JPS61268138A - Production of modified whey protein concentrate - Google Patents

Abstract

PURPOSE:To produce a whey protein concentrate with reduced beta-lactoglobulin, by adjusting milk whey (protein concentrate) from which inorganic salt are removed to a proper pH, heating the milk whey, and collecting precipitate part. CONSTITUTION:Milk whey (protein concentrate) is passed through a plural bed column of a cation exchange resin and an anion exchange resin, >=90wt% inorganic salts are removed and the milk whey is adjusted to 3.6-5.0pH. Then the whey (protein concentrate) is heated at 40-80 deg.C for about 1hr, centrifuged, separated into pasty precipitate and a supernatant liquid, the precipitate is suspended in water, the suspension is neutralized with an alkali, dissolved, sterilized under heating, concentrated and dried to give whey protein concentrate powder with low content of beta-lactoglobulin.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for producing a modified whey protein concentrate.

More specifically, the present invention relates to a method for producing a modified protein concentrate with reduced β-lactoglobulin.

(Prior art) In general, whey produced in cheese production contains most of the water-soluble components in milk, except for fat and casein. It has been isolated and used for food and medicine.

Whey protein concentrate, which is obtained by separating excess lactose and removing remaining salts by desalting, is often used as a food material as is, but it contains Highly effective utilization that takes advantage of the characteristics of various proteins has not been made.

One of the reasons for this is that whey contains a large amount of β-lactoglobulin (hereinafter referred to as β-Lg). In other words, using whey protein as a protein source in food preparations for blue light is preferable in terms of protein utilization efficiency for infants, but β-Lg is a protein that hardly exists in breast milk, and may be used as an allergen depending on individual differences in infants. Sometimes it works.

Therefore, it has been expected as an industrial production technology to obtain whey protein with reduced or eliminated β-Lg.

Therefore, many attempts have been made to remove β-lactoglobulin from whey in order to effectively utilize whey protein. Next, those known techniques and their problems will be listed.

1. Co-precipitation method using polymer-rich turtle solute [J, Hidalgo] 4 Journal of Dairy Science (J, Dairy Sci)
),, 54°1270 (1971) and N. Melakouris (N.

Journal of
Agricultural Food Chemistry (J, A
gr.

Food Chem)-, 20,798 (1972)
) These methods are based on α-lactoglobulin (hereinafter α-La
) is a method of co-precipitation separation with β-Lg without reaction.

The problem with this method is that during coprecipitation, a small amount of highly charged polymer particles, which are foreign substances, remain, which is not preferable.

2 Salting out method [Shea Matsukuchi Armstrong (J.

McD, Armstrong) etc. 7 Hot Iohimika・
Biochimica e
t Biophysica+AC Cheney (ACT
A) Volume 147, page 60 In this method, when salts are added to milk whey, α-La and β-Lg have different solubility; 9. At p) 13.5, α-La is precipitated and β-Lg is dissolved at an ammonium sulfate concentration of about 27%.

The method is to separate this by filtration or centrifugation.

Although this method is suitable for high-purity separation and collection, it cannot be an industrial means because it uses a large amount of ammonium sulfate and is expensive.

5. Molecular sieve fractionation method [Nie Ringquist (A.

Preparative Biochemistry (Ljungquist) etc.
chemistry)”l 5: 131
゜This method separates whey by gel filtration or ultrafiltration based on the difference in molecular weight. For example, if whey is treated with a membrane with an average molecular weight cut-off of about 25,000, β-Lg will be concentrated, and α-Lg will be concentrated. La is separated by filtration.

However, as a result of examination as a practical problem, it was found that the pore sizes of industrially used membranes vary, making accurate separation difficult. Also, in gel filtration, the gel material is expensive,
Various troubles occurred within the column, which was not desirable.

4. Ion exchange chromatography method [Yaguchi
guchi) et al., Journal of Dairy Science (J, Dairy 5science),
Volume 44: 589 Water droplets pass whey through a layer of ion exchanger and adsorb proteins onto the carrier using electrostatic force. Next, this adsorbed protein is eluted and developed using an appropriate salt concentration gradient or -gradient, and α-La and β-Lg are separated and collected.

Although this method is relatively practical, there are problems with the price of the resin, staining of the resin, and recycling.

5. Isoelectric focusing method [C. H. Amundson (C,
H. Amundson), Whey Products Conference
rence ) October (0ctober) 2
1-22 (1980) Chicago Illinois
ago llinois)) This method has some similarities with the present invention. Generally, soluble proteins have a large number of polar groups in their molecules, and have a minimum solubility at the isoelectric point pH. At this time, if salts are present in the solution, these anions and old ions will bond with the polar groups of the protein and affect its solubility. In the case of whey protein, the isoelectric point pH of both α-La and β-Lg is around 4.5, and the two can be separated by adjusting the salt concentration or solution temperature. On page 7 of the same document, whey is UP
Concentrate and adjust pif to 4.65.

