CN101524099A - Method of utilizing supercritical CO2 extraction technology to prepare primitive coconut oil - Google Patents
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Abstract
本发明公开了一种超临界CO2萃取技术制备原生态椰子油的方法,包括原料前处理过程、萃取过程、产物分离过程。将椰子去壳、刨丝后干燥、粉碎;然后用超临界CO2流体对椰肉粉末进行萃取,其间以乙醇为夹带剂,得到萃取物;利用压力增减释放法将萃取物中的超临界CO2流体变为气体回收,然后降温放置使VCO凝固并与乙醇分层,倾出乙醇,即可得到香气浓郁的原生态椰子油。本发明工艺过程简单、快速、高效、条件温和,可以最大限度地保存椰子油中的天然活性成分,所得VCO清亮,有浓郁的椰子油固有的香气,具有多种保健功能,促进了我国椰子油产业中原生态椰子油加工业的发展。The invention discloses a method for preparing original ecological coconut oil by a supercritical CO2 extraction technology, which includes a raw material pretreatment process, an extraction process and a product separation process. The coconut is shelled, shredded, dried and crushed; then the coconut meat powder is extracted with supercritical CO2 fluid, and ethanol is used as an entraining agent to obtain the extract; The CO 2 fluid is changed to gas recovery, and then the temperature is lowered to allow the VCO to solidify and be layered with ethanol, and the ethanol is poured out to obtain the original ecological coconut oil with a strong aroma. The technological process of the present invention is simple, fast, efficient and mild, and can preserve the natural active ingredients in coconut oil to the greatest extent. The development of the original eco-coconut oil processing industry in the industry.
Description
技术领域 technical field
本发明涉及一种原生态椰子油的制备方法,属农产品产后加工技术领域。The invention relates to a method for preparing raw ecological coconut oil, which belongs to the technical field of post-production processing of agricultural products.
技术背景 technical background
原生态椰子油(Virgin coconut oil,简称VCO),按菲律宾国家标准局(The Philippine National Standards,PNS)规定,是用机械或天然的方法,从新鲜、成熟的椰子肉中提取椰子油,不用化学方法进行精炼、漂白或除臭而生产出来的一种不改变椰子油天然性质的产品。VCO在我国台湾地区被称为“处女椰子油”。由于加工时不添加任何化学品,不需要精炼,因此原生态椰子油更多地保留了椰子油原有的生物活性成分,例如维生素E、生育三烯和多酚类化合物等,与一般方法制备的椰子油相比,原生态椰子油更安全、更有益。原生态椰子油具有椰子的天然香味,游离脂肪酸含量低于0.1%,其脂肪酸的碳链分布属于正常范围,饱和脂肪酸和不饱和脂肪酸的组成合理。据报道,VCO具有降低血液中胆固醇、甘油三脂、磷脂、低密度脂蛋白(LDL)和超低密度脂蛋白胆固醇水平的功能;减少羟基等体内自由基的抗氧化功能;破坏单细胞增生李斯特菌、幽门螺旋菌等菌类的抗菌功能;抗HIV、单纯孢疹病毒-1、流行性感冒病毒和细胞巨化病毒等抗病毒功能。目前,原生态椰子油在食品、医药、日用化妆品等行业的用途越来越广泛。在菲律宾、印度尼西亚等国家,原生态椰子油的生产工业发展也很快。K.G.Nevin和T.Rajamohan(2004)报道,VCO的加工工艺为:将成熟椰子的固体胚乳磨碎,制成粘稠的浆状物,用细纱布压榨以获得椰乳,冷却48h,然后缓慢加热到50℃,将所得原生态椰子油用细纱布过虑即得原生态椰子油。该法操作简单,工艺中也无加热和化学工序。但耗时较长,油脂制取虑也低。目前国内有利用水酶法制备VCO的报道,但水酶法作用时间长,工艺复杂,酶解产物易造成油脂酸败。Virgin coconut oil (VCO), according to the Philippine National Standards (The Philippine National Standards, PNS), is to use mechanical or natural methods to extract coconut oil from fresh, mature coconut meat without chemical A product that does not alter the natural properties of coconut oil by refining, bleaching or deodorizing it. VCO is called "virgin coconut oil" in Taiwan. Since no chemicals are added during processing and no refining is required, raw coconut oil retains more of the original biologically active components of coconut oil, such as vitamin E, tocotriene and polyphenolic compounds, which are prepared by common methods Raw coconut oil is safer and more beneficial than natural coconut oil. Raw coconut oil has the natural fragrance of coconut, the content