JPH09172962A - Production of cow's milk fat spherical membrane-containing fraction - Google Patents

Abstract

PROBLEM TO BE SOLVED: To readily obtain cow's milk fat spherical membrane-containing fraction from butter milk without adding any agent, etc., at all in a producing process. SOLUTION: The cow's milk fat spherical membrane-containing fraction contained in butter milk is separated by treating butter milk with a micro- filtering membrane having 0.5-6.0μm pore diameter.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a method for producing a milk fat globule membrane-containing fraction, and more particularly to a method for producing a high-purity milk fat globule membrane-containing fraction using buttermilk as a raw material.

[0002]

2. Description of the Related Art Milk Fat Globule Membr
ane) is often abbreviated as MFGM, but recently the same thing is referred to as Milk Lipid Globule Membrane.
Also called, MLGM is sometimes abbreviated. Here, the name milk fat globule membrane is used, and is abbreviated as MFGM hereinafter. Further, in the present specification, the MFGM-containing fraction may be simply referred to as MFGM. Most of the fat contained in milk is dispersed in milk in the form of fat globules. The reason why these fat globules can form a stable emulsion is that MFGM, which acts as a partition between highly hydrophobic lipids and external water, exists. This MFGM can be expected to have a strong emulsifying property even in view of such a role in milk. In fact, Sugano reported that MFGM has a high emulsifying property (Kanno, CJ Food. S
ci. 54 (6), 1534-1539, (1989)). Therefore, MFGM has high utility value as an emulsifier for food, medicine, or cosmetics.

In the field of dairy products, microfiltration membranes are used for separating cream from milk, removing microorganisms in milk, recovering proteins such as casein in milk, and desalting. However, the use of microfiltration membranes in the production of MFGM has never been attempted. In the laboratory, the MFGM fraction was transferred to the buttermilk side by culturing a cream that had been thoroughly washed with water, so that the isoelectric point (3.9 to 4.0) was reached.
After adjusting H, MFGM is prepared through complicated steps such as a method of precipitating by centrifugation, a method of collecting by ultracentrifugation, a method of extracting with an organic solvent such as alcohol, a method of salting out with ammonium sulfate. There is. Here, washing the cream with water means adding water to the cream and mixing it,
It is an operation to reduce the content of casein and lactose in the cream by repeating the process of separating the cream again with a cream separator. In addition, a method of concentrating buttermilk obtained as a by-product of ordinary butter production by ultrafiltration and the like and then isoelectrically precipitating the same has been reported, but in this case, an additive such as an acid is required, and casein Further purification steps are required to remove the like. Therefore, in these methods, a by-product is generated in the manufacturing process of MFGM and the manufacturing process is complicated.

[0004]

When producing MFGM from buttermilk, the known method was to produce butter from cream washed with water and use the buttermilk produced at that time. Therefore, a large amount of hydrated skim milk is generated,
It is not suitable for commercial production because it not only affects the flavor of butter but also complicates the process. In particular, when MFGM is used in the fields of foods and pharmaceuticals, it is not desirable from a safety standpoint to add other than milk components such as drugs in the manufacturing process. Therefore, it is an object of the present invention to develop a method for obtaining a fraction containing MFGM in high purity from buttermilk produced in the step of producing butter in the simplest possible process and without adding any drug in the production process. Is.

The inventors of the present invention have conducted extensive studies to solve the above problems, and as a result, by using a microfiltration technique, a normal cream that has not been washed with water is cultivated. The inventors have found a method for producing a high-purity fraction containing MFGM from buttermilk and completed the present invention.

