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CN102388988B - Separated extraction method of microorganism oil - Google Patents

Separated extraction method of microorganism oil Download PDF

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CN102388988B
CN102388988B CN 201110350200 CN201110350200A CN102388988B CN 102388988 B CN102388988 B CN 102388988B CN 201110350200 CN201110350200 CN 201110350200 CN 201110350200 A CN201110350200 A CN 201110350200A CN 102388988 B CN102388988 B CN 102388988B
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oil
surfactant
solid
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microbial oil
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CN102388988A (en
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魏芳
江木兰
董绪燕
陈洪
杨湄
黄凤洪
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Oil Crops Research Institute of Chinese Academy of Agriculture Sciences
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Abstract

The invention relates to a separated extraction method of microorganism oil, which is characterized by comprising the following steps: firstly, homogenizing, stirring microorganism oil to be in separated extraction uniformly; secondly, breaking crystals; thirdly, cooling and crystallizing, crystallizing the heat-insulation microorganism oil for 4-7h at the temperature being 4 DEG C, and then arranging the heat-insulation microorganism oil for 1-4h at the low temperature being 10 DEG C, thus obtaining thick slurry containing solid crystallization; fourthly, adding surface active agent water solution in the thick slurry containing solid crystallization, and stirring, thus obtaining elusion system; fifthly, conducting centrifugal separation to obtain liquid oil, standing the emulsion system for 1-5h at the low temperature being 5-10 DEG C, centrifuging the emulsion system in a cooling centrifuge, separating liquid components in a light phase mode, putting the liquid components in light phase in water for cleaning, and dehydrating and drying the liquid components in light phase, thus obtaining the liquid oil of the microorganism oil; and sixthly, breaking the emulsion to obtain solid grease. The liquid oil of the microorganism separated and extracted by the method is not easy to solidify at lower temperature, the method procedure is simple and the cost is low.

Description

一种微生物油的分提方法A kind of fractionation method of microbial oil

技术领域 technical field

本发明属于食品科学领域,具体涉及一种微生物油的分提方法。The invention belongs to the field of food science, and in particular relates to a method for fractionating microbial oil.

背景技术 Background technique

微生物油脂是继植物油脂、动物油脂之后开发出来的又一种人类食用油脂新资源。微生物油脂又称单细胞油脂,是由酵母、霉菌、细菌和藻类等微生物在一定条件下利用碳水化合物、碳氢化合物和普通油脂为碳源、氮源、辅以无机盐生产的油脂及另一些具有商业价值的脂质。微生物生产油脂不仅具有油脂含量高、生产周期短、不受季节影响、不占用耕地等优点,而且可用细胞融合、细胞诱变等方法,使微生物产生高营养油脂或某些特定脂肪酸组成的油脂,如含有花生四烯酸(ARA)、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)等长链多不饱和脂肪酸(LC-PUFAs)的功能性油脂。LC-PUFAs在预防心血管疾病、降血脂、降低胆固醇、减肥、抑制肿瘤生长、抗炎等方面具有明显的作用。20世纪90年代以来,开发利用微生物进行功能性油脂的生产已成为一大热点,如利用微生物培养生产ARA、EPA、DHA等营养价值高且具有特殊保健功能的功能油脂的研究。ARA属于ω-6系列长链多不饱和脂肪酸(LC-PUFA),它在人体内分布广泛,在脑和神经组织中含量一般占多不饱和脂肪酸总量的40%~50%,在神经末梢更高达70%,对大脑功能和视网膜发育是必不可少的物质;此外,ARA还具有促进生长发育的功能以及降血糖、降血脂和降低血液中胆固醇的作用。Microbial oil is another new human edible oil resource developed after vegetable oil and animal oil. Microbial oil, also known as single-cell oil, is oil produced by microorganisms such as yeast, mold, bacteria, and algae under certain conditions using carbohydrates, hydrocarbons, and ordinary oils as carbon sources, nitrogen sources, supplemented by inorganic salts, and other oils. Lipids of commercial value. Microbial oil production not only has the advantages of high oil content, short production cycle, not affected by seasons, and does not occupy cultivated land, but also can use methods such as cell fusion and cell mutagenesis to make microorganisms produce high-nutrition oil or oil composed of certain specific fatty acids. For example, functional oils containing long-chain polyunsaturated fatty acids (LC-PUFAs) such as arachidonic acid (ARA), eicosapentaenoic acid (EPA), and docosahexaenoic acid (DHA). LC-PUFAs have obvious effects in preventing cardiovascular diseases, lowering blood lipids, lowering cholesterol, losing weight, inhibiting tumor growth, and anti-inflammation. Since the 1990s, the development and utilization of microorganisms for the production of functional oils has become a hot spot, such as the research on the use of microorganisms to produce ARA, EPA, DHA and other functional oils with high nutritional value and special health functions. ARA belongs to the omega-6 series of long-chain polyunsaturated fatty acids (LC-PUFA), which is widely distributed in the human body, and its content in the brain and nerve tissues generally accounts for 40% to 50% of the total amount of polyunsaturated fatty acids. Up to 70%, it is an essential substance for brain function and retinal development; in addition, ARA also has the function of promoting growth and development, and the effect of lowering blood sugar, blood fat and blood cholesterol.