of free fatty acid is less than 0.1%, the carbon chain distribution of its fatty acid belongs to the normal range, and the composition of saturated fatty acid and unsaturated fatty acid is reasonable. According to reports, VCO has the function of reducing blood cholesterol, triglycerides, phospholipids, low-density lipoprotein (LDL) and ultra-low-density lipoprotein cholesterol levels; reducing the antioxidant function of free radicals such as hydroxyl groups in the body; destroying single-cell hyperplasia Antibacterial function of special bacteria, Helicobacter pylori and other fungi; anti-HIV, herpes simplex virus-1, influenza virus and cytomegalovirus and other antiviral functions. At present, raw coconut oil is more and more widely used in industries such as food, medicine, and daily cosmetics. In the Philippines, Indonesia and other countries, the production industry of raw ecological coconut oil is also developing rapidly. K.G.Nevin and T.Rajamohan (2004) reported that the processing technology of VCO is as follows: the solid endosperm of mature coconut is ground to make a viscous slurry, pressed with fine gauze to obtain coconut milk, cooled for 48h, and then slowly heated When the temperature reaches 50°C, filter the obtained original ecological coconut oil with fine gauze to obtain original ecological coconut oil. The method is simple to operate, and there is no heating and chemical process in the process. But it takes a long time, and the oil production concerns are also low. At present, there are domestic reports on the preparation of VCO by the aqueous enzymatic method, but the aqueous enzymatic method takes a long time to act, the process is complicated, and the enzymatic hydrolysis product is easy to cause oil rancidity.
超临界二氧化碳萃取技术是一种新型的提取分离技术,具有操作简单、高效、快速、操作条件温和、对有效成分的破坏少、而且易于分离等特点,适合于对生物、食品、化妆品和药物等的提取和纯化。近年来,超临界萃取技术在动植物油脂的提取分离及其有效成分的提取分离中应用的非常广泛和深入。超临界二氧化碳萃取技术的最大特点就是对物料中的有效成分破坏很小、操作简单、快速。Supercritical carbon dioxide extraction technology is a new type of extraction and separation technology. It has the characteristics of simple operation, high efficiency, fast speed, mild operating conditions, less damage to active ingredients, and easy separation. It is suitable for biological, food, cosmetics and pharmaceuticals, etc. extraction and purification. In recent years, supercritical extraction technology has been widely and deeply used in the extraction and separation of animal and vegetable oils and their active ingredients. The biggest feature of supercritical carbon dioxide extraction technology is that it has little damage to the active ingredients in the material, and the operation is simple and fast.
发明内容 Contents of the invention
本发明的目的是提供一种超临界CO2萃取技术制备原生态椰子油的方法,该方法提取工艺简单、快速,可对椰子油的天然活性成分实现最大程度的保护;提取率高,所得原生态椰子油质量好,品质优。The purpose of this invention is to provide a kind of supercritical CO Extraction technology prepares the method for original ecology coconut oil, and this method extraction process is simple, fast, can realize the protection to the maximum degree to the natural active ingredient of coconut oil; Eco Coconut Oil is of good quality and excellent quality.
