KR20030066196A - Method of Producing Egg Yolk Lecithin - Google Patents

Abstract

PURPOSE: A method for producing egg yolk lecithin is provided, thereby easily and cheaply producing high purity egg yolk lecithin by regulating the concentration of ethanol. CONSTITUTION: A method for producing egg yolk lecithin comprises the steps of: (A) adding an ethanol-containing solvent into egg yolk powder and heating the mixture at 30 to 70 deg. C for 10 minutes to 2 hours; (B) filtering the extracted solution, removing powder from the filtered solution, and regulating the ethanol concentration of the filtered solution to 92 to 97%(v/v); (C) cooling the filtered solution to 20 to 55 deg. C and storing it for 10 minutes or more to separate the filtered solution into an upper layer containing phospholipid and a lower layer containing neutral lipid; and (D) concentrating the upper layer under vacuum condition to remove ethanol and water from the upper layer.

Description

Method of Producing Egg Yolk Lecithin {Method of Producing Egg Yolk Lecithin}

The present invention relates to a method for preparing egg yolk lecithin, and more particularly, by adding ethanol-containing solvent such as alcohol to egg yolk powder to extract lipids, and filtering and filtering the filtrate to remove sedimented neutral lipid fraction. It provides a method for easily preparing a high-purity lecithin from egg yolk powder by the process.

Lecithin is a component of the phospholipids that make up lipids, and is scientifically termed phosphatidyl choline, and is found in large amounts in foods such as soybeans and yolks. Phospholipids are a component of the cell membranes of living bodies and are known to play an important role in ex vivo functions such as cell activation and memory enhancement. In addition, lecithin has a strong emulsifying function and is widely used as an emulsifier industrially. It is also applied as a function to prevent arterial wall deposition of cholesterol by emulsifying blood cholesterol in vivo.

In some cases, it is classified according to the content of phospholipids. In general, more than 60% of the phospholipid content is called lecithin, and the case of less than 60% of the phospholipid content is called egg yolk oil. Ingredients other than phospholipids contained in lecithin are mainly neutral lipids, and in addition, trace amounts of polysaccharides and cholesterol are included. The lecithin requirement in the food sector is when the phospholipid content is more than 60% and the water content is within 1.5%. However, when the content of phospholipid is too high, for example, at 80%, the viscosity is greatly increased, which makes it difficult to remove moisture due to processing problems with food additives and the like. Therefore, according to the method of the present invention, it contains 60% or more of the phospholipids, but also contains an appropriate amount of neutral lipids, so that a totally balanced lecithin can be composed.

Lecithin is generally manufactured by extracting and refining soybean and egg yolk as raw materials. In recent years, since the bioactivation function of egg yolk lecithin obtained by using yolk as a raw material has been reported, the demand for egg yolk lecithin is increasing. However, it is not easy to obtain lecithin in high purity because egg yolk contains many kinds of lipids.

In order to solve this problem, various methods have been developed.

U.S. Patent No. 4,157,404 (Process for obtaining yolk lecithin from raw egg yolk) extracts egg yolk with dimethyl ether, removes egg yolk protein and dimethyl ether from the extraction mixture, and then dehyrates the egg yolk lecithin. It is presented how to extract.

US Patent No. 4,844,926 (Egg lecithin process), the first heating step of heating the egg yolk separated from the egg slightly at about 150 degrees Fahrenheit for 5 minutes, the second heating step of heating at about 200 degrees Fahrenheit for about 30 minutes, Egg yolk lecithin through a third heating step of heating at about 190 degrees Fahrenheit for 30 minutes, a fourth heating step of heating at about 200 degrees Fahrenheit for 20 minutes with mild stirring, filtering it by a filter means, and cooling it to about room temperature It is presented a method of preparing.

U.S. Patent No. 4,847,015 (Process for producing egg yolk lecithin having reduced PE content and / or containing substantially no impurities), dissolves egg yolk lecithin in a strong polar solvent or a mixture of a strong polar solvent and a non-polar solvent and ion-exchanges the resulting solution. A method of preparing egg yolk lecithin with a small amount of phosphatidylethanolamine is provided by removing a solvent from a solution by contacting a resin.

U. S. Patent No. 5,028, 449 also discloses a manufacturing method by a substantially similar method to U. S. Patent No. 4,884, 826 differing only in heating temperature and time.