但微生物油在低温贮存时,会出现凝固,如在冬季温度较低时便会成为固态或半固态,不仅造成油品流动性能差,不便使用,不易储藏;还使油品的透明度降低,适口性变差,从而降低了微生物油的营养价值和油脂食品的质量。油脂分提是根据油脂中不同脂肪酸甘油三酯熔点差异,通过冷却使高熔点组分产生结晶,经过滤或离心分离得到熔点不同的组分。油脂分提可将组成复杂的天然油脂分级成相对单一的产品,实现不同熔点的液态油和固体脂的分离,以提高油脂对不同使用要求的适应性能,扩大油脂的用途,提高油脂的使用价值和经济价值。However, when microbial oil is stored at low temperature, it will solidify. For example, when the temperature is low in winter, it will become solid or semi-solid, which not only causes poor fluidity of the oil, is inconvenient to use, and is difficult to store; Poor performance, thereby reducing the nutritional value of microbial oil and the quality of oily food. Oil fractionation is based on the difference in the melting points of different fatty acid triglycerides in the oil, through cooling to crystallize the high melting point components, and obtaining components with different melting points through filtration or centrifugation. Oil fractionation can classify complex natural oils into relatively single products, realize the separation of liquid oils and solid fats with different melting points, improve the adaptability of oils to different use requirements, expand the use of oils, and increase the use value of oils and economic value.

目前油脂分提技术主要有干法分提、溶剂分提和表面活性剂分提。干法分提是指不加入任何溶剂,将处于溶解状态的油脂慢慢冷却到一定程度,然后过滤分离结晶,析出固体酯的方法。干法分提分为三个步骤:加热处理;用冷却法形成晶体原子核以及让晶体增长及成熟;用过滤把软脂从固体中分离出来。虽然干法分提有其独特优越性,但干法分提效率低,且固态脂中液体油含量较高,使固态脂和液态油的晶级低。溶剂分提法是指在油脂中按比例加入某一溶剂形成混合油体系,然后进行冷却结晶、分提的一种分提方法。溶剂分提法能形成容易过滤的稳定结晶,提高分离效果,增加分离产率,缩短分离时间,提高分离产品的纯度。溶剂分提法分提效率高,固态脂组分质量好。然而,由于结晶温度低以及分提过程中涉及溶剂损耗,其投资较大,生产费用高,用作溶剂的己烷,丙酮,异丙醇等具有易燃性。表面活性剂分提法是指在油脂冷却结晶后,添加表面活性剂,改善油和脂的界面张力,借脂和表面活性剂间的亲和力,形成脂在表面活性剂水溶液中的悬浮液,促进脂晶离析的方法。其工艺包括冷却结晶、表面活性剂湿润、离心分离以及表面活性剂回收等工序。表面活性剂法分提分离效率高,产品品质好,用途广,适用于大规模生产。At present, oil fractionation techniques mainly include dry fractionation, solvent fractionation and surfactant fractionation. Dry fractionation refers to the method of slowly cooling the dissolved oil to a certain extent without adding any solvent, and then filtering to separate crystals and precipitate solid esters. Dry fractionation is divided into three steps: heat treatment; cooling to form crystal nuclei and allow the crystals to grow and mature; and filtration to separate the palmitate from the solid. Although dry fractionation has its unique advantages, the efficiency of dry fractionation is low, and the liquid oil content in solid fat is relatively high, which makes the crystal grade of solid fat and liquid oil low. Solvent fractionation refers to a fractionation method in which a certain solvent is added to oil in proportion to form a mixed oil system, and then cooled and crystallized and fractionated. The solvent fractionation method can form stable crystals that are easy to filter, improve the separation effect, increase the separation yield, shorten the separation time, and improve the purity of the separation product. The solvent fractionation method has high fractionation efficiency and good quality of solid lipid components. However, due to the low crystallization temperature and solvent loss involved in the fractionation process, the investment is large and the production cost is high. The hexane, acetone, and isopropanol used as solvents are flammable. The surfactant fractionation method refers to adding a surfactant after the oil is cooled and crystallized to improve the interfacial tension between the oil and the fat, and to form a suspension of the fat in the aqueous surfactant solution by virtue of the affinity between the fat and the surfactant to promote Method of Lipid Crystal Isolation. The process includes cooling crystallization, surfactant wetting, centrifugal separation and surfactant recovery. The fractionation and separation efficiency of the surfactant method is high, the product quality is good, the application is wide, and it is suitable for large-scale production.

发明内容 Contents of the invention

为了解决微生物油在温度较低时(10-20℃)易凝固的问题,本发明的目的是提供一种微生物油的分提方法,该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固,该方法工序简单、成本低。In order to solve the problem that microbial oil is easy to solidify when the temperature is low (10-20 ° C), the object of the invention is to provide a method for fractionating microbial oil, the liquid oil of the microbial oil proposed by the method is separated when the temperature is low (10-20° C.) is not easy to solidify, and the method has simple procedures and low cost.

为了实现上述目的,本发明的技术方案是:一种微生物油的分提方法,其特征在于它包括如下步骤:In order to achieve the above object, the technical scheme of the present invention is: a kind of fractionation method of microbial oil, it is characterized in that it comprises the steps:

1)均化:将待分提的微生物油(或称微生物油脂)搅拌均匀;1) Homogenization: Stir the microbial oil (or microbial oil) to be fractionated evenly;

2)破晶:将搅拌均匀的微生物油升温至25-30℃后,保温5-10min;2) Crystal breaking: After heating the uniformly stirred microbial oil to 25-30°C, keep it warm for 5-10 minutes;

微生物油脂在冷冻前将自然形成的不均匀晶核破坏,微生物油脂在精制、运输、储存过程中,由于微生物油脂温低于固态脂凝固点而析出晶体;这部分晶体由于是在非匀速降温过程中析出的,晶型各异,晶粒大小不一,当转到冷冻结晶阶段后,会不利于脂晶的均匀成长和成熟,使结晶体本身产生缺陷,影响油脂分提,破晶通常将油脂熔融升温至固态脂熔点以上,保持5-10min;Microbial oils destroy the naturally formed uneven crystal nuclei before freezing. During the refining, transportation, and storage of microbial oils, crystals are precipitated because the temperature of microbial oils is lower than the freezing point of solid fats; this part of crystals is due to non-uniform cooling. The precipitated ones have different crystal forms and different grain sizes. When it is transferred to the freezing and crystallization stage, it will not be conducive to the uniform growth and maturation of lipid crystals, causing defects in the crystal itself, affecting oil fractionation, and breaking crystals usually melts oil Raise the temperature above the melting point of the solid fat and keep it for 5-10 minutes;

