach, not only the extraction of ceramide, but also the physiological activity of the peach fruit itself. It has also been reported that the polyphenols contained in peach fruit and the active oxygen scavenging energy of peach itself have been reviewed (non- (Patent Documents 1 to 3).
在上述專利文獻2中記載來自桃之神經醯胺的萃取,係使用氯仿/甲醇混合液作為萃取溶劑的萃取方法而調製葡萄糖苷神經醯胺分畫,但在考量作為萃取溶劑使用的氯仿及甲醇之毒性時,由安全性之面而言並不理想。 The above-mentioned Patent Document 2 describes the extraction of ceramide from peach. The extraction method uses a chloroform / methanol mixture as the extraction solvent to prepare the glucosylceramide profile. However, chloroform and methanol used as the extraction solvent are considered. In terms of toxicity, it is not ideal from the aspect of safety.
因此,要求檢討由桃萃取神經醯胺之更可確保安全性的方法。 Therefore, it is required to review the method of extracting neural crestamine from peach to ensure safety.
目前為止,所提出的以各種果實、蔬菜等植物成分萃取/製造神經醯胺成分之技術,已知有例如:葡萄、櫻桃、小麥、米、大豆等植物原料經由醇系溶劑(如乙醇)萃取的方法(專利文獻1);在山茶子油渣經由己烷脫脂/前處理之後,再以乙醇萃取的方法(專利文獻3);將米糠以選自:水、乙醇、丙酮、己烷的2種以上之混合溶劑萃取的方法(專利文獻4);將小麥、大豆、玉米、米糠等植物原料經過鹼性乙醇溶劑水解之後,再經由己烷、丙酮、及水之混合溶劑萃取的方法(專利文獻5及專利文獻6)等。 So far, the proposed technology for extracting / manufacturing neural cramine from plant components such as various fruits and vegetables is known. For example, grapes, cherries, wheat, rice, soybeans, and other plant materials are extracted through an alcohol-based solvent (such as ethanol). Method (Patent Document 1); a method in which camellia seed oil residue is degreased / pretreated with hexane and then extracted with ethanol (Patent Document 3); rice bran is selected from the group consisting of: water, ethanol, acetone, and hexane. A method of extracting more than one mixed solvent (Patent Document 4); a method of extracting plant materials such as wheat, soybean, corn, and rice bran with alkaline ethanol solvent, and then extracting the mixed solvent with hexane, acetone, and water (patent) Documents 5 and 6).
本發明人等,曾嘗試以桃經由上述各專利文獻中記載的可萃取神經醯胺成分之方法萃取,但均無法滿意。因而,鑑於現狀,再檢討由桃有效率且安全地萃取神經醯胺成分,結果發現以新穎之方法將桃原料經過乙 醇、或乙醇/己烷混合液進行萃取,再將所獲得之萃取液以己烷/水分段(Partitioning Extraction)萃取,而可有效率地獲得具有活性氧清除能、且含神經鞘糖脂質(神經醯胺成分)之桃萃取物,遂而完成本發明。 The present inventors have attempted to extract peaches by the method of extracting neural crestamine components described in each of the above-mentioned patent documents, but they have not been satisfactory. Therefore, in view of the current situation, we reviewed the efficient and safe extraction of neural amines from peaches. Extraction with alcohol or ethanol / hexane mixed solution, and then extracting the obtained extract with hexane / water Partitioning Extraction, can efficiently obtain active oxygen scavenging energy and sphingomyelin-containing lipid (Nervamine component) peach extract, then completed the present invention.
[專利文獻1]專利第4108069號公告公報 [Patent Document 1] Patent Publication No. 4108069
[專利文獻2]專利第4723630號公告公報 [Patent Document 2] Patent Publication No. 4723630
[專利文獻3]日本特開2007-308424號公報 [Patent Document 3] Japanese Patent Laid-Open No. 2007-308424
[專利文獻4]日本特開平11-279586號公報 [Patent Document 4] Japanese Patent Application Laid-Open No. 11-279586
[專利文獻5]日本特開2002-30093號公報 [Patent Document 5] Japanese Patent Laid-Open No. 2002-30093
[專利文獻6]日本特開2006-232699號公報 [Patent Document 6] Japanese Patent Laid-Open No. 2006-232699
[非專利文獻1]山梨縣工業技術中心研究報告No.22,p.59(2008) [Non-Patent Document 1] Yamanashi Industrial Technology Center Research Report No. 22, p. 59 (2008)
[非專利文獻2]岡山縣農業研報No.2,p.21(2011) [Non-Patent Document 2] Okayama Prefecture Agricultural Research Report No. 2, p. 21 (2011)
[非專利文獻3]營養學雜誌Vol.70,No.3,p.207(2012) [Non-Patent Document 3] Journal of Nutrition Vol.70, No.3, p.207 (2012)
因此本發明之課題,係在於提供一種將由桃獲得具有活性氧清除能之桃萃取物,有效率且安全地萃取之方法、及提供一種以該製造方法製得具有活性氧清除 能、且含神經鞘糖脂質(神經醯胺成分)之桃萃取物。 Therefore, the subject of the present invention is to provide a method for efficiently and safely extracting a peach extract having active oxygen scavenging energy from peach, and to provide a method for producing active oxygen scavenging by the manufacturing method. A peach extract containing sphingomyelin (neuraminyl component).
為解決該課題,本發明之基本實施態樣之桃萃取物,其特徵係:將疏果桃、熟桃、或者疏果桃或熟桃經除去種子及果汁後之含纖維成分的桃加工殘渣,經過乙醇、或乙醇/己烷混合液萃取,再以該萃取液,經己烷/水分段萃取而獲得之具有活性氧清除能且含神經鞘糖脂質(神經醯胺成分)。 In order to solve this problem, the peach extract of the basic embodiment of the present invention is characterized in that: a peach processing residue containing fiber components after removing seeds and fruit juice from sparse peach, ripe peach, or sparse peach or ripe peach After being extracted with ethanol or a mixed solution of ethanol / hexane, the extract is then extracted with hexane / water in stages to obtain active oxygen scavenging energy and sphingomyelin (neuraminamine component).
更具體言之,本發明之桃萃取物,其中上述活性氧清除能係DPPH(二苯基苦味肼基)(diphenyl picryl hydrazyl)活性。 More specifically, in the peach extract of the present invention, the above-mentioned active oxygen scavenging energy is DPPH (diphenyl picryl hydrazyl) activity.
再更具體言之,本發明之桃萃取物,其中DPPH活性為5%以上,神經醯胺含量為0.5%以上。 To be more specific, the peach extract of the present invention has a DPPH activity of 5% or more and a neural amine content of 0.5% or more.