[0006]

According to the first aspect of the present invention,
A milk fat globule membrane-containing fraction characterized by treating buttermilk with a microfiltration membrane having a pore size of 0.5 to 6.0 μm to separate the milk fat globule membrane-containing fraction contained in the buttermilk. It is a manufacturing method. The invention according to claim 2 treats buttermilk with a microfiltration membrane having a pore size of 0.5 to 6.0 µm, and dialysis treatment is carried out by adding water to a retentate that has not passed through the membrane to carry out dialysis treatment. A method for producing a high-purity milk fat globule membrane-containing fraction, which comprises concentrating the membrane-containing fraction.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION As described above, MFGM is produced by using buttermilk as a raw material. Buttermilk is the aqueous phase portion that remains when the butter grains are formed during the production of butter by churning. The composition is almost the same as skim milk. According to the present invention, when buttermilk is treated with a microfiltration membrane having a large pore size of 0.5 μm to 6.0 μm, proteins such as casein in milk and components such as lactose can be removed, and MFGM can be efficiently prepared.
It is possible to obtain For example, if the recovery rate of MFGM component from raw buttermilk by microfiltration is 5%, 95% of MFGM component is contained in the permeate,
The components of the permeate are virtually the same as those of the buttermilk used as the raw material, and can be used as they are for the production of buttermilk powder or concentrated buttermilk.
Raw material costs in MFGM manufacturing can be very low.

The membrane fraction of fat globules crushed by the production of butter is considered to be dispersed as MFGM in buttermilk, but the size of the particles is considered to be distributed over a wide range. Therefore, in the method of the present invention in which MFGM is produced using a microfiltration membrane having a large pore size, most of MFGM cannot be recovered and leaks to the permeate side. However, as described above, this product can be used as buttermilk, so that the loss thereof need not be practically taken into consideration. The present invention was established based on this idea.

The method for producing the MFGM of the present invention will be described in detail below. First, as a raw material, butter milk produced during the production of normal butter is prepared. In addition, butter milk powder obtained by pulverizing butter milk or a concentrated butter milk product reduced to an appropriate concentration with water or the like can be used as a raw material in the same manner. Furthermore, when producing butter oil (anhydrous butter) directly from cream, butter milk is produced as a by-product, and this can be used as a raw material. In addition, the pH of buttermilk produced during the production of fermented butter is usually around pH 4.5 to 5.4 depending on the degree of fermentation, but if the isoelectric point of casein (pH 4.6) or higher, then leave it as is. It can be used as a raw material of the present invention. If the pH is 4.
When it is less than 6, since the proteins such as casein in buttermilk aggregate at the isoelectric point, the pH of the raw buttermilk is reduced.
Needs to be adjusted to neutral (pH around 7.0).
With these exceptions, the pH of normal buttermilk is 6.
It exhibits a neutrality of about 5 and can be used as it is as a raw material of the present invention. The method of the present invention is a manufacturing process of MFGM,
One of the characteristics of manufacturing is that no chemicals such as compounds are added, and the buttermilk that is the raw material used for manufacturing MFGM has buttermilk without pH adjustment as much as possible if the pH is 4.6 or higher. It is desirable to practice the invention at the pH of the milk itself.

There are no restrictions on the material of the microfiltration membrane, and various materials can be used. Examples of the material include glass fibers, stainless steel, various metal fibers such as alloys, various ceramics and ceramics, and various natural substances. There are synthetic polymer substances and the like. There are also various shapes (supervised by Masayuki Nakagaki, Fuji Techno System, a membrane processing technology system, 1
991). In the present invention, a ceramic microfiltration membrane is suitable, as shown in Examples described later.
When selecting the material of the filtration membrane, the range of pore size distribution and the treatment capacity should be taken into consideration.

It should be kept in mind when determining the pore size of the microfiltration membrane that casein contained in a large amount in buttermilk associates with each other to form huge particles called casein micelles. Casein (average about 0.2
It is said that it has a size of about μm),
MFGM is to select a microfiltration membrane that cannot pass at least part of it. Therefore, although a microfiltration membrane having a pore size of 0.5 μm or more and 6.0 μm or less is used in the present invention, a microfiltration membrane having a pore size of 0.5 μm or more and 2.0 μm or less is preferable.

By the way, when the buttermilk is processed using a microfiltration membrane and the MFGM fraction is obtained, the flow rate is improved by adjusting the temperature of the buttermilk as a raw material to 5 to 70 ° C, preferably 35 to 60 ° C. Or, if the temperature is adjusted to 5 to 20 ° C., the recovery rate of MFGM increases, and microfiltration can be efficiently performed.