3)冷冻结晶(逐渐冷却的过程):将步骤2)保温后的微生物油于4℃结晶4-7h(低温条件下充分),再置于10℃低温条件下1-4h,得到含有固体结晶的粘稠料浆(此时油脂物料经过降温冷冻后形成了含有固体结晶的粘稠料浆);3) Freeze crystallization (gradual cooling process): crystallize the microbial oil after step 2) at 4°C for 4-7h (full under low temperature conditions), and then place it under low temperature conditions of 10°C for 1-4h to obtain solid crystals The viscous slurry (at this time, the grease material forms a viscous slurry containing solid crystals after being cooled and frozen);

4)表面活性剂溶液的加入:按含有固体结晶的粘稠料浆∶表面活性剂水溶液的体积比=1∶0.5-1∶2,选取含有固体结晶的粘稠料浆和表面活性剂水溶液;其中,表面活性剂水溶液由表面活性剂、无机盐和水组成,表面活性剂的浓度为0.08-0.4wt%,无机盐的浓度为0.5-3wt%;4) Addition of surfactant solution: according to the volume ratio of thick slurry containing solid crystals: aqueous surfactant solution = 1: 0.5-1: 2, select the thick slurry containing solid crystals and aqueous surfactant solution; Wherein, the surfactant aqueous solution is composed of surfactant, inorganic salt and water, the concentration of surfactant is 0.08-0.4wt%, and the concentration of inorganic salt is 0.5-3wt%;

向含有固体结晶的粘稠料浆中加入表面活性剂水溶液,搅拌0.5-1.0h,得到乳化液体系;Add an aqueous surfactant solution to the viscous slurry containing solid crystals, and stir for 0.5-1.0 hours to obtain an emulsion system;

充分搅拌使混合体系分散均匀形成乳化液体系,油脂中的液体组分因仍保持液相,不能被表面活性剂润湿而在搅拌作用下成为微细液滴分散于水溶液中,而被表面活性剂分子包裹的结晶颗粒因得到充分润湿,排除了附于结晶面的液体组分,于是转入到水相中;Stir fully to disperse the mixed system evenly to form an emulsion system. The liquid components in the oil still remain in the liquid phase and cannot be wetted by the surfactant, so they become fine droplets and disperse in the aqueous solution under the action of stirring, and are dispersed by the surfactant. The molecularly wrapped crystalline particles are fully wetted, eliminating the liquid components attached to the crystalline surface, and then transfer to the water phase;

5)离心分离得液体油:将步骤4)的乳化液体系于5-10℃低温条件静置0.5-5h,在冷冻离心机中离心,液体组分便以轻相分出,加入水清洗后经脱水干燥(20-25℃干燥2-6h),即得微生物油的液态油(产品);5) Centrifuge to obtain liquid oil: put the emulsion system in step 4) at a low temperature of 5-10°C for 0.5-5h, centrifuge in a refrigerated centrifuge, the liquid component will be separated as a light phase, add water to wash After dehydration and drying (drying at 20-25°C for 2-6h), the liquid oil (product) of microbial oil can be obtained;

而悬浮着固体结晶的表面活性剂水溶液则以重相分出,得到固相油脂混合液。The aqueous surfactant solution with solid crystals suspended is separated as a heavy phase to obtain a solid phase oil mixture.

表面活性剂为十二烷基硫酸钠(SDS)、烷基苯磺酸钠或脂肪醇硫酸钠等。The surfactant is sodium dodecyl sulfate (SDS), sodium alkylbenzene sulfonate or sodium fatty alcohol sulfate, etc.

无机盐为硫酸镁(MgSO4)、硫酸钠、硫酸铝或氯化钠等。Inorganic salts are magnesium sulfate (MgSO 4 ), sodium sulfate, aluminum sulfate, or sodium chloride.

步骤5)所述的离心分离的条件是:3000-6000rpm,离心5-10min。The centrifugation conditions in step 5) are: 3000-6000rpm, centrifugation for 5-10min.

6)破乳后得固体脂:取出微生物油的液态油(即液体组分)后,所得的固相油脂混合液经过80-95℃加热破乳处理2-10min,结晶熔化,固体组分即与水相分开,除去下层的水相即得到固体脂组分,加入水进行水洗除去残余的表面活性剂水溶液,经脱水干燥后,即得微生物油的固体硬脂。6) Obtain solid fat after demulsification: After taking out the liquid oil (i.e. the liquid component) of the microbial oil, the obtained solid-phase oil mixture is heated at 80-95°C for 2-10 minutes to demulsify, the crystallization is melted, and the solid component is Separate from the water phase, remove the lower water phase to obtain the solid fat component, add water to wash to remove the residual surfactant aqueous solution, and after dehydration and drying, obtain the solid stearin of microbial oil.

本发明分提后微生物菌油的液态油(是本发明所需要得到的产品),10℃条件下透明时间可长达120h以上(其物理化学指标见表1)。该发明解决了微生物油在温度较低时(<20℃)易凝固的问题,从而提高了微生物油脂的使用价值和经济价值。The liquid oil (which is the product that the present invention needs to obtain) after fractionation of the microbial bacterial oil of the present invention, the transparent time can reach more than 120h under the condition of 10 ℃ (its physicochemical index sees Table 1). The invention solves the problem that the microbial oil is easy to solidify when the temperature is low (<20° C.), thereby improving the use value and economic value of the microbial oil.