同時本發明之其他實施態樣,係一種桃萃取物之製造方法,其係具有活性氧清除能且含神經鞘糖脂質(神經醯胺成分)之桃萃取物的製造方法,具體言之,係將疏果桃、熟桃、或者疏果桃或熟桃經除去種子及果汁而得之含纖維成分的桃加工殘渣,經過乙醇、或乙醇/己烷混合液萃取,所得之萃取液再經過己烷/水分段萃取。 At the same time, other aspects of the present invention are a method for producing a peach extract, which is a method for producing a peach extract having active oxygen scavenging energy and containing a sphingomyelin (neuraminyl component). Specifically, the method The fruit processing peach, the ripe peach, or the peach or ripe peach is removed from the seeds and fruit juice, containing the fiber component of the peach processing residue, and then extracted with ethanol, or an ethanol / hexane mixture, and the resulting extract is passed through Alkane / water staged extraction.
更具體言之,本發明係桃萃取物、及其製造方法,其中桃加工殘渣萃取所使用之萃取液與萃取液之分段萃取用的己烷及水之容量比為1:0.5:0.5至1:2:2。 More specifically, the present invention is a peach extract and a method for producing the same, wherein the volume ratio of the hexane and water used for the staged extraction of the extraction liquid and the extraction liquid of the extraction residue of the peach processing residue is 1: 0.5: 0.5 to 1: 2: 2.
同時,本發明係為含上述桃萃取物之食品、化妝品或準藥品,及該等之加工品。 Meanwhile, the present invention is a food, a cosmetic or a quasi-drug containing the above-mentioned peach extract, and processed products thereof.
更具體言之,本發明係為將上述萃取物與環狀糊精混合而成之粉狀物、或水溶液狀態之食品、化妝品或準藥品,及該等之加工品。 More specifically, the present invention is a powder, a food, a cosmetic, or a quasi-drug in the form of an aqueous solution obtained by mixing the above-mentioned extract with a cyclodextrin, and processed products thereof.
以本發明可以安全性優異、較為簡便之方法,由桃原料有效率地獲得具有活性氧清除能之桃萃取物。 According to the present invention, a peach extract having active oxygen scavenging energy can be efficiently obtained from a peach raw material by a method with excellent safety and a relatively simple method.
本發明所提供之桃萃取物的製造方法,係對桃原料以乙醇、或乙醇/己烷混合液所得之萃取液,亦即所謂一次萃取液,再經過己烷/水之分段萃取,就此點而言,係目前為止未曾經過任何檢討的製造方法,因此極為特別。 The method for producing a peach extract provided by the present invention is an extraction liquid obtained by using ethanol or an ethanol / hexane mixed liquid on a peach raw material, which is a so-called primary extraction liquid, and then subjected to hexane / water segment extraction. In point of view, this is a special manufacturing method that has not been reviewed so far.
其結果,可使所製造之桃萃取物,含神經醯胺(神經鞘糖脂質)、多酚及醣苷,而具有活性氧清除能,且安全性高,在作為食品、化妝品或準藥品,及該等之加工品之素材上具有極高的可用性。 As a result, the produced peach extract can contain ceramide (sphingomyelin), polyphenols, and glycosides, and has active oxygen scavenging ability and high safety. It can be used as food, cosmetics, or quasi drugs, and These processed products have extremely high availability.
如上所述,本發明之桃萃取物,其特徵係:將疏果桃、熟桃、或者疏果桃或熟桃經除去種子及果汁而得之含纖維成分的桃加工殘渣之桃原料,經過乙醇、或乙醇/己烷混合液萃取,再將該萃取液經己烷/水之分段萃取所獲得之具有活性氧清除能、且含神經鞘糖脂質(神經醯胺成分)者。 As described above, the peach extract of the present invention is characterized in that the peach raw material containing peach processing residues containing fiber components obtained by removing seeds and fruit juice from sparse peach, ripe peach, or sparse peach or ripe peach is subjected to Ethanol, or ethanol / hexane mixed liquid extraction, and then the extract is obtained by hexane / water segmented extraction has active oxygen scavenging energy and contains sphingomyelin lipid (neuraminyl component).
其原料之疏果桃,係指在桃生產過程中所摘除之疏果 桃(幼桃);熟桃,係指桃中適於出貨至市場之桃。 The raw fruit sparse peach refers to the sparse fruit removed in the peach production process Peach (young peach); ripe peach refers to the peach in the peach suitable for shipment to the market.
再者,桃加工殘渣,係指疏果桃(幼桃)或熟桃經除去種子及果汁而得之含纖維成分的桃之加工殘渣。 Moreover, the peach processing residue refers to the processing residue of the peach containing fiber components obtained by removing seeds and fruit juice from sparse peach (young peach) or ripe peach.
桃之收獲量在全日本每年約為15萬噸,而收獲過程中所產生之疏果桃(幼桃),據稱約為桃收獲量之10%之約1.5萬噸。該疏果桃,只有極少部分加工作為食用醃漬品等,大半不經過處理直接以原來形態撒布在桃子農場(桃子園)作為肥料使用,因此並無有效利用之技法。 The amount of peaches harvested in Japan is about 150,000 tons per year, and the sparse peaches (young peaches) produced during the harvest process are said to be about 15,000 tons of 10% of the peach harvest. Only a very small part of this sparse fruit peach is processed as edible pickles, etc., and most of it is directly spread on the peach farm (peach garden) as a fertilizer without treatment, so there is no effective utilization method.
另一方面,桃果汁(桃汁)等的加工企業,年中約可產生1500噸左右之桃加工殘渣的副產物,但均未能有效地利用而丟棄。 On the other hand, processing companies such as peach juice (peach juice) can produce by-products of peach processing residues of about 1,500 tons in the middle of the year, but they are not effectively used and discarded.
本發明,係具有以該等未能有效利用而丟棄之疏果桃、或桃加工殘渣,以特別組合之萃取溶劑製造成桃萃取物,而可有效利用該副產物之點,因此極為特別。 The present invention is very special because it has the point that the peach fruit or the peach processing residues that have been discarded that cannot be effectively used are made into a peach extract with a special combination of extraction solvents, and this by-product can be effectively used.
作為萃取原料之桃原料,在使用疏果桃(幼桃)、或熟桃時,係將以此類疏果桃(幼桃)或熟桃經去除種子而含果肉及果皮的桃,視其需要預先予以冷凍,再將各以粉碎機等微細粉碎,以經暖風乾燥或減壓乾燥加以乾燥者,使用作為萃取用之原料。 As a raw material for peaches, when using sparse peaches (young peaches) or ripe peaches, the peaches containing flesh and peel are removed from the seeds of this type of sparse peaches (young peaches) or ripe peaches. Those that need to be frozen in advance, and each are finely pulverized by a pulverizer or the like, and dried by warm air drying or reduced pressure drying, and used as raw materials for extraction.