When the raw material buttermilk was treated with a microfiltration membrane by the method of the present invention, MFGM was contained in the retained retentate without being passed through the filtration membrane, and an MFGM-containing fraction was obtained. can do. When microfiltration is performed while adding dialysis to this fraction with water, most of the proteins contained in the retentate, including low-molecular-weight lactose and micellar casein, migrate to the permeate side. . Therefore,
By this operation, only MFGM is relatively concentrated on the retentate side, and casein, lactose, etc. can be efficiently removed. Further, the degree of purification can be increased by increasing the amount of water to be added. In this way, high-purity MFGM can be obtained.

The fraction containing a large amount of concentrated MFGM can be used as it is as an emulsifier, etc., but if desired, the MFGM-containing fraction can be subjected to treatments such as concentration, spray drying or freeze drying. High-purity MFGM preparation can be obtained. It should be noted that whether or not the MFGM component is concentrated can be confirmed by SDS-polyacrylamide gel electrophoresis (SDS-PAGE) as described in Example 2 below.
It may be confirmed that the membrane proteins, such as xanthine oxidase and butyrophilin, which are peculiar to MFGM, are concentrated.

As a result of investigations by the present inventors, some of them have a relatively large size even after crushing fat globules, and even a microfiltration membrane having the above-mentioned pore size, for example, a very large pore size of 2 μm, retains some MFGM. It became clear that it could be retained on the liquid side. In particular, the size distribution of the micelle-like casein particles overlaps with the size distribution of the MFGM particles, but as is clear from Test Example 1 described later, even the large micelle-like casein particles have a size of 1.2 μm or less. In contrast to MFGM, MFGM has a large size distribution with a large size of 1.2 μm to 60 μm.
Therefore, for example, in the case of a membrane with a pore size of 1.4 μm, a part with a larger particle size in the MFGM component dispersed in buttermilk is recovered, and micellar casein is effectively removed by dialysis. Because you can
It is possible to economically produce a fraction containing a large amount of MFGM components.

[0016]

The present invention will be described in more detail with reference to the following examples, but the present invention is not limited thereto. Test Example 1 Particle size distribution of MFGM component in buttermilk In order to grasp the size of the MFGM component separated and collected by the method of the present invention as particles, fresh cream (47% fat fresh cream) and skim milk are used. The particle size distribution of colloidal particles in buttermilk used as a raw material was investigated. Each sample was dispersed in water, and the particle size distribution of each liquid was examined by a laser diffraction / scattering type particle size distribution measuring device (LA-700 type manufactured by Horiba Ltd.). The obtained results are summarized in FIG. This figure shows the particle size distributions of the respective solutions superimposed on each other based on the measured values. It can be seen that the particle size distribution of the fresh cream has a median diameter of about 3 μm. This indicates that the fat globule size is distributed around 3 μm. Casein is contained in the fresh cream in the same degree as skimmed milk, but since the figure shows a relative particle size distribution, the peak due to micellar casein is apparently
Not seen in the graph.

On the other hand, in the particle size distribution of skim milk, fat globules are scarcely present, so that the resulting peak is due to micellar casein, and its median diameter is 0.17 μm. Regarding the particle size distribution of buttermilk, the largest peak still shows the particle size distribution of micellar casein. The component showing a particle size distribution with a peak around 1.8 μm on the right side is considered to be a distribution mainly caused by the MFGM component. Most of the fat globules are thought to be crushed by the butter production, so the components showing a particle size distribution of 0.8 μm or more, which is not found in the particle size distribution of skim milk, are mainly MF.
It is considered to be a GM component. Therefore, if a microfiltration membrane with a pore size that can collect a part of such a fraction is used, the target MF
It is expected that GM components can be recovered.