表1物理化学指标的比较(实施例1-5)The comparison (embodiment 1-5) of table 1 physicochemical index

Figure BDA0000106498090000031
Figure BDA0000106498090000031

本发明的有益效果是:The beneficial effects of the present invention are:

1)该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。本发明分提后微生物菌油的液态油(是本发明所需要得到的产品),10℃条件下透明时间可长达120h以上。1) The liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C). The liquid oil (which is the product required by the present invention) after fractionation of the microbial bacterial oil in the present invention has a transparent time of more than 120 hours at 10°C.

经分提后得到的微生物油的液态油熔点低,抗冻性强,在南方冬季仍然保持液态,可以作为调和油组分也可以改变微生物油冬季使用不便的状况,丰富油脂市场。The liquid oil of the microbial oil obtained after fractionation has a low melting point and strong frost resistance, and remains liquid in the southern winter. It can be used as a blending oil component or change the inconvenient use of microbial oil in winter, enriching the oil market.

2)该方法工序简单,不需要复杂设备。2) The process of the method is simple and does not require complex equipment.

本发明与干法分提相比具有生产周期短,分离效率高,生产过程易于控制的优点;与溶剂分提法相比不需使用有机溶剂,因而安全,设备投资少,成本较低。Compared with the dry fractionation method, the invention has the advantages of short production period, high separation efficiency and easy control of the production process; compared with the solvent fractionation method, no organic solvent is needed, so it is safe, has less equipment investment and lower cost.

3)微生物油的液态油(产品)质量更好,液油的得率比较高,没有任何有机溶剂的污染;3) The liquid oil (product) quality of microbial oil is better, the yield of liquid oil is relatively high, and there is no pollution of any organic solvent;

4)工艺中所用到的表面活性剂可以回收后重复使用;4) The surfactant used in the process can be recycled and reused;

5)由于不需要复杂设备及不需用有机溶剂,节省了大量设备投资、运行费用,从而降低了生产成本,适用于工业化生产。5) Since no complex equipment and no organic solvent are needed, a large amount of equipment investment and operating costs are saved, thereby reducing production costs and being suitable for industrial production.

附图说明 Description of drawings

图1为本发明的工艺流程图。Fig. 1 is a process flow diagram of the present invention.

具体实施方式 Detailed ways

为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the examples, but the content of the present invention is not limited to the following examples.

实施例1:Example 1:

如图1所示,一种微生物油的分提方法,它包括如下步骤:As shown in Figure 1, a kind of fractionation method of microbial oil, it comprises the steps:

1)均化:将待分提的微生物油搅拌均匀;1) Homogenization: Stir the microbial oil to be fractionated evenly;

2)破晶:将搅拌均匀的微生物油熔融升温至固态脂熔点以上(25℃),保持5min;2) Crystal breaking: Melt the evenly stirred microbial oil and heat it up to above the melting point of solid fat (25°C) and keep it for 5 minutes;

3)冷冻结晶:将步骤2)保温后的微生物油于4℃低温条件下充分结晶5h,再置于10℃低温恒温水浴锅中2h,得到含有固体结晶的粘稠料浆(此时油脂物料经过降温冷冻后形成了含有固体结晶的粘稠料浆);3) Frozen crystallization: The microbial oil after step 2) is fully crystallized at a low temperature of 4°C for 5 hours, and then placed in a low-temperature constant temperature water bath at 10°C for 2 hours to obtain a viscous slurry containing solid crystals (at this time, the oil material After cooling and freezing, a viscous slurry containing solid crystals is formed);

4)表面活性剂溶液的加入:按含有固体结晶的粘稠料浆∶表面活性剂水溶液的体积比=1∶1,选取含有固体结晶的粘稠料浆和表面活性剂水溶液;其中,表面活性剂水溶液由表面活性剂、无机盐和水组成,表面活性剂的浓度为0.4wt%,无机盐的浓度为1wt%;4) Adding of surfactant solution: press the viscous slurry containing solid crystals: the volume ratio of surfactant aqueous solution=1:1, select the viscous slurry containing solid crystals and aqueous surfactant solution; wherein, surface active The aqueous agent solution is made up of surfactant, inorganic salt and water, and the concentration of surfactant is 0.4wt%, and the concentration of inorganic salt is 1wt%;

表面活性剂为十二烷基硫酸钠(SDS);无机盐为硫酸镁(MgSO4);The surfactant is sodium dodecyl sulfate (SDS); the inorganic salt is magnesium sulfate (MgSO 4 );

向含有固体结晶的粘稠料浆中加入表面活性剂水溶液,搅拌0.5h,得到乳化液体系;Add an aqueous surfactant solution to the viscous slurry containing solid crystals, and stir for 0.5 hours to obtain an emulsion system;

5)离心分离得液体油:将步骤4)的乳化液体系于10℃低温条件静置0.5h,在冷冻离心机中离心,液体组分便以轻相分出(图1中简称为液油),加入水清洗后经脱水干燥(20℃干燥6h),即得微生物油的液态油(产品,得率为59.9%);5) Liquid oil obtained by centrifugation: put the emulsion system in step 4) at a low temperature of 10°C for 0.5h, centrifuge in a refrigerated centrifuge, and the liquid component will be separated with a light phase (abbreviated as liquid oil in Figure 1 ), adding water to wash and then dehydrating and drying (drying at 20° C. for 6 hours) to obtain liquid oil of microbial oil (product, yield 59.9%);

而悬浮着固体结晶的表面活性剂水溶液则以重相分出(为固相油脂混合液);The aqueous surfactant solution with solid crystals suspended is separated out with the heavy phase (it is a solid-phase oil mixture);