本发明的原理如下:Principle of the present invention is as follows:
超临界CO2流体是处于临界温度(TC=31.1℃)和临界压力(PC=7.38MPa)以上的非凝缩性的高密度流体,具有优异的溶剂性质,粘度低,密度大,有较好的流动、传质、传热和溶解性能。CO2流体处于超临界状态时,其密度接近于液体密度,并且随流体压力和温度的改变发生十分明显的变化,而溶质在超临界流体中的溶解度随超临界流体密度的增大而增大。夹带剂是指超临界流体气体中加入的一种少量的可与之混溶的、挥发性介于被分离物质与超临界组分之间的物质,通常能使超临界流体的萃取能力增强,降低操作压力,降低能耗。在较高压力下,超临界CO2流体将椰子油溶解于流体中,其间,以95%乙醇为夹带剂,然后降低流体溶液的压力或升高流体溶液的温度,使超临界CO2流体与原生态椰子油的混溶物中CO2密度下降,溶解度降低而析出,再利用乙醇的凝固点比VCO的凝固点高的特点使VCO凝固后将乙醇和VCO分离,从而实现对椰子油的萃取。由于CO2稳定、无毒、安全、廉价,临界温度和临界压力低(TC=31.1℃,PC=7.38MPa),操作条件温和,因此,对椰子油中有效成分的破坏极少,而且易于分离,适合于提取原生态椰子油,剩余的脱脂椰子粉可以用来提取椰子分离蛋白、椰子活性多糖等成分,利于实现对椰子的综合利用,变废为宝。Supercritical CO 2 fluid is a non-condensable high-density fluid above the critical temperature (T C =31.1°C) and critical pressure (P C =7.38MPa), with excellent solvent properties, low viscosity, high density, and Good flow, mass transfer, heat transfer and solubility properties. When the CO2 fluid is in a supercritical state, its density is close to that of the liquid, and it changes significantly with the change of fluid pressure and temperature, and the solubility of solute in the supercritical fluid increases with the increase of the density of the supercritical fluid . Entrainer refers to a small amount of miscible substance added to the supercritical fluid gas, whose volatility is between the separated substance and the supercritical component, which usually enhances the extraction ability of the supercritical fluid. Reduce operating pressure and reduce energy consumption. Under higher pressure, the supercritical CO2 fluid dissolves coconut oil in the fluid, during which, 95% ethanol is used as an entrainer, and then the pressure of the fluid solution is reduced or the temperature of the fluid solution is raised to make the supercritical CO2 fluid and The density of CO 2 in the miscible of raw coconut oil decreases, the solubility decreases and precipitates, and then the freezing point of ethanol is higher than that of VCO to separate ethanol and VCO after VCO is solidified, so as to realize the extraction of coconut oil. Because CO 2 is stable, nontoxic, safe, cheap, critical temperature and critical pressure are low (T C =31.1 ℃, P C =7.38MPa), and operating conditions are mild, therefore, the destruction of active ingredients in coconut oil is very little, and It is easy to separate and is suitable for extracting raw ecological coconut oil. The remaining defatted coconut powder can be used to extract coconut protein isolate, coconut active polysaccharide and other components, which is beneficial to realize the comprehensive utilization of coconut and turn waste into treasure.
本发明所采用的技术方案是:The technical scheme adopted in the present invention is:
超临界CO2萃取技术制备原生态椰子油的方法,包括原料前处理过程、萃取过程、产物分离过程,其步骤如下:Supercritical CO Extraction technology prepares the method for original ecology coconut oil, comprises raw material pretreatment process, extraction process, product separation process, and its steps are as follows:
一、原料前处理过程:选择成熟老椰子果实,经去壳、去种皮、清洗、刨丝后于低温下干燥使椰肉含水量小于7%,粉碎,过筛,得到椰肉粉末。1. Raw material pretreatment process: select ripe old coconut fruit, after shelling, peeling, cleaning, shredding, dry at low temperature to make the water content of coconut meat less than 7%, pulverize and sieve to obtain coconut meat powder.
二、萃取过程:用超临界CO2流体在压力25~40MPa、温度35~45℃、CO2流量10~25L/h的条件下萃取椰肉粉末1~3小时,得到萃取物。其间,添加95%乙醇为夹带剂,按重量比计添加量为椰肉粉末的35~45%。2. Extraction process: use supercritical CO2 fluid to extract the coconut meat powder for 1 to 3 hours under the conditions of pressure 25~40MPa, temperature 35~45°C, CO2 flow 10~25L/h, to obtain the extract. Meanwhile, adding 95% ethanol is an entraining agent, and the addition amount is 35~45% of coconut meat powder by weight.