同時,作為萃取原料之桃原料,在使用以疏果桃或熟桃經去除種子及果汁而含纖維成分的桃加工殘渣時,可以在桃之果汁等加工步驟中所產生的副產物之桃加工殘渣(即所謂桃漿),以與上述相同的方法加以乾燥,再使用為萃取用之原料。 At the same time, as a raw material for peaches, when using peach processing residues containing sparse peaches or ripe peaches to remove fiber and seeds, the peach can be processed as a by-product of peach juice and other processing steps. The residue (so-called peach pulp) is dried in the same manner as described above, and then used as a raw material for extraction.
當然,由桃之果汁等加工步驟所產生的副產物之桃加工殘渣,亦可不經乾燥而怍為萃取用之原料。 Of course, peach processing residues produced as by-products from processing steps such as peach juice may also be used as raw materials for extraction without drying.
本發明所提供之由該等桃原料製造桃萃取物所使用之一次萃取溶劑,其特徵係:單獨使用乙醇、或使用乙醇/己烷之混合液。 The primary extraction solvent used in the present invention to produce peach extracts from these peach materials is characterized by using ethanol alone or using a mixed solution of ethanol / hexane.
在專利文獻2中所揭示之桃的萃取溶劑,係氯仿/甲醇以1:1體積比混合的溶劑,因此在獲得之醣苷神經醯胺分畫(萃取物)中,有毒性強之氯仿或甲醇殘留的虞慮,未必良好。 The extraction solvent of peach disclosed in Patent Document 2 is a solvent in which chloroform / methanol is mixed at a volume ratio of 1: 1. Therefore, in the obtained glycoside neural crestamine extract (extract), chloroform or methanol having strong toxicity is included. Residual concerns may not be good.
相對於此,本發明中係使用食品加工及油脂加工所使用的乙醇及己烷者,因此獲得之萃取物有極高之安全性。 In contrast, in the present invention, ethanol and hexane used in food processing and fat processing are used, and therefore the obtained extract has extremely high safety.
一次萃取溶劑,除了乙醇或乙醇/己烷之外,亦可使用甲醇、丙醇、異丙醇、丁醇、異丁醇等可與水混合的低級醇類、及單獨之丙酮等、或該等溶劑間之混合液、或者該等溶劑與己烷之混合液。 One-time extraction solvent, in addition to ethanol or ethanol / hexane, methanol, propanol, isopropanol, butanol, isobutanol, and other lower alcohols that can be mixed with water, acetone alone, etc. A mixed liquid between solvents, or a mixed liquid of such solvents and hexane.
萃取溶劑相對於屬於萃取用原料之桃原料之使用量並無特別之限定,惟相對於屬於原料之桃微粉末、或桃加工殘渣100g,以換算為0.1至1L左右而使用為佳。 The use amount of the extraction solvent with respect to the peach raw material which is the raw material for extraction is not particularly limited, but it is preferably used in a conversion of about 0.1 to 1 L with respect to 100 g of the peach fine powder or the peach processing residue which belongs to the raw material.
同時,在以乙醇/己烷之混合液萃取時,其混合比為,相對於己烷1容量,乙醇以1至5容量為佳,以1至3容量更佳。 At the same time, when extracting with a mixed liquid of ethanol / hexane, the mixing ratio is: 1 to 5 capacity of ethanol is better than 1 to 3 capacity of ethanol relative to 1 capacity of hexane.
在該情形下之萃取溫度、時間並無特別限定,以在室溫至80℃左右之溫度,0.1至24小時左右進行者為佳。 The extraction temperature and time in this case are not particularly limited, but it is preferably carried out at a temperature from room temperature to about 80 ° C. for about 0.1 to 24 hours.
如上之情形,本發明的桃萃取物之製造方法中的萃取步驟,可單獨用乙醇、或以乙醇/己烷之混合液進行一次萃取。在單獨用乙醇萃取時,亦可使用含水乙醇。 As described above, in the extraction step in the method for producing a peach extract of the present invention, one extraction can be performed with ethanol alone or with a mixed solution of ethanol / hexane. When extracting with ethanol alone, aqueous ethanol can also be used.
本發明的桃萃取物之製造方法,係將單獨用乙醇、或以乙醇/己烷之混合液萃取之所謂一次萃取液,再經過己烷/水進行分段萃取,即可由己烷溶液層獲得目的之具有活性氧清除能、且含神經鞘糖脂質(神經醯胺成分)之桃萃取物。 The method for producing a peach extract according to the present invention is a so-called one-time extraction solution which is extracted with ethanol alone or with a mixed solution of ethanol / hexane, and then subjected to segment extraction through hexane / water to obtain the hexane solution layer. Purpose: Peach extract with active oxygen scavenging ability and sphingomyelin (neuraminyl component).
經過本發明人等之檢討,可知一次萃取中之萃取液、及萃取液之分段萃取中所使用的己烷與水之容量比,以1:0.5:0.5至1:2:2為佳(參考後述之實施例)。 After review by the inventors, it can be known that the volume ratio of hexane to water used in the extraction liquid in a single extraction and the stepwise extraction of the extraction liquid is preferably 1: 0.5: 0.5 to 1: 2: 2 ( (Refer to the embodiment described later).
因此,在以一次萃取中所使用之萃取液(單獨用乙醇、或乙醇/己烷之混合液)為1容量時,相對於一次萃取液之己烷/水的分段萃取中之己烷與水之容量比,可在己烷0.5至2容量、水0.5至2容量的範圍內適當地選擇。 Therefore, when the volume of the extraction liquid (ethanol alone or ethanol / hexane mixed liquid) used in one extraction is 1 volume, the hexane and The capacity ratio of water can be appropriately selected within the range of 0.5 to 2 capacity of hexane and 0.5 to 2 capacity of water.
在以該容量比進行一次萃取液、己烷/水之分段萃取時,可提高分段萃取中之分離度、及神經醯胺成分之含有率。 When the extraction ratio and the hexane / water stepwise extraction are performed at this capacity ratio, the separation degree and the content of neural amines in the staged extraction can be improved.