6)破乳后得固体脂:取出微生物油的液态油(即液体组分)后,所得的固相油脂混合液经过90℃加热破乳处理2-10min,结晶熔化,固体组分即与水相分开,除去下层的水相即得到固体脂组分,加入水进行水洗除去残余的表面活性剂水溶液,经脱水干燥后,即得微生物油的固体硬脂(图1中简称为固体脂)。剩余溶液即表面活性剂溶液,经回收后再利用。6) Obtain solid fat after demulsification: After taking out the liquid oil (i.e. the liquid component) of the microbial oil, the obtained solid-phase oil mixture is heated at 90°C for 2-10 minutes to demulsify, crystallize and melt, and the solid component is mixed with water Separate the phases, remove the lower water phase to obtain the solid fat component, add water to wash to remove the residual surfactant aqueous solution, and after dehydration and drying, obtain the solid stearin of microbial oil (abbreviated as solid fat in Figure 1). The remaining solution is the surfactant solution, which is recovered and reused.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上(其物理化学指标见表1)。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C (see Table 1 for its physical and chemical indicators). It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

实施例2:Example 2:

一种微生物油的分提方法,它包括如下步骤:A fractionation method of microbial oil, it comprises the steps:

1)均化:将待分提的微生物油搅拌均匀;1) Homogenization: Stir the microbial oil to be fractionated evenly;

2)破晶:将搅拌均匀的微生物油熔融升温至固态脂熔点以上(30℃),保持5min;2) Crystal breaking: Melt the uniformly stirred microbial oil and heat it up to above the melting point of solid fat (30°C) and keep it for 5 minutes;

3)冷冻结晶:将微生物油于4℃低温条件下充分结晶5h,再置于10℃低温恒温水浴锅中2h,得到含有固体结晶的粘稠料浆(此时油脂物料经过降温冷冻后形成了含有固体结晶的粘稠料浆);3) Freeze crystallization: The microbial oil is fully crystallized at 4°C for 5 hours, and then placed in a low-temperature constant temperature water bath at 10°C for 2 hours to obtain a viscous slurry containing solid crystals (at this time, the oil material has been cooled and frozen to form a viscous slurry containing solid crystals);

4)表面活性剂溶液的加入:按含有固体结晶的粘稠料浆∶表面活性剂水溶液的体积比=1∶1,选取含有固体结晶的粘稠料浆和表面活性剂水溶液;其中,表面活性剂水溶液由表面活性剂、无机盐和水组成,表面活性剂的浓度为0.4wt%,无机盐的浓度为2wt%;4) Adding of surfactant solution: press the viscous slurry containing solid crystals: the volume ratio of surfactant aqueous solution=1:1, select the viscous slurry containing solid crystals and aqueous surfactant solution; wherein, surface active The aqueous agent solution is made up of surfactant, inorganic salt and water, and the concentration of surfactant is 0.4wt%, and the concentration of inorganic salt is 2wt%;

表面活性剂为十二烷基硫酸钠(SDS);无机盐为硫酸镁(MgSO4);The surfactant is sodium dodecyl sulfate (SDS); the inorganic salt is magnesium sulfate (MgSO 4 );

向含有固体结晶的粘稠料浆中加入表面活性剂水溶液,搅拌1.0h,得到乳化液体系;Add an aqueous surfactant solution to the viscous slurry containing solid crystals, and stir for 1.0 h to obtain an emulsion system;

5)离心分离得液体油:将步骤4)的乳化液体系于10℃低温条件静置1h,在冷冻离心机中离心,液体组分便以轻相分出,加入水清洗后经脱水干燥(25℃干燥6h),即得微生物油的液态油(产品,得率为57.1%);5) Centrifuge to obtain liquid oil: put the emulsion system in step 4) at 10°C for 1 hour, centrifuge in a refrigerated centrifuge, and the liquid component will be separated into a light phase, add water to wash, and then dehydrate and dry ( Dry at 25°C for 6h), to obtain the liquid oil of microbial oil (product, the yield is 57.1%);

而悬浮着固体结晶的表面活性剂水溶液则以重相分出(为固相油脂混合液);The aqueous surfactant solution with solid crystals suspended is separated out with the heavy phase (it is a solid-phase oil mixture);

6)破乳后得固体脂:取出微生物油的液态油(即液体组分)后,所得的固相油脂混合液经过90℃加热破乳处理2-10min,结晶熔化,固体组分即与水相分开,除去下层的水相即得到固体脂组分,加入水进行水洗除去残余的表面活性剂水溶液,经脱水干燥后,即得微生物油的固体硬脂。6) Obtain solid fat after demulsification: After taking out the liquid oil (i.e. the liquid component) of the microbial oil, the obtained solid-phase oil mixture is heated at 90°C for 2-10 minutes to demulsify, crystallize and melt, and the solid component is mixed with water The phases are separated, and the lower water phase is removed to obtain the solid fat component. Water is added to wash to remove the residual surfactant aqueous solution. After dehydration and drying, the solid stearin of microbial oil is obtained.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上(其物理化学指标见表1)。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C (see Table 1 for its physical and chemical indicators). It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

实施例3:Example 3:

一种微生物油的分提方法,它包括如下步骤:A fractionation method of microbial oil, it comprises the steps:

1)均化:将待分提的微生物油搅拌均匀;1) Homogenization: Stir the microbial oil to be fractionated evenly;

2)破晶:将搅拌均匀的微生物油熔融升温至固态脂熔点以上(28℃),保持5min;2) Crystal breaking: Melt the uniformly stirred microbial oil and heat it up to above the melting point of solid fat (28°C) and keep it for 5 minutes;

3)冷冻结晶:将微生物油于4℃低温条件下充分结晶5h,再置于10℃低温恒温水浴锅中2h,此时油脂物料经过降温冷冻后形成了含有固体结晶的粘稠料浆;3) Frozen crystallization: The microbial oil is fully crystallized at 4°C for 5 hours, and then placed in a low-temperature constant temperature water bath at 10°C for 2 hours. At this time, the oily material is cooled and frozen to form a viscous slurry containing solid crystals;