The actual pore size distribution of a membrane varies depending on the manufacturer with respect to the nominal pore size of the membrane. Generally, the nominal pore size of a membrane is often indicated by the maximum pore size distributed in the membrane.
For example, when looking at a commercially available ceramic microfiltration membrane, the nominal pore diameter (the pore diameter of the membrane present on the surface of the ceramic filtration membrane is particularly referred to as the pore diameter, and shows the actual fractionation performance,
Here, all are referred to as the pore size. In the microfiltration membrane having a diameter of 0.1 μm), pore diameters of 0.05 μm to 0.1 μm are actually distributed. Therefore, if a microfiltration membrane with a nominal pore size of 0.1 μm is used, the micellar casein will be easily concentrated, and the MFGM component will be recovered to effectively remove the micellar casein, which is the main contaminant. 0.5 μm to remove
It can be seen that it is necessary to use a membrane having the above pore size. For example, if a membrane with a nominal pore size of 1.0 to 2.0 μm is used, a considerable part of MFGM will permeate, but since micellar casein can be effectively removed to the filtrate side, only the MFGM component should be recovered. Is possible. MF for even larger pore size membranes
Although the recovery rate of the GM component is low, the micelle-like casein can be removed more effectively, so that it can be used for MFGM production.

Test Example 2 Production of MFGM from Washed Buttermilk As a comparison for producing the MFGM fraction according to the method of the present invention, the MFGM fraction was produced using a washed cream. Four
7% fat cream (18 kg) was heated to 40 ° C., 3 times amount of water (40 ° C.) was added, and a cream fraction was obtained with a cream separator. This operation was repeated 3 times to obtain a water-washed cream fraction with a cream separator. The fraction that migrates to the aqueous phase was removed. This aqueous phase fraction mainly contains casein and lactose. The cream fraction obtained here (12.7
Since the fat content of 1 kg) was 55.8%, water was added to adjust the fat content to 40%, the mixture was cooled to 10 ° C., and then the mixture was churned with butter churn. After the churning, the buttermilk was collected. Also, after heating the butter (9.29 kg) produced at this time to 40 ° C., half the amount of water (40 ° C., 4.65 kg) was added, and the aqueous phase was again collected with a cream separator, and the butter milk and Combined (24.47 kg).

Next, this fraction was concentrated by a reverse osmosis membrane (RO membrane) treatment (2.76 kg) and lyophilized to obtain 2
9.52 g of freeze-dried product was obtained. In this method, the cream is thoroughly washed with water, prepared from buttermilk produced by churning, and the whole is freeze-dried without treatment such as isoelectric precipitation, ultracentrifugation, salting-out and the like. Therefore, since MFGM contains all the essential components, this was used as a water-washed MFGM preparation as a material for comparison with the MFGM preparation prepared with a microfiltration membrane.

Example 1 Production of MFGM from Buttermilk by Microfiltration Device Production of MFGM by microfiltration using buttermilk as a raw material was carried out as follows. The microfiltration device used is Alfa Laval's Micro filtration pilot plantType MFS-1
Type, membrane module is Type SCT-MEMBRALOX, special A
LFA-LAVALexecution (1P19-40-0.2M2-316L-1.4MICRON)
And the nominal pore size is about 1.4 μm (value in the catalog)
Met.

First, 30 kg of buttermilk was heated to 50 ° C. and subjected to the above microfiltration device at a flow rate of about 480 liters / m ² h (permeate flow rate per 1 m ^{2 of} membrane area per hour). As a result, about 5.0 liters of retentate was obtained. This is called Retentate 1. To the retentate 1, 27 liters of water heated to 50 ° C. was added and treated again in the same manner with the MFS-1 type apparatus. The retentate obtained by this treatment is called retentate 2.
To the retentate 2, 27 liters of water heated at 50 ° C. was added again, and the solution was similarly applied to the MFS-1 type microfiltration device. The retentate obtained here is referred to as retentate 3. To the retentate 3, 27 liters of water heated to about 50 ° C. was added and similarly treated with the MFS-1 type. The retentate obtained as a result is designated as retentate 4. The final retentate 4 was about 5 kg. The components of these retentates were analyzed by a near infrared analyzer (Milco Scan 104, manufactured by Foss Electric Co., Ltd.).
The results shown in the table were obtained. As is clear from this table, it was revealed that the lactose content of the retentate was significantly reduced after about 3 times of water addition.

[0023]

[Table 1]

When the particle size distribution of the retentate 4 was measured in the same manner as in Test Example 1, the results shown in FIG. 2 were obtained, and the concentrated components were distributed from 0.5 μm to 6 μm. It became clear. Lyophilize this retentate 4,
23 g of freeze-dried product was obtained. This was used as a microfiltration MFGM preparation. Typical component analysis values of the microfiltration MFGM preparation produced by this method are 98.5% total solids and 3 protein.
The content was 8.7%, fat content 57.03%, ash content 1.68%, and lactose 0.25%.