一般所知,在有機層與水層不分離而呈乳化狀態時,經由鹽的添加及加溫/冷卻、或使用矽藻土等非活性載體之過濾等處理即可消除乳化。當然在本發明中,亦曾檢討採用該類方法,並已確認有在呈乳化狀態之混合比下,經由鹽析、及加溫/冷卻、或使用矽藻土等非活性載體之過濾等處理即可消除乳化之情形。 It is generally known that when the organic layer and the water layer are in an emulsified state without being separated, the emulsification can be eliminated by adding salt, heating / cooling, or filtering using an inactive carrier such as diatomaceous earth. Of course, in the present invention, this type of method has been reviewed and adopted, and it has been confirmed that under the mixing ratio in the emulsified state, it is processed through salting out, heating / cooling, or filtration using inactive carriers such as diatomaceous earth. Can eliminate the situation of emulsification.
然而,在鹽之添加及以矽藻土過濾等的處理中,萃取 物中無可避免會混入鹽及載體。同時,加溫/冷卻等之方法,不僅溫度管理及時間管理等處理步驟繁瑣,亦多有無法保證必定可以分離之情形。 However, in the process of adding salt and filtering with diatomaceous earth, extraction It will inevitably be mixed with salts and carriers. At the same time, methods such as heating / cooling not only have tedious processing steps such as temperature management and time management, but also often cannot guarantee that they can be separated.
另一方面,以本發明之溶劑比中,混合後,只要靜置,即可有效率地分離。 On the other hand, in the solvent ratio of the present invention, after mixing, it can be efficiently separated as long as it is left to stand.
此種相對於一次萃取液之以己烷/水所進行的分段萃取、其溶劑比,係本發明人等經過檢討之結果的新穎發現,此點極為特別。 This stepwise extraction with hexane / water with respect to the primary extraction solution, and its solvent ratio are novel findings based on the review results of the present inventors, which is very special.
再者,該以己烷/水之分段萃取所得之己烷溶液層,亦可視所需,再進行如活性碳處理、及層析處理等以更提高萃取物之精製度。 Furthermore, the hexane solution layer obtained by the hexane / water segmented extraction can also be subjected to, for example, activated carbon treatment and chromatographic treatment, if necessary, to further improve the refined system of the extract.
同時,本發明的桃萃取物之製造方法的萃取技法中,將萃取對象之幼桃、熟桃、或者幼桃或熟桃經去除種子及果汁而含纖維成分的桃加工殘渣之微粉碎乾燥物,亦可預先以己烷加以脫脂處理,即可藉由該脫脂處理使桃萃取物中的脂質含量減少,結果可提高神經醯胺之含有比例。 At the same time, in the extraction technique of the method for producing a peach extract of the present invention, a young crushed peach, a ripe peach, or a young peach or a ripe peach, which has been removed from seeds and juice, is finely pulverized and dried with a fiber-containing peach processing residue. It can also be degreased with hexane in advance, and the lipid content in the peach extract can be reduced by the degreasing treatment. As a result, the content of neural amine can be increased.
同時,上述一次萃取之操作中,亦可在適度之鹼條件下進行萃取操作,惟在該鹼條件下之萃取操作,並非必要。 At the same time, in the above-mentioned one-time extraction operation, the extraction operation can also be performed under moderate alkaline conditions, but the extraction operation under the alkaline conditions is not necessary.
再者,亦已知在使用萃取溶劑之單獨用乙醇溶劑萃取時,可使萃取物中的多酚含量高。 Furthermore, it is also known that when using an extraction solvent alone for extraction with an ethanol solvent, the polyphenol content in the extract can be made high.
因此,對應目的萃取物所含成分為何之時的用途,可適當地選擇萃取條件,由此點,本發明的桃萃取物之製造 方法可說是極為特別。 Therefore, the extraction conditions can be appropriately selected according to the use of the ingredients contained in the target extract. From this point, the production of the peach extract of the present invention The method is extremely special.
將上述經萃取處理獲得之萃取物,再經過減壓下濃縮,並經過減壓乾燥即可成為固狀物,而製得本發明目的之桃萃取物。 The extract obtained by the above-mentioned extraction treatment is concentrated under reduced pressure, and dried under reduced pressure to become a solid, thereby preparing the peach extract of the present invention.
該製成之桃萃取物中,含有神經醯胺(神經鞘糖脂質)、多酚及醣苷等,由於其含多酚及其他抗氧化活性物質而具有活性氧清除能,同時,神經醯胺之含量亦高,所謂之「桃神經醯胺」,可有效地應用在食品、化妝品或準藥品,及該等之加工品上。 The prepared peach extract contains ceramide (sphingomyelin), polyphenols, and glycosides. It contains active oxygen scavenging ability due to its polyphenol and other antioxidant active substances. The content is also high. The so-called "Peach Nervamine" can be effectively used in food, cosmetics or quasi drugs, and processed products of these.
特別是本發明提供之桃萃取物,其活性氧清除能係DPPH(二苯基苦味肼基)活性為5%以上,神經醯胺含量為0.5%以上。 In particular, the peach extract provided by the present invention has an active oxygen scavenging energy DPPH (diphenyl bitter hydrazine) activity of 5% or more, and a neuroniamine content of 0.5% or more.
該桃萃取物,更具體而言,例如可怍成與如環狀糊精混合之粉狀物、或溶在水溶液中成溶液之狀態,使用在食品、化妝品或準藥品,及該等之加工品中。 More specifically, the peach extract can be used, for example, in a powdery state mixed with, for example, cyclodextrin, or dissolved in an aqueous solution to form a solution, and used in food, cosmetics, or quasi-drugs, and the like. Product.
以下,將本發明的桃萃取物之具體製造方法,以實施例中所記載,更詳細地說明本發明,惟本發明並不限定於此等實施例,在不脫離本發明之技術思想上之範圍下亦可作各種變更。 Hereinafter, the specific production method of the peach extract of the present invention will be described in more detail with reference to the examples, but the present invention is not limited to these examples, and it does not depart from the technical idea of the present invention. Various changes can be made within the scope.
試驗例1:神經醯胺含量之測定 Test Example 1: Determination of Neuraminamine Content
以下實施例中的桃萃取物之神經醯胺含量(純度)的測定,可如下進行。 The measurement of the ceramide content (purity) of the peach extract in the following examples can be performed as follows.
1.測定試樣係以使桃萃取物成為20mg/mL之方式溶於氯 仿/甲醇(2:1 v/v)混合液中,作成試樣溶液。 1. The measurement sample is dissolved in chlorine so that the peach extract becomes 20 mg / mL. A sample solution was prepared in a mixture of imitation / methanol (2: 1 v / v).
2.標準品係使用美國Matreya公司之標準品(來自大豆之精製品),以使其成為2mg/mL之方式,溶於氯仿/甲醇(2:1 v/v)混合液中,並製作依序稀釋之系列,作成標準液。 2. The standard product uses a standard product from American Matreya Company (a refined product from soybeans) so that it becomes 2 mg / mL, and is dissolved in a chloroform / methanol (2: 1 v / v) mixed solution, and produced according to Sequential dilution series to make a standard solution.