三、产物分离过程:利用压力增减释放法使萃取物在4~10MPa、温度45~60℃的条件下分离,超临界CO2流体变为气体被回收,所余物在常温常压下放置使CO2挥发干净,然后在4~15℃下放置使VCO凝固并与乙醇分层(由于VCO的凝固点为26~28℃,乙醇的凝固点为-114℃,VCO凝固居于下层,乙醇仍然为液态处于上层),倾出乙醇,即可得到常温下清亮的、略显黄色、香气浓郁的原生态椰子油。3. Product separation process: use the pressure increase and decrease release method to separate the extract under the conditions of 4-10MPa and temperature 45-60°C, the supercritical CO2 fluid becomes gas and is recovered, and the rest is placed at normal temperature and pressure Make the CO 2 volatilize cleanly, and then place it at 4-15°C to solidify the VCO and layer it with ethanol (since the freezing point of VCO is 26-28°C and the freezing point of ethanol is -114°C, VCO solidifies and resides in the lower layer, and ethanol is still liquid In the upper layer), pour out the ethanol to obtain the clear, slightly yellow, and rich-flavored original ecological coconut oil at room temperature.
本发明工艺简单,成本低,利用超临界CO2萃取技术制备原生态椰子油快速、安全、对椰子油的活性成份破坏极小,采用夹带剂能有效地提高提取率,提升产品品质,所得VCO清亮、具有浓郁的椰子油香气,剩余的脱脂椰子粉可以用来提取椰子分离蛋白、椰子活性多糖等成分,利于实现对椰子的综合利用。The process of the present invention is simple, and cost is low, utilizes supercritical CO Extraction technology to prepare original ecology coconut oil fast, safe, very little damage to the active component of coconut oil, adopt entrainer to effectively improve extraction rate, improve product quality, obtained VCO It is clear and has a strong aroma of coconut oil. The remaining defatted coconut powder can be used to extract coconut protein isolate, coconut active polysaccharide and other components, which is beneficial to the comprehensive utilization of coconut.
具体实施方式 Detailed ways
下面结合非限定性实施例对本发明作进一步说明。The present invention will be further described below in conjunction with non-limiting examples.
实施例一、Embodiment one,
一、原料前处理过程:选择生长期在12个月以上的老椰子果实(这种椰子果实肉厚,含油量高),去壳,削皮,清洗、刨丝,然后将椰子肉丝在45℃的温度下干燥3小时,使椰子肉中水分含量小于7%,再粉碎,过20目筛。1. The raw material pretreatment process: select the old coconut fruit with a growth period of more than 12 months (this kind of coconut fruit has thick flesh and high oil content), shells, peels, cleans, shreds, and then shreds the coconut meat at 45 Dry at a temperature of 10°C for 3 hours, make the moisture content in the coconut meat less than 7%, then pulverize and cross a 20-mesh sieve.
二、萃取过程:用超临界CO2流体在压力30MPa、温度45℃、CO2流量25L/h的条件下萃取椰肉粉末1.5小时,得到萃取物。以95%乙醇为夹带剂,添加量为椰肉粉末的40%(v/m)。2. Extraction process: use supercritical CO2 fluid to extract the copra powder for 1.5 hours under the conditions of pressure 30MPa, temperature 45°C, CO2 flow rate 25L/h, to obtain the extract. With 95% ethanol as entrainer, the addition is 40% (v/m) of coconut meat powder.
三、产物分离过程:利用压力增减释放法使萃取物在8MPa、温度42℃的条件下分离,超临界CO2流体变为气体被回收,所余物在常温常压下放置1小时使CO2挥发干净,然后在12℃下放置使VCO凝固并与乙醇分层,倾出乙醇,即可得到常温下清亮的、略显黄色、香气浓郁的原生态椰子油。VCO提取率可以达到85%~88%。3. Product separation process: Use the pressure increase and decrease release method to separate the extract at 8 MPa and a temperature of 42°C. The supercritical CO 2 fluid becomes a gas and is recovered, and the rest is placed at normal temperature and pressure for 1 hour to make the CO 2. Volatilize cleanly, then place it at 12°C to solidify the VCO and separate it with ethanol, pour out the ethanol, and you can get clear, slightly yellow, and rich-flavored original ecological coconut oil at room temperature. The VCO extraction rate can reach 85% to 88%.