4)表面活性剂溶液的加入:按含有固体结晶的粘稠料浆∶表面活性剂水溶液的体积比=1∶1.5,选取含有固体结晶的粘稠料浆和表面活性剂水溶液;其中,表面活性剂水溶液由表面活性剂、无机盐和水组成,表面活性剂的浓度为0.4wt%,无机盐的浓度为1wt%;4) Adding of surfactant solution: press the viscous slurry containing solid crystals: the volume ratio of surfactant aqueous solution=1: 1.5, select the viscous slurry containing solid crystals and aqueous surfactant solution; wherein, surface active The aqueous agent solution is made up of surfactant, inorganic salt and water, and the concentration of surfactant is 0.4wt%, and the concentration of inorganic salt is 1wt%;

表面活性剂为十二烷基硫酸钠(SDS);无机盐为硫酸镁(MgSO4);The surfactant is sodium dodecyl sulfate (SDS); the inorganic salt is magnesium sulfate (MgSO 4 );

向含有固体结晶的粘稠料浆中加入表面活性剂水溶液,搅拌0.8h,得到乳化液体系;Add an aqueous surfactant solution to the viscous slurry containing solid crystals, and stir for 0.8 hours to obtain an emulsion system;

5)离心分离得液体油:将步骤4)的乳化液体系于10℃低温条件静置2h,在冷冻离心机中离心,液体组分便以轻相分出,加入水清洗后经脱水干燥(22℃干燥4h),即得微生物油的液态油(产品,56.8%);5) Centrifuge to obtain liquid oil: put the emulsion system in step 4) at 10°C for 2 hours, centrifuge in a refrigerated centrifuge, and the liquid component will be separated as a light phase, add water to wash, and then dehydrate and dry ( Dry at 22°C for 4h), to obtain the liquid oil of microbial oil (product, 56.8%);

而悬浮着固体结晶的表面活性剂水溶液则以重相分出(为固相油脂混合液);The aqueous surfactant solution with solid crystals suspended is separated out with the heavy phase (it is a solid-phase oil mixture);

6)破乳后得固体脂:取出微生物油的液态油(即液体组分)后,所得的固相油脂混合液经过80℃加热破乳处理2-10min,结晶熔化,固体组分即与水相分开,除去下层的水相即得到固体脂组分,加入水进行水洗除去残余的表面活性剂水溶液,经脱水干燥后,即得微生物油的固体硬脂。6) Obtain solid fat after demulsification: After taking out the liquid oil (i.e. the liquid component) of the microbial oil, the obtained solid-phase oil mixture is heated at 80°C for 2-10 minutes to demulsify, the crystallization melts, and the solid component is mixed with water The phases are separated, and the lower water phase is removed to obtain the solid fat component. Water is added to wash to remove the residual surfactant aqueous solution. After dehydration and drying, the solid stearin of microbial oil is obtained.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上(其物理化学指标见表1)。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C (see Table 1 for its physical and chemical indicators). It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

实施例4:Example 4:

一种微生物油的分提方法,它包括如下步骤:A fractionation method of microbial oil, it comprises the steps:

1)均化:将待分提的微生物油搅拌均匀;1) Homogenization: Stir the microbial oil to be fractionated evenly;

2)破晶:将搅拌均匀的微生物油熔融升温至固态脂熔点以上(26℃),保持5min;2) Crystal breaking: Melt the uniformly stirred microbial oil and heat it up to above the melting point of solid fat (26°C) and keep it for 5 minutes;

3)冷冻结晶:将微生物油于4℃低温条件下充分结晶4h,再置于10℃低温恒温水浴锅中1h,此时油脂物料经过降温冷冻后形成了含有固体结晶的粘稠料浆;3) Freeze crystallization: The microbial oil is fully crystallized at 4°C for 4 hours, and then placed in a low-temperature constant temperature water bath at 10°C for 1 hour. At this time, the oily material is cooled and frozen to form a viscous slurry containing solid crystals;

4)表面活性剂溶液的加入:按含有固体结晶的粘稠料浆∶表面活性剂水溶液的体积比=1∶0.5,选取含有固体结晶的粘稠料浆和表面活性剂水溶液;其中,表面活性剂水溶液由表面活性剂、无机盐和水组成,表面活性剂的浓度为0.08wt%,无机盐的浓度为0.5wt%;4) Adding of surfactant solution: press the viscous slurry containing solid crystals: the volume ratio of surfactant aqueous solution=1:0.5, select the viscous slurry containing solid crystals and aqueous surfactant solution; wherein, surface active The aqueous agent solution is made up of surfactant, inorganic salt and water, and the concentration of surfactant is 0.08wt%, and the concentration of inorganic salt is 0.5wt%;

表面活性剂为十二烷基硫酸钠(SDS);无机盐为硫酸镁(MgSO4);The surfactant is sodium dodecyl sulfate (SDS); the inorganic salt is magnesium sulfate (MgSO 4 );

向含有固体结晶的粘稠料浆中加入表面活性剂水溶液,搅拌0.6h,得到乳化液体系;Add an aqueous surfactant solution to the viscous slurry containing solid crystals, and stir for 0.6 hours to obtain an emulsion system;

5)离心分离得液体油:将步骤4)的乳化液体系于5℃低温条件静置1h,在冷冻离心机中离心,液体组分便以轻相分出,加入水清洗后经脱水干燥(20℃干燥2h),即得微生物油的液态油(产品,得率为58.8%);5) Centrifugal separation to obtain liquid oil: put the emulsion system in step 4) at 5°C for 1 hour, centrifuge in a refrigerated centrifuge, the liquid component will be separated as a light phase, add water to wash, and then dehydrate and dry ( 20 ℃ drying 2h), namely the liquid oil of microbial oil (product, the yield is 58.8%);

而悬浮着固体结晶的表面活性剂水溶液则以重相分出(为固相油脂混合液);The aqueous surfactant solution with solid crystals suspended is separated out with the heavy phase (it is a solid-phase oil mixture);