3.再於TLC層析板(Analtech公司,Silica Gel GF,Scored 10×20cm,250μm)上,各以試樣溶液及標準液1μL點樣,之後以展開溶劑(氯仿:甲醇:乙酸:水=20:3.5:2.3:0.7 v/v/v/v)展開。展開後,再於室溫下將層析板乾燥,並以50%硫酸噴霧,於150℃下加熱6分鐘呈色。 3. On a TLC chromatography plate (Analtech, Silica Gel GF, Scored 10 × 20cm, 250 μm), spot each with 1 μL of the sample solution and the standard solution, and then develop the solvent (chloroform: methanol: acetic acid: water = 20: 3.5: 2.3: 0.7 v / v / v / v). After development, the chromatography plate was dried at room temperature, sprayed with 50% sulfuric acid, and heated at 150 ° C for 6 minutes to develop a color.
桃萃取物中之神經醯胺含量(純度),係將層析板上之呈色點濃度,以感光密度計(Atto公司製造,CS Analyzer)測定,再以由標準液製作之標準曲線計算。 The Neuramin content (purity) in the peach extract was determined by measuring the color point concentration on the chromatography plate using a photodensitometer (manufactured by Atto Corporation, CS Analyzer), and then calculating using a standard curve prepared from a standard solution.
試驗例2:DPPH自由基消除活性之測定 Test Example 2: Determination of DPPH radical elimination activity
以下之實施例中,DPPH(二苯基苦味肼基)自由基消除活性的測定,係如下進行。 In the following examples, the measurement of the DPPH (diphenylpictrazine) radical elimination activity was performed as follows.
1.測定試樣分別以乙醇調整為2mg/mL。 1. The measurement samples were adjusted to 2 mg / mL with ethanol.
2.DPPH以乙醇調整為0.4mM。 2. DPPH was adjusted to 0.4 mM with ethanol.
3.如下調整測定試樣溶液。 3. Adjust the measurement sample solution as follows.
(1)試樣組 (1) Sample group
在2mL之2mg/mL試樣溶液中混合DPPH溶液1mL、乙醇1mL 1mL of DPPH solution and 1mL of ethanol in 2mL of 2mg / mL sample solution
(2)試樣空白組 (2) Sample blank group
在2mL之2mg/mL試樣溶液中混合乙醇2mL Mix 2mL of ethanol in 2mL of 2mg / mL sample solution
(3)控制組 (3) Control group
將3mL之乙醇與1mL之DPPH溶液混合 Mix 3mL of ethanol with 1mL of DPPH solution
(4)空白控制組 (4) Blank control group
4mL之乙醇 4mL of ethanol
4.上述測定試樣溶液在調製後,進行遮光20分鐘使之反應。反應後,以分光光度計測定571nm下之吸光度(OD)。 4. After the above measurement sample solution is prepared, it is shielded from light for 20 minutes to react. After the reaction, the absorbance (OD) at 571 nm was measured with a spectrophotometer.
自由基消除率(%)係以下式求出。 The radical elimination rate (%) is determined by the following formula.
自由基消除率(%)=[1-(試樣組之OD-空白試樣組之OD)÷(控制組之OD-空白控制組之OD)]×100 Free radical elimination rate (%) = [1- (OD of sample group-OD of blank sample group) ÷ (OD of control group-OD of blank control group) × 100
試驗例3:總多酚含量之測定 Test example 3: determination of total polyphenol content
同時,以下之實施例中的總多酚含量之測定,係如下進行。 Meanwhile, the measurement of the total polyphenol content in the following examples was performed as follows.
1.測定試樣以80%乙醇調整為10mg/mL,再以蒸餾水稀釋10倍成1.0mg/mL,作為測定試樣。 1. The measurement sample was adjusted to 10 mg / mL with 80% ethanol, and then diluted 10 times with distilled water to 1.0 mg / mL as the measurement sample.
2.標準品之沒食子酸係如下製作。28ppm、14ppm、7ppm、33.5ppm、1.75ppm 2. The gallic acid of the standard product is prepared as follows. 28ppm, 14ppm, 7ppm, 33.5ppm, 1.75ppm
3.再製作10%碳酸鈉水溶液。 3. Make a 10% sodium carbonate aqueous solution.
4.之後以精製水製作成稀釋5倍之酚試劑。 4. After that, make a 5-fold diluted phenol reagent with purified water.
5.再於各測定試樣2mL中加入稀釋5倍之酚試劑2mL、10%碳酸鈉水溶液2mL,並攪拌1小時使之反應。 5. To 2 mL of each measurement sample, add 2 mL of a 5-fold diluted phenol reagent and 2 mL of a 10% sodium carbonate aqueous solution, and stir for 1 hour to react.
6.過濾該反應液,並測定760nm下之吸光度。 6. The reaction solution was filtered, and the absorbance at 760 nm was measured.
7.製作沒食子酸標準曲線,求出總多酚(總PP)含量(mg/g)。 7. Prepare a gallic acid standard curve and find the total polyphenol (total PP) content (mg / g).
參考例1:由桃加工殘渣以乙醇單獨萃取之萃取物的製造 Reference Example 1: Manufacture of an extract from a peach processing residue separately extracted with ethanol
在乾燥之桃加工殘渣10g中,加入95%乙醇20mL,並於42℃、30分鐘之攪拌下萃取。再將該萃取物減壓過濾而獲得萃取液,另一方面,萃取之殘渣亦再次經過相同之萃取處理而獲得萃取液。將兩萃取液合併,並以蒸餾裝置減壓濃縮,將殘渣以60℃減壓乾燥,即可製得橙色固形物1.17g。 To 10 g of the dried peach processing residue, 20 mL of 95% ethanol was added, and extraction was performed at 42 ° C. with stirring for 30 minutes. The extract was then filtered under reduced pressure to obtain an extract. On the other hand, the extraction residue was subjected to the same extraction treatment again to obtain an extract. The two extracts were combined and concentrated under reduced pressure in a distillation apparatus, and the residue was dried under reduced pressure at 60 ° C to obtain 1.17 g of an orange solid.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,其結果如下。 The obtained extract was measured for Neuramin content (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, and the results were as follows.