It is described that the precipitate obtained by electrodialytic desalting and readjustment of Kp)1 to 4.65 was centrifuged as a de-β-Lg fraction. However, this method is fundamentally different from the present invention in that it does not include a heating step and that the amount of β-Lg 1IJIi removed is used as the upper groove. Further, as a result of experimenting with this method, it was not possible to clearly separate α-La and β-Lg.

(Structure of the Invention) The present invention desalinates milk whey or milk whey protein concentrate by removing 90% or more of inorganic salts, and collects the resulting desalted solution by 3.6 ml.
- 5.0, then heating the adjusted solution to 40 to 80°C, and collecting the precipitate produced.
- A method for producing a modified protein concentrate with reduced Lg.

(Problem to be solved by the invention) When comparing the protein fractions of human milk and cow's milk based on analysis examples,
As per 1.

As is clear from Table 1, the concentration ratio of casein in cow's milk is significantly higher than that in human milk;
It can also be seen that human milk contains 14.8% of -Lg, but human milk does not contain it at all.

Table 1 also shows that β-Lg can sometimes be an allergen for infants, so when whey is to be used in infant preparations, β-Lg should be removed or reduced as much as possible. It should be said that it is preferable to use it as a whey protein concentrate.

(Means for Solving the Problems) In the present invention, first, milk whey or milk whey protein concentrate is desalted to remove 90% or more of inorganic salts, preferably for 9 days or more. For desalting, it is preferable to use an ion exchange resin, such as a mixed column of cation exchange resin and anion exchange resin. When the desalination of inorganic salts is 90% or more, α-La
If the precipitation rate of α-La is increased to 60 or more and the desalination is 98 or more, the precipitation rate of α-La can be increased to 9 or more.

Then, the desalination solution is adjusted to a pH of preferably 3.6 to 5.0.
Adjust to 4.2 to 4.4.

Generally, whey has a pti of about 41j, and when this is desalted using an ion exchange resin, it has a pti of about 41j.
．． decreases to 0. Pti&6~5.
0. Preferably, pli is adjusted to 4.2 to 4.4. pi
(3.6 to 5.0, α-L of 55 inches or more by heating
A precipitate of α-La is obtained, but when the pt is adjusted to 14.2 to 4.4, a precipitate of 80 or more α-La is obtained.

The desalination solution with a mea of 3.6 to 5.0 is heated to 40 to 80°C, preferably 45 to 70°C. When the heated liquid is left at that temperature for about 1 hour, a precipitate of α-La is formed, which can be separated into a paste-like precipitate and a supernatant by centrifugation.

Most of β-Lg and lactose are present in the supernatant,
When this supernatant is concentrated using an ultrafiltration membrane method, lactose and water permeate through the membrane, and β-Lg is blocked by the membrane, making it possible to obtain a concentrate consisting mostly of β-Lg. . Further, by concentrating and drying this, a β-Lg product can be obtained.

On the other hand, the precipitate contains most of α-La and other milk proteins, but the content of β-Lg is extremely low.

The precipitate is dissolved in water, neutralized with an alkali, heat sterilized, then concentrated and dried to prepare a powdered whey protein with an extremely low β-Lg content.

Since the obtained whey protein aMi product contains almost no α-Lg, it can be effectively used as a protein raw material for infant preparations and other foods.

Next, test examples and examples of the present invention will be shown.

Test Example 1゜ Cheese whey (...6.4) was packed in an ion exchange resin bottle (double-bed column filled with IR-120B, a cation exchange resin, and IRA-410, an anion exchange resin manufactured by Amberlite) The liquid was passed through.

The treated solution was 98% desalted compared to the original solution. This 98
% Desalted solution and undesalted stock solution are mixed appropriately to give 50%, 80%
Five levels of desalinated whey were prepared: 1, 90%, 95%, and 98%.

Using 5 levels of desalinated whey, 1% of each whey is -4
．． 6, heated to 60°C, held for 1 hour, centrifuged at 10.0 OOG for 10 minutes, and collected the precipitate. Analyze the precipitate part of the 5 mallets obtained in this way, *
The result of examining the extent to which β-Lg and α-La in cheese whey precipitated was $-2. It has been determined that a degree of desalination of 90% or more, preferably about 98% in consideration of efficiency etc., is most suitable for industrial purposes.