Example 2 Analysis of MFGM Preparation Product The water-washed MFGM preparation product prepared in Test Example 2 and the microfiltration MFGM preparation product obtained in Example 1 were compared by SDS-polyacrylamide gel electrophoresis (SDS-PAGE) ( 3 and 4). The gel concentration was 10%, and the method of Lemmley (UK Laemmli, Nat
ure (London), 227, 680-685 (1975)). In Figure 3
SDS-PAGE gel stained with Coomassie Brilliant Blue is shown. Lane 1 shows the migration pattern of buttermilk as a raw material, and in lane 1, all the bands of major proteins contained in buttermilk are seen. CB1 is xanthine oxidas
It is a component known as e). This name is because at least a part of the protein is known to have xanthine oxidase activity, and it is also known to have various other enzyme activities. Also, CB5 is a protein called butyrophilin, which is very hydrophobic and has a high affinity for fat. CB6,
The bands designated as CB7 mainly have molecular weights of 44,000 and 480.
It is composed of 100 glycopolypeptides and is known as glycoprotein B.

Various methods are known for preparing MFGM, but xanthine oxidase, butyrophilin and glycoprotein B having a molecular weight of 44000 and 48000 are always found (TW Keenan and S. Patton, in
"Handbook of Milk Composition", ed. By RG Jens
en, Academic Press, San Diego, Calif., 1995, pp.5-
50), which is the main protein component of MFGM. Therefore, the relative density of these bands is a good indicator of the extent of recovery of MFGM components. The dark bands around 30,000 compared with the molecular weight markers are mainly α-casein, β-casein and κ-casein bands. Furthermore, the two bands below that having a molecular weight of 14400 to 20100 are considered to be mainly lipoproteins derived from MFGM.

Lane 2 shows the migration pattern of the permeated liquid that had passed through the 1.4 μm microfiltration membrane in Example 1 but before water addition. As is clear from the figure, the pattern shows almost the same as that of the buttermilk used as the raw material, and it can be seen that casein and the like permeate as it is. However, it is clear that the bands corresponding to CB1 and CB5, which are the main components of MFGM, are relatively thin compared to the permeate in lane 1. Lane 3
Is the migration pattern of retentate 2. Since the retentate 2 is hydrolyzed and dialyzed, the casein band becomes thin,
The bands corresponding to CB1, CB5, CB6, and CB7, which are the constituents of MFGM, are relatively dark, and it is clear that MFGM is concentrated. Further, the lane 4 shows the migration pattern of the retentate 4, showing that the band of casein was hardly seen due to further dialysis as compared with the retentate 2, and that the band of CB5 was particularly dark. Lane 5 is the separation pattern of the washed MFGM preparation of Test Example 2 used for comparison.

Thus, as can be seen from Lane 2, the permeated liquid that has permeated the microfiltration membrane is considered to have a composition very similar to that of the raw buttermilk, and is slightly MF.
Only the GM component was recovered. Therefore, by returning the permeate to the raw material, the raw material buttermilk can be used for the production of products such as buttermilk powder and concentrated buttermilk with almost no loss of its components. Also,
As can be seen by comparing Lane 4 and Lane 5, the microfiltration membrane MFGM preparation produced with the microfiltration membrane is considered to have a composition very similar to that of MFGM prepared from water-washed cream. Important as CB1, CB5, CB6, C
All ingredients such as B7 are included. Also, it can be seen that casein is scarcely contained. In addition, lane 6
Is a molecular weight marker

FIG. 4 shows the same SDS-PAGE stained by a method called PAS staining, particularly for glycoproteins having sugar chains. As a result, in the microfiltration MFGM preparation,
It can be seen that CB1, CB5, CB6, CB7 are efficiently concentrated. In particular, CB5 butyrophilin is well stained with sugar. From this, it became clear that the microfiltration MFGM preparation contains the MFGM component similarly to the water-washed MFGM preparation. Considering the results of the particle size distribution together, the particle size distribution of the MFGM component is widely distributed over 0.5 μm to 6.0 μm, so even if the microfiltration membrane has a wide nominal pore size of 6 μm, the actual pore size Most are 6.0 μm
Since it is distributed below, it is considered that MFGM can be recovered depending on the type of membrane.