神經醯胺含量(純度):0.7% Nervamine content (purity): 0.7%
DPPH活性:88.8% DPPH activity: 88.8%
總多酚含量:19.0mg/g Total polyphenol content: 19.0mg / g
參考例2:由桃加工殘渣以己烷單獨萃取之萃取物的製造 Reference Example 2: Production of an extract from a peach processing residue separately extracted with hexane
在乾燥之桃加工殘渣60g中加入己烷240mL,並於60℃、加以攪拌操作下萃取(脫脂)2小時。之後將該萃取物減壓過濾,並以己烷60mL排出。再將所得之濾液減壓濃縮,並將殘渣減壓乾燥,即可製得金黃色的糖漿狀物0.3g。 To 60 g of the dried peach processing residue, 240 mL of hexane was added, and the mixture was extracted (defatted) at 60 ° C. with stirring for 2 hours. The extract was then filtered under reduced pressure and discharged with 60 mL of hexane. The obtained filtrate was concentrated under reduced pressure, and the residue was dried under reduced pressure to obtain 0.3 g of a golden yellow syrup.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,其結果如下。 The obtained extract was measured for Neuramin content (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, and the results were as follows.
神經醯胺含量(純度):0.0% Nervamine content (purity): 0.0%
DPPH活性:24.6% DPPH activity: 24.6%
總多酚含量:2.7mg/g Total polyphenol content: 2.7mg / g
再者,該萃取物,幾乎全為脂質。 Moreover, this extract is almost entirely lipid.
實施例1:由疏果桃(幼桃)製造萃取物 <萃取溶劑:單獨用乙醇 己烷/水分段萃取經鹼處理> Example 1: Extraction from sparse peach (young peach) <Extraction solvent: Separate extraction with ethanol, hexane / water, and alkali treatment>
冷凍疏果桃(幼桃)先經過微波爐解凍15分鐘,並以粉碎機微細粉碎,並加以乾燥。之後於粉末50g中加入95%乙醇300mL(含氫氧化鈉9.6g)及精製水37.5mL,並於42℃、30分鐘之攪拌下萃取。再將該萃取物減壓過濾,並於濾液中加入己烷300mL及精製水150mL加以攪拌並分段萃取。之後回收己烷層,該溶劑以蒸餾裝置減壓濃縮,將殘渣以60℃減壓乾燥,製得綠色固形物160.7mg。 Frozen sparse peaches (young peaches) were thawed in a microwave oven for 15 minutes, finely pulverized with a pulverizer, and dried. Subsequently, 300 mL of 95% ethanol (containing 9.6 g of sodium hydroxide) and 37.5 mL of purified water were added to 50 g of the powder, and extracted at 42 ° C. with stirring for 30 minutes. The extract was filtered under reduced pressure, and 300 mL of hexane and 150 mL of purified water were added to the filtrate, stirred, and extracted in stages. Thereafter, the hexane layer was recovered, the solvent was concentrated under reduced pressure in a distillation apparatus, and the residue was dried under reduced pressure at 60 ° C to obtain 160.7 mg of a green solid.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,其結果如下。 The obtained extract was measured for Neuramin content (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, and the results were as follows.
神經醯胺含量(純度):1.8% Nervamine content (purity): 1.8%
DPPH活性:6.5% DPPH activity: 6.5%
總多酚含量:0.4mg/g Total polyphenol content: 0.4mg / g
實施例2:由疏果桃(幼桃)製造萃取物 <萃取溶劑:單獨用乙醇 己烷/水之分段萃取未經鹼處理> Example 2: Extraction from sparse peach (young peach) <Extraction solvent: Separate extraction with ethanol, hexane / water without alkali treatment>
冷凍疏果桃(幼桃)先經過微波爐解凍15分鐘,以粉碎機微細粉碎,並加以乾燥。之後於粉末50g中加入95%乙醇300mL及精製水37.5mL,再於42℃、30分鐘之攪拌下萃取30分鐘。然後將該萃取物減壓過濾,並於濾液中加入己烷300mL及精製水150mL加以攪拌並分段萃取。之後 回收己烷層,該溶劑以蒸餾裝置減壓濃縮,將殘渣以60℃減壓乾燥,製得綠色固形物486.0mg。 The frozen sparse peach (young peach) was thawed for 15 minutes in a microwave oven, pulverized finely with a pulverizer, and dried. Thereafter, 300 mL of 95% ethanol and 37.5 mL of purified water were added to 50 g of the powder, and extracted at 42 ° C. for 30 minutes with stirring for 30 minutes. Then, the extract was filtered under reduced pressure, and 300 mL of hexane and 150 mL of purified water were added to the filtrate, stirred, and extracted in stages. after that The hexane layer was recovered, the solvent was concentrated under reduced pressure in a distillation apparatus, and the residue was dried under reduced pressure at 60 ° C to obtain 486.0 mg of a green solid.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,其結果如下。 The obtained extract was measured for Neuramin content (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, and the results were as follows.
神經醯胺含量(純度):2.2% Nervamine content (purity): 2.2%
DPPH活性:22.5% DPPH activity: 22.5%
總多酚含量:3.4mg/g Total polyphenol content: 3.4mg / g
實施例3:由桃加工殘渣製造萃取物 <脫脂處理後 萃取溶劑:單獨用乙醇 己烷/水之分段萃取> Example 3: Manufacturing extracts from peach processing residues <Extraction solvent after degreasing: Separate extraction with ethanol and hexane / water>
先將桃榨汁製造後之榨渣(桃加工殘渣)乾燥,再於該桃加工殘渣200g中加入己烷800mL,並於70℃下攪拌4小時進行脫脂處理。再將脫脂處理後之桃加工殘渣減壓過濾並回收。之後於獲得之脫脂處理後的桃加工殘渣中加入95%乙醇800mL,並於70℃下萃取60分鐘,經過減壓過濾而獲得萃取液。再將萃取殘渣再次同樣處理獲得萃取液。 First, the pressed residue (peach processing residue) after the production of the peach juice was dried, and then 800 mL of hexane was added to 200 g of the peach processing residue, and the mixture was stirred at 70 ° C. for 4 hours for degreasing treatment. The peach processing residue after the degreasing treatment was filtered under reduced pressure and recovered. Then, 800 mL of 95% ethanol was added to the obtained peach-processed residue after the degreasing treatment, and extraction was performed at 70 ° C. for 60 minutes, followed by filtering under reduced pressure to obtain an extract. The extraction residue was treated again to obtain an extract.
之後將兩萃取液合併,並以95%乙醇調整成容量1600mL,再加入己烷1600mL,並於70℃下攪拌60分鐘。之後再次加入精製水1600mL,於70℃下,分段萃取60分鐘。之後回收己烷層,該溶劑以蒸餾裝置減壓濃縮,將殘渣以60℃減壓乾燥,製得褐色固形物4.36g。 After that, the two extracts were combined, adjusted to a capacity of 1600 mL with 95% ethanol, and then 1600 mL of hexane was added, followed by stirring at 70 ° C. for 60 minutes. After that, 1600 mL of purified water was added again, and the extraction was performed at 70 ° C. for 60 minutes in stages. Thereafter, the hexane layer was recovered, and the solvent was concentrated under reduced pressure in a distillation apparatus, and the residue was dried under reduced pressure at 60 ° C to obtain 4.36 g of a brown solid.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量, 其結果如下。 The obtained extract was then used to determine the Neuramin content (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, The results are as follows.