On the other hand, Korean Patent Application Publication No. 1987-6843 (Method for manufacturing egg yolk oil), a sterile water-washed dried egg is aseptically removed by degassing and collecting only egg yolk, homogenized, and nitrogen atmosphere through a sealed conduit so that there is no contact with outside air. Transfer to packed hot spray dryer and dry to below 5% of water content. The dried yolk powder is extracted after impregnated with n-nucleic acid through continuous connection conduit to extract enough egg yolk oil, and then known centrifugation or filtration and vacuum distillation apparatus. Suggests a method of extracting pure yolk oil.

Korean Patent Application Publication No. 1989-4713 (Method of Extracting Egg Yolk), after immersing an egg in a seran bath containing 200 ppm of free chlorine for a certain time, rupturing the egg shell to separate egg yolk and egg white, After extracting and sterilizing at about 65 ℃ for 3 to 5 minutes, the sterilized yolk solution is dried in a drier to remove moisture, and then the yolk powder is put into a bladder of about 100 mesh filter cloth, which is about twice the amount of egg yolk, A method of extracting egg yolk oil is disclosed in which a solvent of normal hexane or ethylene dichloride is selected and added to egg yolk powder to extract egg oil contained in egg yolk.

As described above, the conventional method for preparing egg yolk lecithin (or extraction method) employs a variety of means such as extraction using a specific solvent, stepwise heat treatment or contact with an ion exchange resin, but the extraction yield is very low, or a production plant It is difficult to always maintain the same quality of the product when applied to, the purity of the obtained lecithin is low, the cost of the solvent or material used in the manufacturing method is high. Therefore, there is a strong need for a method capable of producing high purity egg yolk lecithin in high yield despite a simple manufacturing method.

Accordingly, an object of the present invention is to solve the problems of the prior art and the technical problems that have been requested from the past.

After conducting numerous experiments and studies, the present inventors have been able to obtain high-purity lecithin while recovering phospholipids in high yield. Upon cooling, the inventors found that the upper layer supernatant containing 60% or more of phospholipids and the lower layer consisting mostly of neutral lipids resulted in the separation of the present invention.

It is known that phospholipids are soluble in alcohol and partially soluble in water, but it is well known that neutral lipids are also soluble in alcohols when egg yolks are dissolved. It is a new fact that the lecithin contained above can be separated by layer separation by cooling, and there is no prior art teaching or suggesting this. Therefore, the problem and the past of the prior art can be solved by the use of inexpensive solvents and simple processes, such as dissolution / extraction by ethanol, control of ethanol purity of the extract filtrate, layer separation by cooling the filtrate, and removal of the neutral lipid lower layer. It can solve the important technical challenges of high purity and high recovery rate that have been requested from

The present invention for achieving this object is a method for producing egg yolk lecithin having a phospholipid purity of 60% or more with a recovery rate of 90% or more,

(A) adding ethanol-containing solvent to egg yolk powder and warming to 30 to 70 ℃ for 10 minutes to 2 hours to extract;

(B) filtering the extract to remove the powder and adjusting the ethanol purity of the obtained filtrate to 92 to 97% (v / v);

(C) cooling the resulting filtrate to 20-55 ° C. and then standing for at least 10 minutes to separate the upper layer supernatant containing phospholipids and the lower layer of neutral lipids; And,

(D) removing sedimentary neutral lipids in the lower layer and vacuum condensing the supernatant in the upper layer to remove ethanol and water.

According to the method of the present invention, yolk lecithin having a purity of 60% (w / w) or more can be easily produced with a recovery rate of 90% or more by using an inexpensive solvent and a simple manufacturing process. It has a significant advantage in that it can be obtained.

Egg yolk is an egg yolk, about 50% (w / w) of which is water, about 60% (w / w) of solids, and 30% (w / w) of lipids It is known that the amount to be phospholipid. Egg yolk powder to be used as a raw material in the present invention is to dry the liquid yolk is used that has a moisture content of 1 to 3% (w / w). If the moisture content is too high, there is a problem that the purity of ethanol is much lowered to make it difficult to remove neutral lipids. On the contrary, if the amount is too small, it is difficult to prepare egg yolk powder in a high quality state. Methods of preparing egg yolk powder are well known in the art and will not be described separately.

As described above, since phospholipid is soluble in alcohol, ethanol is used in the present invention to extract phospholipid from powdered egg yolk. Preferred examples of the ethanol-containing solvent include alcohol having a purity of 90% (v / v) or higher which is edible ethanol. In general, it is easy to obtain spirits whose purity is 95-96% (v / v).