Example 3 Effect of Pore Size of Microfiltration Membrane As described above, MF was obtained with a microfiltration membrane having a pore size of 1.4 μm.
It was shown that it is possible to produce GM, but here, it was confirmed that when the buttermilk was filtered using a ceramic microfiltration membrane with nominal pore diameters of 0.5 μm, 1.0 μm and 2.0 μm. The particle size distribution of the concentrated solution was investigated and the results are shown. The microfiltration equipment used is as follows. Device name: NGK Ceramic film filter device manufactured by Filtec Co., Ltd. Membrane module: CEFILT-MF Dimensions: φ30mm × φ4mm-19mm hole × 1000mm (monolith type) Nominal pore size: 0.5μm, 1.0μm, 2.0μm Operating condition Filtration Method: Constant pressure cross-flow filtration (method of constant total circulation concentration) Circulation flow rate: 3 m / s Filtration pressure: 1 kg / cm ² Filtration temperature: 50 ° C. The buttermilk as a raw material is filtered under the conditions above, and the filtration rate becomes equilibrium. The filtration and retentate samples were obtained. No dialysis with water was used in this experiment.

The particle size distribution of buttermilk used as the raw material is shown in FIG. Fig. 5 shows 0.5μ of buttermilk as a raw material.
The particle size distributions of the permeated liquids that have permeated the microfiltration membranes of m, 1.0 μm, and 2.0 μm are shown. From these results, 0.5
It is clear that all the micellar casein leaks to the permeate side in the microfiltration membrane having a size of from μm to 2.0 μm. In addition, the particle size distribution of the solution remaining on the concentrated liquid side that could not pass through the 2.0 μm membrane is shown in FIG. Compared with the particle size distribution of skim milk, it is clear that these microfiltration membranes have relatively accumulated particle sizes from 0.5 μm to about 60 μm. When this solution was observed with an optical microscope,
It was clear that the crushed fat globule fragments were aggregated.

As described above, in this experiment, it is clear that micellar casein permeates the permeate side in the membranes of all pore sizes. Therefore, dialysis with water was performed to obtain micellar cases of any pore size. It is clear that it is possible to effectively remove casein and lower molecular weight lactose and to relatively concentrate the MFGM component. For example, the nominal pore size is 6
Even if a membrane with a large pore size of μm is used, as shown in FIG.
From the fact that the actual particle size of MFGM is distributed over 0.5 μm to about 60 μm and the actual pore size of the membrane is distributed from a smaller pore size, it can be easily understood that concentration is possible.

Example 4 Effect of buttermilk temperature during microfiltration The effect of the processing temperature of the raw buttermilk when producing MFGM by microfiltration on the components, membrane permeation rate and recovery rate of the microfiltration MFGM preparation. investigated. The apparatus and method were the same as in Example 1. However, the processing temperature is 5 ° C, 13
It carried out at ° C, 20 ° C, 35 ° C, 50 ° C, 60 ° C, 70 ° C. The temperature of water when water was added and dialyzed was also used as the treatment temperature. The average flow rate of MFGM at each temperature (permeate flow rate per membrane area) and the concentration solution (microfiltration MFGM preparation before freeze-drying corresponding to retentate 4 in Example 1) by the near infrared analyzer Ingredients, total solids, yield (raw buttermilk K
(per g) is shown in Table 2.