神經醯胺含量(純度):8.8% Nervamine content (purity): 8.8%
DPPH活性:72.7% DPPH activity: 72.7%
總多酚含量:7.6mg/g Total polyphenol content: 7.6mg / g
實施例4:由桃加工殘渣製造萃取物 <萃取溶劑:單獨用乙醇 己烷/水之分段萃取經鹼處理> Example 4: Extraction from Peach Processing Residue <Extraction solvent: Separate extraction with ethanol, hexane / water, and alkali treatment>
在未乾燥之桃加工殘渣100g中加入95%乙醇200mL(含氫氧化鈉6.4g)及精製水25mL,於42℃、30分鐘之攪拌下萃取。再將該萃取物減壓過濾獲得萃取液,並將萃取殘渣再次同樣處理獲得萃取液。將兩萃取液合併,加入己烷400mL及精製水200mL,再攪拌1小時並分段萃取。之後回收己烷層,該溶劑再以蒸餾裝置減壓濃縮,將殘渣以60℃減壓乾燥,製得橙色固形物131.3mg。 200 g of 95% ethanol (containing 6.4 g of sodium hydroxide) and 25 mL of purified water were added to 100 g of undried peach processing residues, and extracted at 42 ° C. with stirring for 30 minutes. The extract was filtered under reduced pressure to obtain an extract, and the extraction residue was treated again to obtain an extract. The two extracts were combined, 400 mL of hexane and 200 mL of purified water were added, and the mixture was stirred for 1 hour and extracted in stages. Then, the hexane layer was recovered, and the solvent was concentrated under reduced pressure in a distillation apparatus, and the residue was dried under reduced pressure at 60 ° C to obtain 131.3 mg of an orange solid.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,其結果如下。 The obtained extract was measured for Neuramin content (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, and the results were as follows.
神經醯胺含量(純度):10.7% Nervamine content (purity): 10.7%
DPPH活性:22.2% DPPH activity: 22.2%
總多酚含量:4.3mg/g Total polyphenol content: 4.3mg / g
實施例5:由桃加工殘渣製造萃取物 <萃取溶劑:單獨用乙醇 己烷/水之分段萃取未經鹼處理> Example 5: Extraction from Peach Processing Residue <Extraction solvent: Separate extraction with ethanol, hexane / water without alkali treatment>
在未乾燥之桃加工殘渣100g中加入95%乙醇200mL 及精製水25mL,於42℃、30分鐘之攪拌下萃取。再將該萃取物減壓過濾獲得萃取液,並將萃取殘渣再次同樣處理獲得萃取液。將兩萃取液合併,加入己烷400mL及精製水200mL,再攪拌1小時並分段萃取。之後回收己烷層,該溶劑再以蒸餾裝置減壓濃縮,將殘渣以60℃減壓乾燥,製得橙色固形物172.1mg。 Add 100 mL of 95% ethanol to 100 g of undried peach processing residue And 25 mL of purified water, and extracted at 42 ° C with stirring for 30 minutes. The extract was filtered under reduced pressure to obtain an extract, and the extraction residue was treated again to obtain an extract. The two extracts were combined, 400 mL of hexane and 200 mL of purified water were added, and the mixture was stirred for 1 hour and extracted in stages. Thereafter, the hexane layer was recovered, and the solvent was concentrated under reduced pressure in a distillation apparatus, and the residue was dried under reduced pressure at 60 ° C to obtain 172.1 mg of an orange solid.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,其結果如下。 The obtained extract was measured for Neuramin content (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, and the results were as follows.
神經醯胺含量(純度):11.7% Nervamine content (purity): 11.7%
DPPH活性:61.9% DPPH activity: 61.9%
總多酚含量:4.4mg/g Total polyphenol content: 4.4mg / g
實施例6:由桃加工殘渣製造萃取物 <萃取溶劑:乙醇/己烷之混合液 己烷/水分段萃取> Example 6: Extraction from Peach Processing Residue <Extraction solvent: ethanol / hexane mixed solution hexane / water staged extraction>
在未乾燥之桃加工殘渣100g中加入95%乙醇200mL、己烷100mL及精製水25mL,於42℃、30分鐘之攪拌下萃取。再將該萃取物減壓過濾獲得萃取液,並於濾液中加入己烷100mL及精製水100mL,之後於42℃下攪拌1小時,以己烷/水分段萃取。然後回收己烷層,該溶劑再以蒸餾裝置減壓濃縮,將殘渣以60℃減壓乾燥,製得橙色固形物177.8mg。 To 100 g of undried peach processing residues, 200 mL of 95% ethanol, 100 mL of hexane, and 25 mL of purified water were added, and extracted at 42 ° C. with stirring for 30 minutes. The extract was filtered under reduced pressure to obtain an extract, and 100 mL of hexane and 100 mL of purified water were added to the filtrate, and the mixture was stirred at 42 ° C. for 1 hour, and then extracted with hexane / water in stages. Then, the hexane layer was recovered, the solvent was concentrated under reduced pressure in a distillation apparatus, and the residue was dried under reduced pressure at 60 ° C to obtain 177.8 mg of an orange solid.
該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,結果如下。 The obtained extract was measured for the content of neural cramine (purity), DPPH activity, and total polyphenol content in accordance with Test Examples 1, 2, and 3, and the results were as follows.
神經醯胺含量(純度):10.7% Nervamine content (purity): 10.7%
DPPH活性:21.4% DPPH activity: 21.4%
總多酚含量:1.4mg/g Total polyphenol content: 1.4mg / g
實施例7:由桃加工殘渣製造萃取物 <萃取溶劑:單獨用乙醇 己烷/水之分段萃取> Example 7: Extraction from Peach Processing Residue <Extraction solvent: Separate extraction with ethanol, hexane / water>
在乾燥之桃加工殘渣50g中加入95%乙醇200mL,於42℃、30分鐘之攪拌下萃取。該萃取物經減壓過濾,並以95%乙醇50mL排出。該殘渣以同樣之方法再次萃取,經減壓過濾後排出。之後於合併之濾液(150mL)中加入己烷150mL,並攪拌30分鐘,接著再加入蒸餾水150mL,攪拌處理30分鐘進行己烷/水之分段萃取。之後回收己烷層並進行減壓濃縮,將殘渣減壓乾燥後,所製得之萃取物為橙色糖漿狀物質3.85g。 200 mL of 95% ethanol was added to 50 g of the dried peach processing residue, and extracted at 42 ° C. with stirring for 30 minutes. The extract was filtered under reduced pressure and discharged with 50 mL of 95% ethanol. The residue was extracted again in the same manner, and filtered off under reduced pressure and discharged. Then, 150 mL of hexane was added to the combined filtrate (150 mL), and the mixture was stirred for 30 minutes. Then, 150 mL of distilled water was added, and the mixture was stirred for 30 minutes to perform hexane / water stepwise extraction. Thereafter, the hexane layer was recovered and concentrated under reduced pressure, and the residue was dried under reduced pressure. The obtained extract was 3.85 g of an orange syrupy substance.