Test Example 2 Using the whey with a desalination degree of 98% prepared in Test Example 1,
This is divided into five parts, and the voices are 3.6, 4.0°4.6.4
．． Adjust the heating conditions to 5 stages of 6.5.0.

The method of collecting the precipitate was the same as in Test 1, and the results of examining the precipitation rate of β-Lg and α-La in the raw whey are shown in Table 3. It was confirmed that the most suitable value for the purpose of the present invention, which is to precipitate La at a high concentration, is around 4.3.

(10% hydroxide is used to adjust the contents) 17um and 10
Thihydrochloric acid was used.

Test Example 6 The 98% demineralized whey prepared in Test Example 1 was adjusted to a strength of 4.6 and heated. Heating conditions were 20℃, 40℃,
The mixture was maintained at trough temperature for 60 minutes in 6 steps of 60°C, 70°C, 80°C, and 100°C, centrifuged, and the precipitated portion was collected in the same manner as in Test 1.

Table 4 shows the results of investigating the precipitation rate of β-Lg and α-La in raw whey. β-α in the low range of Lg transfer rate
The condition for a high migration rate of -La is around 60°C, and if the holding time was shortened, the migration rate of β-Lg could be kept low even in the temperature range of 60°C to 80°C, but on the contrary, Since almost no increase in the precipitation rate of α-La can be expected, in consideration of the desired properties of the precipitated portion, it was determined that a holding condition of 60° C. for 60 minutes would be preferable for practical use.

Example 1 9,000 g of -6.6 cheese whey separated during the production of Gouda cheese by processing 10,000 Icg of milk
kg was used and the entire amount was passed through an ion exchange column.

The ion exchange tower contains a cation exchange resin 1-120 manufactured by Amberlite and an anion exchange resin ■A-1.
410 was packed into a double-bed column, and whey was passed through the column. Electrical conductivity ranges from 6000μη false before passing to 120 after passing.
It decreased to μ7f/cm and the difficulty decreased from 6.6 to 4.0. The desalination rate was 98%.

The voice of the obtained desalted solution was adjusted to 4.25 using 10% sodium hydroxide.

The resulting prepared solution was heated to 60° C. in a tank equipped with a jacketed heating stone and a stirrer, and maintained for 1 hour.

Next, the desalted whey was cooled to 40° C. and separated into a precipitate portion and a supernatant portion using an Alfa Laval MRPX-418 centrifuge. Tables 5 and 6 show the amounts and analytical values of the precipitate and supernatant obtained at this time, as well as the analytical values of the raw material whey.
, 7.

Table 5 (Analysis values of raw whey) Table 6 (Analysis values of supernatant part) After neutralizing the obtained precipitate with 10% NaOH solution, sterilization, concentration, and spray drying were performed according to a conventional method to remove β-Lg. , a desalinated, lactose-reduced modified whey protein powder was obtained.

The obtained modified whey protein powder is used as an additive to powdered milk for infants and other foods.

On the other hand, the supernatant portion was sterilized, concentrated, and dried according to conventional methods.
- Desalinated whey powder with a large Lg fraction can be obtained.

It is used as a normal milk ingredient, especially as a nutritional material, for food production.

Note that a β-Lg concentrate can be obtained by sterilizing the supernatant portion, concentrating it by ultrafiltration, and separating excess lactose by filtration. This can be effectively used as a special nutritional material for the production of nutritional foods.

When lactose is purified and collected, the desired product is obtained by concentrating, cooling, crystallizing, and centrifuging the lachrymal fluid using conventional methods.

(Effects of the Invention) The modified whey protein concentrate produced from milk whey or milk whey protein concentrate by the method of the present invention has a lower β-L content than milk.
Since the content of α-La is extremely low and α-La is relatively high, the composition approximates that of whey protein in human milk.For example, the modified whey protein concentrate according to the present invention contains 6 parts of protein and 4 parts of casein protein.
The composition of protein, which has not been put to practical use in the past, can also be brought close to that of human milk (by adding solubilized protein and adding lipids, carbohydrates, and other trace components to approximate the balance of ingredients to that of human milk). This became possible.

Agent Patent Attorney 1) Parent Male Procedural amendment (voluntary) July 2-6, 1985

Claims (2)

[Claims] (1) Remove 90% or more of inorganic salts from milk whey or milk whey protein concentrate, and desalinate the resulting desalted solution to pH 3.6.
-5.0, then heating the pH-adjusted solution to 40-80°C, and collecting the generated precipitate. A method for producing a modified protein concentrate with reduced β-lactoglobulin. . (2) The manufacturing method according to claim 1, wherein the desalting is desalting using an ion exchange resin.