6)破乳后得固体脂:取出微生物油的液态油(即液体组分)后,所得的固相油脂混合液经过85℃加热破乳处理2-10min,结晶熔化,固体组分即与水相分开,除去下层的水相即得到固体脂组分,加入水进行水洗除去残余的表面活性剂水溶液,经脱水干燥后,即得微生物油的固体硬脂。6) Obtain solid fat after demulsification: After taking out the liquid oil (i.e. the liquid component) of the microbial oil, the obtained solid-phase oil mixture is heated at 85°C for 2-10 minutes to demulsify, the crystallization is melted, and the solid component is mixed with water The phases are separated, and the lower water phase is removed to obtain the solid fat component. Water is added to wash to remove the residual surfactant aqueous solution. After dehydration and drying, the solid stearin of microbial oil is obtained.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上(其物理化学指标见表1)。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C (see Table 1 for its physical and chemical indicators). It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

实施例5:Example 5:

一种微生物油的分提方法,它包括如下步骤:A fractionation method of microbial oil, it comprises the steps:

1)均化:将待分提的微生物油搅拌均匀;1) Homogenization: Stir the microbial oil to be fractionated evenly;

2)破晶:将搅拌均匀的微生物油熔融升温至固态脂熔点以上(30℃),保持10min;2) Crystal breaking: Melt the evenly stirred microbial oil and heat it up to above the melting point of solid fat (30°C) and keep it for 10 minutes;

3)冷冻结晶:将微生物油于4℃低温条件下充分结晶7h,再置于10℃低温恒温水浴锅中4h,得到含有固体结晶的粘稠料浆(此时油脂物料经过降温冷冻后形成了含有固体结晶的粘稠料浆);3) Freeze crystallization: fully crystallize the microbial oil at 4°C for 7 hours, and then place it in a low-temperature constant temperature water bath at 10°C for 4 hours to obtain a viscous slurry containing solid crystals (at this time, the oil material is cooled and frozen to form a viscous slurry containing solid crystals);

4)表面活性剂溶液的加入:向这种料浆中按照油水比1∶1的比例加入含有0.3%SDS和1%MgSO4的表面活性剂水溶液,充分搅拌使混合体系分散均匀形成乳化液体系;4) Addition of surfactant solution: add an aqueous surfactant solution containing 0.3% SDS and 1 % MgSO to the slurry according to the oil-water ratio of 1:1, stir well to make the mixed system disperse evenly to form an emulsion system ;

5)离心分离得液体油:将此乳化液体系于10℃条件静置0.5h,在冷冻离心机中以5000rpm,离心5min,液体组分便以轻相分出,加入去离子水清洗后经脱水干燥即得微生物油的液态油(得率为57.2%),而悬浮着固体结晶的表面活性剂水溶液则以重相分出;5) Centrifuge to obtain liquid oil: put the emulsion system at 10°C for 0.5h, centrifuge at 5000rpm in a refrigerated centrifuge for 5min, the liquid component will be separated as light phase, add deionized water to wash, and then The liquid oil (yield rate: 57.2%) of microbial oil is obtained by dehydration and drying, and the surfactant aqueous solution with solid crystals suspended is separated with heavy phase;

4)表面活性剂溶液的加入:按含有固体结晶的粘稠料浆∶表面活性剂水溶液的体积比=1∶2,选取含有固体结晶的粘稠料浆和表面活性剂水溶液;其中,表面活性剂水溶液由表面活性剂、无机盐和水组成,表面活性剂的浓度为0.2wt%,无机盐的浓度为3wt%;4) Adding of surfactant solution: press the viscous slurry containing solid crystals: the volume ratio of surfactant aqueous solution=1:2, select the viscous slurry containing solid crystals and aqueous surfactant solution; wherein, surface active The aqueous agent solution is made up of surfactant, inorganic salt and water, and the concentration of surfactant is 0.2wt%, and the concentration of inorganic salt is 3wt%;

表面活性剂为十二烷基硫酸钠(SDS);无机盐为硫酸镁(MgSO4);The surfactant is sodium dodecyl sulfate (SDS); the inorganic salt is magnesium sulfate (MgSO 4 );

向含有固体结晶的粘稠料浆中加入表面活性剂水溶液,搅拌1.0h,得到乳化液体系;Add an aqueous surfactant solution to the viscous slurry containing solid crystals, and stir for 1.0 h to obtain an emulsion system;

5)离心分离得液体油:将步骤4)的乳化液体系于8℃低温条件静置5h,在冷冻离心机中离心,液体组分便以轻相分出,加入水清洗后经脱水干燥(25℃干燥2h),即得微生物油的液态油(产品,得率为57.2%);5) Liquid oil obtained by centrifugation: put the emulsion system in step 4) at a low temperature of 8°C for 5 hours, centrifuge in a refrigerated centrifuge, and the liquid component will be separated as a light phase, add water to wash, and then dehydrate and dry ( 25 ℃ drying 2h), obtain the liquid oil of microbial oil (product, the yield rate is 57.2%);

而悬浮着固体结晶的表面活性剂水溶液则以重相分出(为固相油脂混合液);The aqueous surfactant solution with solid crystals suspended is separated out with the heavy phase (it is a solid-phase oil mixture);

6)破乳后得固体脂:取出微生物油的液态油(即液体组分)后,所得的固相油脂混合液经过95℃加热破乳处理2-10min,结晶熔化,固体组分即与水相分开,除去下层的水相即得到固体脂组分,加入水进行水洗除去残余的表面活性剂水溶液,经脱水干燥后,即得微生物油的固体硬脂。6) Obtain solid fat after demulsification: After taking out the liquid oil (i.e. the liquid component) of the microbial oil, the obtained solid-phase oil mixture is heated at 95°C for 2-10 minutes to demulsify, the crystallization is melted, and the solid component is mixed with water The phases are separated, and the lower water phase is removed to obtain the solid fat component. Water is added to wash to remove the residual surfactant aqueous solution. After dehydration and drying, the solid stearin of microbial oil is obtained.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上(其物理化学指标见表1)。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C (see Table 1 for its physical and chemical indicators). It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