再對該獲得之萃取物,再依照上述試驗例1、2及3,測定神經醯胺含量(純度)、DPPH活性及總多酚含量,其結果如下。 With respect to the obtained extract, according to the above-mentioned Test Examples 1, 2 and 3, the Neuramin content (purity), DPPH activity, and total polyphenol content were measured. The results are as follows.
神經醯胺含量(純度):2.4% Nervamine content (purity): 2.4%
DPPH活性:36.5% DPPH activity: 36.5%
總多酚含量:29.2mg/g Total polyphenol content: 29.2mg / g
實施例8:對桃原料之萃取液之己烷/水的分段萃取條件之檢討 Example 8: Review of hexane / water staged extraction conditions of peach raw material extract
先對乾燥之桃加工殘渣加以脫脂處理,再對經95%乙醇萃取的一次萃取液,以下述表1記載之溶劑比(一次萃取液:己烷:水),檢討己烷/水之分段萃取的溶劑容量之比。 Degrease the dried peach processing residues first, and then review the hexane / water segmentation based on the solvent ratio (primary extraction solution: hexane: water) described in Table 1 below for the primary extraction solution extracted with 95% ethanol. Extracted solvent capacity ratio.
先在試管中加入一次萃取液,接著加入己烷並激烈振盪10秒鐘,其次加入水,並再激烈振盪10秒鐘後靜置,檢討溶液之分離狀態。 First add the extract once to the test tube, then add hexane and shake vigorously for 10 seconds, then add water, and shake vigorously for another 10 seconds, then let it stand and review the separation state of the solution.
同時,對己烷層(上清液層),以感光密度計,對薄層層析(TLC),比較神經醯胺之含量。 At the same time, the content of neuraminine was compared with respect to the hexane layer (supernatant layer) and thin layer chromatography (TLC) in terms of sensitivity.
接著以經過一次萃取液:己烷:水=1:1:1萃取處理時之神經醯胺含量為100%,比較各混合比之神經醯胺量。 Then, the content of Neuramin during the extraction treatment with one extraction solution: hexane: water = 1: 1: 1 is 100%, and the amount of Neuramin in each mixing ratio is compared.
其結果,如下述表1所示。 The results are shown in Table 1 below.
注1:分離度所表示之意如下。 Note 1: The meaning of resolution is as follows.
◎:在10分鐘內即可分離,分離極為良好。 :: Separation is possible within 10 minutes, and the separation is extremely good.
○:無須分離時間,30分鐘以內可良好地分離。 ○: No separation time is required, and good separation can be achieved within 30 minutes.
△:分離須30分鐘以上,可見到中間層,但大致可分離。 △: It takes more than 30 minutes to separate, and the intermediate layer is visible, but it is roughly separable.
×:為乳化之狀態,無法分離。 ×: It is in an emulsified state and cannot be separated.
由以上之結果判斷,在本發明自桃原料以一次萃取溶劑、接著以己烷/水之分段萃取中,一次萃取中之萃取液、及萃取液之分段萃取使用的己烷及水的容量比,可以良好地理解在1:0.5:0.5至1:2:2時,分離度及神經醯胺的回收量良好。 Judging from the above results, in the present invention, the hexane and water used in the one-stage extraction of the hexane and water in the one-stage extraction of the solvent from the peach raw material followed by the hexane / water stage extraction are used. The capacity ratio can be well understood. When the ratio is 1: 0.5: 0.5 to 1: 2: 2, the resolution and the recovered amount of ceramide are good.
由上述所示之各實施例可知,本發明由桃原料使用特別之萃取方法,可有效地獲得具有活性氧清除能的桃萃取物。 As can be seen from the examples shown above, the present invention can effectively obtain a peach extract having active oxygen scavenging energy by using a special extraction method from a peach raw material.
而且所獲得之萃取物不只具有活性氧清除能,亦含有桃神經醯胺,同時,其萃取溶劑,在使用乙醇及己烷之點方面的安全性亦高,且將此類溶劑適當組合,再經由對應各目的之萃取技法,即可調製含目的桃神經醯胺的萃取物之點,亦極為特別。 In addition, the obtained extract not only has active oxygen scavenging energy, but also contains ceramide, and its extraction solvent is also highly safe in the point of using ethanol and hexane. Through the extraction technology corresponding to each purpose, the point that can prepare the extract containing the target peach nerve amine is also very special.
因此以本發明,可以安全之萃取方法,自桃製造含神經醯胺(神經鞘糖脂質)、醣苷、多酚,且具有活性氧清除能的桃萃取物。 Therefore, according to the present invention, a peach extract containing ceramide (sphingomyelin), glycosides, polyphenols, and active oxygen scavenging ability can be produced from peaches by a safe extraction method.
以本發明所獲得之桃萃取物,可經其萃取所使用的萃取溶劑之各種組合,獲得可變化目的含有成分之含量的桃萃取物,而可提供提高如桃神經醯胺含量之萃取物,而且,在適當組合活性碳處理及層析等精製方法時,可再提供提高精製度之萃取物,而可使用作為食品、化妝品或準藥品,及該等之加工品之素材。 The peach extract obtained by the present invention can be used to extract various combinations of extraction solvents used to obtain peach extracts that can vary the content of the ingredients contained in the target, and can provide extracts that increase the content of peach neural amine, In addition, when an appropriate combination of purification methods such as activated carbon treatment and chromatography can be used to provide extracts that enhance the purification system, they can be used as food, cosmetics, or quasi-drugs, as well as processed materials.
並且,原料方面,係桃之生產過程中所產生之疏果桃 (幼桃)、或桃之果汁等加工步驟中所產生之桃加工殘渣,在可有效利用副產物之點方面,亦極為特別。 And, in terms of raw materials, it is the sparse fruit peach produced in the production process of peach (Young peach), or peach processing residues produced in processing steps such as peach juice are also very special in terms of the effective use of by-products.
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