实施例二、Embodiment two,
一、原料前处理:选择生长期在12个月以上的老椰子果实(这种椰子果实肉厚,含油量高),去壳,削皮,清洗、刨丝,然后将椰子肉丝在40℃的温度下干燥3小时,使椰子肉中水分含量小于7%,再粉碎,过40目筛。1. Pre-treatment of raw materials: select old coconut fruit with a growth period of more than 12 months (this kind of coconut fruit has thick meat and high oil content), shells, peels, cleans, shreds, and then shredded coconut meat at 40 ° C Under the temperature of drying for 3 hours, make the moisture content in the coconut meat be less than 7%, pulverize again, cross 40 mesh sieves.
二、萃取过程:用超临界CO2流体在压力35MPa、温度45℃、CO2流量20L/h的条件下萃取椰肉粉末1.5小时,得到萃取物。以95%乙醇为夹带剂,添加量为椰肉粉末的40%(v/m)。2. Extraction process: use supercritical CO2 fluid to extract the copra powder for 1.5 hours under the conditions of pressure 35MPa, temperature 45°C, CO2 flow rate 20L/h, to obtain the extract. With 95% ethanol as entrainer, the addition is 40% (v/m) of coconut meat powder.
三、产物分离过程:利用压力增减释放法使萃取物在5MPa、温度48℃的条件下分离,超临界CO2流体变为气体被回收,所余物在常温常压下放置1小时使CO2挥发干净,然后在8℃下放置使VCO凝固并与乙醇分层,倾出乙醇,即可得到常温下清亮的、略显黄色、香气浓郁的原生态椰子油。VCO提取率可以达到86%~90%。3. Product separation process: Use the pressure increase and decrease release method to separate the extract at 5MPa and a temperature of 48°C. The supercritical CO 2 fluid becomes a gas and is recovered, and the rest is placed at normal temperature and pressure for 1 hour to make the CO 2 Volatilize cleanly, then place at 8°C to solidify the VCO and separate layers with ethanol, pour out the ethanol, and you can get clear, slightly yellow, and rich-flavored original ecological coconut oil at room temperature. The extraction rate of VCO can reach 86%-90%.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102936532A (en) * | 2012-11-22 | 2013-02-20 | 海南建邦制药科技有限公司 | Extraction process of coconut oil |
CN106967494A (en) * | 2016-12-04 | 2017-07-21 | 文昌椰村人家椰子加工专业合作社 | A kind of method for extracting coconut oil |
CN107624945A (en) * | 2016-12-06 | 2018-01-26 | 胡方芽 | A kind of coconut ash ice cream |
CN110452788A (en) * | 2019-09-03 | 2019-11-15 | 北京汇真源科技有限公司 | A kind of fruits and vegetables cleaning agent and preparation method thereof |
CN111302908A (en) * | 2020-02-13 | 2020-06-19 | 厦门大学 | A kind of method for supercritical carbon dioxide extraction and separation of triethylene glycol and triethylene glycol monomethyl ether |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102936532A (en) * | 2012-11-22 | 2013-02-20 | 海南建邦制药科技有限公司 | Extraction process of coconut oil |
CN106967494A (en) * | 2016-12-04 | 2017-07-21 | 文昌椰村人家椰子加工专业合作社 | A kind of method for extracting coconut oil |
CN107624945A (en) * | 2016-12-06 | 2018-01-26 | 胡方芽 | A kind of coconut ash ice cream |
CN110452788A (en) * | 2019-09-03 | 2019-11-15 | 北京汇真源科技有限公司 | A kind of fruits and vegetables cleaning agent and preparation method thereof |
CN110452788B (en) * | 2019-09-03 | 2021-08-27 | 北京汇真源科技有限公司 | Fruit and vegetable cleaning agent and preparation method thereof |
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