[0034]

[Table 2] Table 2 ──────────────────────────────────── Average concentrate component MFGM yield Rate Temperature Flow rate Protein Fat Lactose Total solids (g / raw butter (L / m^Twoh) (%)^* (%)^* (%)^* (%)^** Per kg of milk ──────────────────────────────────── 5 ℃ 102 0.28 0.10 0.02 0.41 2.01 13 ℃ 145 0.29 0.08 0.03 0.41 1.92 20 ° C 86 0.55 0.19 0.01 0.77 1.64 35 ° C 486 0.29 0.11 0.02 0.43 1.10 50 ° C 545 0.28 0.16 0.03 0.48 1.19 60 ° C 523 0.31 0.14 0.03 0.49 1.15 70 ° C 98 0.34 0.13 0.03 0.51 1.07 ────── ─────────────────────────────── ^* By near-infrared analyzer,^**By dry method

As a result, the recovery rate of MFGM tended to be higher as the treatment temperature was lower. The membrane throughput per unit time is expressed by the average flow rate, which is the highest at 50 ° C.
It decreased when the temperature was below or 70 ° C. From these results, it is desirable to carry out microfiltration at a low temperature of 5 ° C to 20 ° C to increase the recovery rate of MFGM, and to increase the membrane throughput per hour, 35 ° C to 60 ° C.
It is desirable to carry out at a moderate temperature. Thus, it is considered that the method of the present invention can be carried out in a wide range from 5 ° C to 70 ° C.

[0036]

According to the present invention, MFGM can be obtained from buttermilk by a simple method. Moreover, it does not require any complicated purification steps such as the addition of a solvent for purification, other chemicals, salting out with ammonium sulfate, isoelectric point precipitation by pH adjustment, and centrifugation. It is possible to get minutes.

[Brief description of the drawings]

FIG. 1 is a diagram showing a particle size distribution of fresh cream, skim milk and buttermilk.

FIG. 2 is a diagram showing a particle size distribution of a stock solution (retention solution 4) of a microfiltration MFGM preparation produced in Example 1 before freeze-drying.

FIG. 3 is an SDS-polyacrylamide gel electrophoretic diagram of the water-washed MFGM preparation prepared in Test Example 2 and the microfiltration MFGM preparation prepared in Example 1.

FIG. 4 is an SDS-polyacrylamide gel electrophoresis diagram of the water-washed MFGM preparation prepared in Test Example 2 and the microfiltration MFGM preparation prepared in Example 1.

FIG. 5: Buttermilk was prepared with a nominal pore size of 0.5 μm and 1.0
It is a figure which shows the particle size distribution of the permeate at the time of processing with a microfiltration membrane of (mu) m or 2.0 micrometers.

FIG. 6 is a diagram showing a particle size distribution of a retentate when buttermilk is treated with a microfiltration membrane having a nominal pore diameter of 2.0 μm.

[Procedure amendment]

[Submission date] January 9, 1996

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0034

[Correction method] Change

[Correction contents]

[0034]

[Table 2]

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0035

[Correction method] Change

[Correction contents]

As a result, the recovery rate of MFGM tended to be higher as the treatment temperature was lower. The processing capacity of the membrane per time is expressed by the average flow rate, but the maximum at 50 ° C
It decreased when the temperature was lower than 35 ° C or 70 ° C. From these results, it is necessary to increase the recovery rate of MFGM from 5 ° C to 2 ° C.
It is desirable to carry out microfiltration at a low temperature of 0 ° C,
Further, in order to improve the throughput of the film per hour, it is desirable to carry out at a temperature of 35 ° C. or higher and about 60 ° C. Thus, it is considered that the method of the present invention can be carried out in a wide range from 5 ° C to 70 ° C.

 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Masaki Yamane, 465-1 Waatsu, Hiroshima-cho, Sapporo-gun, Hokkaido Yotsuba Dairy Co., Ltd. Research Center (72) Fuji-shi Shiji, 465-1 Wa-atsu, Hiroshima-cho, Sapporo-gun, Hokkaido Banchi Yotsuba Dairy Co., Ltd. Research Center

Claims (2)

[Claims] 1. A milk fat globule characterized by treating a buttermilk with a microfiltration membrane having a pore size of 0.5 to 6.0 μm to separate a milk fat globule membrane-containing fraction contained in the buttermilk. Method for producing a membrane-containing fraction. 2. A milk fat globule membrane-containing fraction is obtained by treating buttermilk with a microfiltration membrane having a pore size of 0.5 to 6.0 μm, and adding water to the retentate that has not permeated the membrane to perform dialysis treatment. A method for producing a highly purified milk fat globule membrane-containing fraction, which comprises concentrating.