Therefore, as a specific example of the step (A), a purity of 95 to 96% (v / v) is added to 3 to 10 times (volume ratio) with respect to egg yolk powder, it is 10 minutes at 30 to 70 ℃ while stirring slowly Warm for 2 hours to extract lipids from egg yolk. A further preferred amount of ethanol solution is 4 to 8 times (volume ratio) relative to egg yolk powder. Although the time and temperature of the extraction process are not particularly limited, the extraction efficiency is generally lower when the extraction process is performed at 30 ° C. or lower or 10 minutes or less, and oxidation of lipids is performed when the extraction process is performed at 70 ° C. or higher or for 2 hours or longer. Can cause.

In step (B), the solids are first removed from the extracted extract, which is preferably filtered into a network of 50 to 200 meshes first, and secondly to a filter of 0.5 to 10 microns, thereby filtering the solids. Remove it completely. As a result of the experiment, the purity of lecithin in this state was found to be 25 to 45% (w / w).

Layer separation of the filtrate obtained through the removal of solids (step (C)) requires maintaining the ethanol purity of the filtrate at a certain level and then cooling and standing the filtrate. First, the ethanol purity of the filtrate is at least 92 to 97% (v). / v). If the purity of ethanol is too low, not only the sedimentation of the lower layer of neutral lipids is too much, but also the sedimentation of phospholipids increases, resulting in a lower yield. On the contrary, if the purity of ethanol is too high, neutral lipid does not settle and there is a problem in that lecithin containing 60% or more of phospholipid cannot be obtained. Especially preferred filtrate ethanol purity is 93-96%.

The ethanol purity of the filtrate may be automatically adjusted within the set range by the ethanol purity used in step (A), in which case there is no need to adjust the purity separately. In general, the ethanol purity of the ethanol solution used in step (A) is slightly diluted through the extraction process, because the water contained in the yolk powder is incorporated into the filtrate. In some cases, it may be carried out separately in step (B). For example, when the ethanol purity of the filtrate is low, an additional high purity ethanol solution may be added to the filtrate. Conversely, when the ethanol purity of the filtrate is low, the purity can be adjusted by adding low purity ethanol or distilled water to the filtrate.

Another process for layer separation, cooling and standing, as described above for step (C), allowed to cool to 20-55 ° C. and left to stand for at least 10 minutes, with excess neutral lipids extracted excessively forming droplets. While settling to the bottom of the filtrate. If the cooling temperature is too low, the settling loss of lecithin increases, and if it is too high, the amount of neutral lipid sedimented is not preferable. A more preferable range of the cooling temperature is 30 to 40 ° C. In some cases, it is also possible to increase the sedimentation rate of the neutral lipid by stirring slowly at 1 to 30 rpm (rotation / minute), more preferably at 2 to 15 rpm. If the stirring speed is too low, the effect of stirring is less, if too high it will hinder the sedimentation of the neutral lipid.

The time for allowing the filtrate to stand still is sufficient for 10 minutes or more after the temperature of the filtrate drops to the set temperature, and in some cases, it may be left for 24 hours or more. After cooling, the settled neutral lipids are generally red in color and settle down at the bottom of the container so that they can be easily removed. The lower layer contains more than 95% pure lipids and trace amounts of phospholipids. As a result, the purity of the lecithin of the supernatant was found to be 50 to 75% with neutral lipid removed.

In step (D), the supernatant is concentrated in vacuo to remove ethanol and water to obtain a lecithin in the form of a paste. Preferred examples of the vacuum concentration is carried out at 0.005 to 0.1 atm so that the temperature of the contents does not exceed 40 ℃. If the temperature at the time of vacuum concentration is 40 degreeC or more, oxidation of phospholipid may be caused and odor may generate | occur | produce. The resulting yolk lecithin in paste form has a very high viscosity of 1.5% or less of moisture and becomes hard as a solid when cooled to 10 ° C or lower. If the ethanol purity of the filtrate in step (B) is too low, in addition to the problems described above, the concentration time is increased for the removal of water having a high heat of vaporization, resulting in a problem of deterioration of the product quality.

Detailed description of the manufacturing method of the present invention with reference to the following examples, but the scope of the present invention is not limited thereto.