实施例6Example 6

与实施例1基本相同,不同之处在于:表面活性剂为烷基苯磺酸钠。无机盐为硫酸钠。It is basically the same as Example 1, except that the surfactant is sodium alkylbenzene sulfonate. The inorganic salt is sodium sulfate.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C. It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

实施例7Example 7

与实施例1基本相同,不同之处在于:表面活性剂为脂肪醇硫酸钠。无机盐为硫酸铝。Substantially the same as Example 1, the difference is that the surfactant is fatty alcohol sodium sulfate. The inorganic salt is aluminum sulfate.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C. It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

实施例7Example 7

与实施例1基本相同,不同之处在于:表面活性剂为烷基苯磺酸钠。无机盐为氯化钠。It is basically the same as Example 1, except that the surfactant is sodium alkylbenzene sulfonate. The inorganic salt is sodium chloride.

本实施例分提后微生物菌油的液态油,10℃条件下透明时间可长达120h以上。说明该方法分提出的微生物油的液态油在温度较低时(10-20℃)不易凝固。The liquid oil of microbial bacterial oil after separation in this embodiment can be transparent for more than 120 hours at 10°C. It shows that the liquid oil of the microbial oil proposed by this method is not easy to solidify when the temperature is low (10-20°C).

本发明各工艺参数(如温度、时间等)的上下限取值、以及其区间值,都能实现本发明,在此不一一列举实施例。The upper and lower limits of each process parameter (such as temperature, time, etc.) of the present invention, as well as the interval values thereof, can realize the present invention, and the embodiments are not listed here one by one.

Claims (2)

1.一种微生物油的分提方法,其特征在于它包括如下步骤:1. a fractionation method of microbial oil is characterized in that it comprises the steps: 1)均化:将待分提的微生物油搅拌均匀;1) Homogenization: Stir the microbial oil to be fractionated evenly; 2)破晶:将搅拌均匀的微生物油升温至25-30 ℃后,保温5-10 min;2) Crystal breaking: After heating the uniformly stirred microbial oil to 25-30 °C, keep it warm for 5-10 min; 3)冷冻结晶:将步骤2)保温后的微生物油于4 ℃结晶4-7 h,再置于10 ℃低温条件下1-4 h,得到含有固体结晶的粘稠料浆;3) Freezing and crystallization: crystallize the microbial oil after step 2) at 4°C for 4-7 hours, and then place it at a low temperature of 10°C for 1-4 hours to obtain a viscous slurry containing solid crystals; 4)表面活性剂溶液的加入:按含有固体结晶的粘稠料浆﹕表面活性剂水溶液的体积比=1:0.5-1:2,选取含有固体结晶的粘稠料浆和表面活性剂水溶液;其中,表面活性剂水溶液由表面活性剂、无机盐和水组成,表面活性剂的浓度为0.08-0.4 wt%,无机盐的浓度为0.5-3 wt%;4) Addition of surfactant solution: According to the volume ratio of viscous slurry containing solid crystals: surfactant aqueous solution = 1:0.5-1:2, select viscous slurry containing solid crystals and aqueous surfactant solution; Wherein, the surfactant aqueous solution is made up of surfactant, inorganic salt and water, and the concentration of surfactant is 0.08-0.4 wt%, and the concentration of inorganic salt is 0.5-3 wt%; 表面活性剂为十二烷基硫酸钠、烷基苯磺酸钠或脂肪醇硫酸钠;The surfactant is sodium lauryl sulfate, sodium alkylbenzenesulfonate or sodium fatty alcohol sulfate; 无机盐为硫酸镁、硫酸钠、硫酸铝或氯化钠;The inorganic salt is magnesium sulfate, sodium sulfate, aluminum sulfate or sodium chloride; 向含有固体结晶的粘稠料浆中加入表面活性剂水溶液,搅拌0.5-1.0h,得到乳化液体系;Add an aqueous surfactant solution to the viscous slurry containing solid crystals, and stir for 0.5-1.0 hours to obtain an emulsion system; 5)离心分离得液体油:将步骤4)的乳化液体系于5-10 ℃低温条件静置1-5h,在冷冻离心机中离心,液体组分便以轻相分出,加入水清洗后经脱水干燥,即得微生物油的液态油;5) Centrifuge to obtain liquid oil: put the emulsion system in step 4) at a low temperature of 5-10 ℃ for 1-5h, centrifuge in a refrigerated centrifuge, the liquid component will be separated into a light phase, add water to wash After dehydration and drying, the liquid oil of microbial oil can be obtained; 而悬浮着固体结晶的表面活性剂水溶液则以重相分出,得到固相油脂混合液。The aqueous surfactant solution with solid crystals suspended is separated as a heavy phase to obtain a solid phase oil mixture. 2.根据权利要求1所述的一种微生物油的分提方法,其特征在于:所得的固相油脂混合液经过80-95 ℃加热破乳处理2-10 min,结晶熔化,固体组分即与水相分开,取上清,得到的固体组分并加入水进行水洗除去残余的表面活性剂水溶液,经脱水干燥后,即得微生物油的固体硬脂。2. The fractionation method of a kind of microbial oil according to claim 1, characterized in that: the obtained solid-phase oil mixture is heated at 80-95°C for 2-10 min, crystallized and melted, and the solid component is Separate from the water phase, take the supernatant, and add water to the obtained solid component to wash to remove the residual surfactant aqueous solution. After dehydration and drying, the solid stearin of microbial oil is obtained.
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