Example 1

5 l of spirit (containing 96.2% (v / v) ethanol) was added to 1 kg of egg yolk powder having a water content of 1.5% (w / w) and extracted with stirring at 60 ° C for 30 minutes. This was filtered to obtain 4.2 L of filtrate, wherein the ethanol purity of the filtrate was 95.8% (v / v). The obtained filtrate was cooled to 25 ° C., and then allowed to stand for 1 hour to separate layers. The upper phospholipid concentration was 60.6% (w / w), the lower phospholipid concentration was 2.1% (w / w), and the lower neutral phospholipid was 9 g. The supernatant of the upper layer was concentrated in vacuo at 20 DEG C at 0.004 atm. As a result, 278.5 g of lecithin having a high phospholipid purity of 60% (w / w) having a reddish yellow color was obtained. The recovery of phospholipids was 92.8%.

Example 2

To 100 kg of the same egg yolk powder as in Example 1, 300 L of alcohol (containing 95.1% (v / v) of ethanol) was added and extracted with stirring at 60 ° C for 30 minutes. The extract was filtered to obtain 203 L of filtrate, and 300 L of alcohol was further added to the remaining egg yolk to extract for 1 hour at 60 ° C., followed by filtration to obtain 307 L of filtrate. The 203 L filtrate obtained first and the 307 L filtrate obtained further were mixed, and the ethanol purity of the mixed filtrate obtained at this time was 94.2% (v / v). This mixture was allowed to stand at 45 ° C. for 1 hour to remove the neutral lipids that settled to the bottom. The obtained supernatant was concentrated under vacuum at 0.08 atmosphere at 35 ° C., and 27.5 kg of lecithin was obtained. The phospholipid purity of the obtained lecithin was 62.1% (w / w), and the recovery rate of phospholipid was 94.8%. Therefore, it could be confirmed that high-purity lecithin was obtained under the same conditions in the mass-experiment experiment under the same conditions as the small-volume experiment under the experimental conditions of Example 1.

Example 3

To 150 kg of the same egg yolk powder as in Example 1, 600 L of alcohol (containing 94.1% (v / v) of ethanol) was added, and the mixture was extracted with stirring at 55 ° C. for 60 minutes. The obtained extract was filtered to obtain 440 L of filtrate, and 450 L of alcohol (containing 95.0% (v / v) of ethanol) was added thereto, followed by extraction at 55 DEG C for 60 minutes, and then 440 L of the filtrate was mixed. Ethanol purity of the mixed filtrate was 93.5% (v / v). The mixed filtrate was allowed to stand at 38 ° C. for 60 minutes to separate the layers, and the neutral lipids that settled on the separated layers were removed, and the supernatant was concentrated under vacuum at 0.03 atmosphere at 30 ° C. to obtain 40.8 kg of lecithin. . The phospholipid purity of the obtained lecithin was 65.2%. The amount of lecithin obtained is a high yield corresponding to 94% of the phospholipid theory present in egg yolk.

Example 4

700 ml of 99.9% (v / v) anhydrous ethanol was added to 100 g of the same yolk powder as in Example 1, which was extracted at 60 ° C. and filtered, to obtain 604 ml of the filtrate. 33 ml of distilled water was added to the obtained filtrate, and the ethanol purity was adjusted to 94.5% (v / v). After adjusting the ethanol purity of the filtrate was allowed to stand for 1 hour at 38 ℃ to separate the layers, the lower neutral lipid layer was removed. The supernatant was concentrated in vacuo at 0.05C to 30 atmospheres, yielding 26.8 g of lecithin with a water content of 1.2% (w / w). The phospholipid purity of the obtained lecithin was 62.3% (w / w). The recovery of phospholipids was 92.8%.

Example 5

To 500 g of the same yolk powder as in Example 1, 7 times of ethanol having a purity of 92.5% (v / v) was added thereto, which was extracted at 60 ° C. and filtered. The purity of the extract obtained after filtration was 92% (v / v) and that of phospholipid was 32% (v / v). 2.93 L of the obtained extract was cooled to 39 ° C. to remove 24 g of neutral lipid that settled at the bottom. The neutral lipid layer contained 1.1% (w / w) phospholipids. The supernatant was concentrated in vacuo to give 140.8 g of lecithin of 60.3% (w / w) phospholipid. The recovery of phospholipid was 94% and the final lecithin was 1.48% (w / w).

Comparative Example 1

1.5 g of ethanol having a purity of 90% (v / v) was added to 250 g of powdered egg yolk and extracted at 60 ° C. for 20 minutes, followed by filtration to obtain 1.18 L of the filtrate (the filtration time after extraction was higher than that of the high-purity ethanol of Example 1). It took about twice as much). The ethanol purity of this filtrate was 89.1% (v / v). Purity of the phospholipid in the filtrate obtained was 45% (w / w), the amount of the neutral lipid layer to sink to the bottom when cooled to 45 ℃ was insignificant. After further cooling to 10 ° C, 11.2 g of neutral lipid layer could be separated, and the neutral lipid layer contained 2.1 g of phospholipid (18.8% of phospholipid contained in the neutral lipid layer, high purity ethanol). Very high compared to 1% of Example 1). The neutral lipid layer was removed and the supernatant was concentrated in vacuo to give 44.2 g of lecithin with a water content of 3.7% (w / w) and a phospholipid 75% (w / w), where the high moisture content requires phospholipid purity. This is because the viscosity is too high, the viscosity is too high, and it is difficult to remove water any more by vacuum concentration. If you extend the time a lot, you can lower the moisture, but in that case, excessive heat may cause deterioration such as odor of lecithin. In the present embodiment, the recovery rate of phospholipid is low as 75%, and it can be seen that the production cost is significantly increased considering excessive cooling and quality deterioration.

Comparative Example 2

700 ml of alcohol (containing 95.1% (v / v) ethanol) was added to 100 g of the same egg yolk powder as in Example 1, which was extracted at 60 ° C. and filtered. After cooling the obtained filtrate at 15 degreeC, it left still for 1 hour, the neutral lipid which settled in the lower layer was removed, and the supernatant supernatant was vacuum-concentrated at 0.04 atmosphere at 25 degreeC, and 16.1 g of lecithin was obtained. The phospholipid purity of the obtained lecithin was 71.3% (w / w), and the recovery of phospholipid was 62%.

In Comparative Example 2, by cooling more than necessary, the neutral lipid and some of the phospholipids are settled and removed at the same time, so that the purity of the supernatant is increased and the recovery is significantly lower than that of 94% of Example 4.

Comparative Example 3

To 500 g of the same egg yolk powder as in Example 1, 2 L of alcohol (containing 95.1% (v / v) of ethanol) was added and extracted with stirring at 55 ° C. for 25 minutes. Filtration gave 1.45 L of the filtrate, and the ethanol purity of the filtrate was 94.5% (v / v). The filtrate obtained was cooled to 40 ° C., left to stand for 30 minutes, and then separated and neutral lipids settled to the bottom. As a result of vacuum concentration of the obtained supernatant liquid at 25 degreeC at 0.5 atmosphere, 161.8 g of lecithin of 55% (w / w) which is high red-yellow viscosity was obtained. The moisture content was 8% (w / w). Since the atmospheric pressure for vacuum concentration was 0.5 atm, which is relatively high pressure, the residual amount of water and the like increased after concentration, thereby obtaining lecithin having a purity of 60% or less of phospholipid. In order to evaporate ethanol at the atmospheric pressure, the ethanol should be at least about 50 ° C., and if it is concentrated at this temperature for a long time, odor occurs and there is a problem in that the water content after concentration is very high as 5 to 10%.

Those skilled in the art to which the present invention pertains, various applications and modifications are possible within the scope of the claims based on the above description.

According to the egg yolk lecithin manufacturing method of the present invention, high-purity lecithin can be produced from egg yolk with high recovery rate by using a low cost solvent and mild conditions and simple processes, and thus the production cost is low and the quality control of the product during mass production (mass production) It is easy to work and simple and easy to get high purity lecithin.

Claims (2)

In the method for producing lecithin from egg yolk, (A) adding ethanol-containing solvent to egg yolk powder and warming to 30 to 70 ℃ for 10 minutes to 2 hours to extract; (B) filtering the extract to remove the powder and adjusting the ethanol purity of the obtained filtrate to 92 to 97% (v / v); (C) cooling the resulting filtrate to 20-55 ° C. and then standing for at least 10 minutes to separate the upper layer supernatant containing phospholipids and the lower layer of neutral lipids; And, (D) a method for producing egg yolk lecithin, which has a phospholipid purity of 60% or more and a recovery rate of 90% or more, comprising the step of removing sedimentary neutral lipids of the lower layer and vacuum-concentrating the upper supernatant. The method of claim 1, wherein the ethanol purity of the filtrate in step (B) is 93 to 96%, phospholipid purity of 60% or more and recovery of egg yolk lecithin of 90% or more.