Method for treating sweet whey material containing cgMP and related method for producing protein material having target tryptophan / threonine ratio

Abstract

The present invention relates to methods for treating sweet whey materials containing CGMP and related methods for producing proteinaceous materials having a target tryptophan / threonine ratio. The present invention discloses a method for treating a sweet whey material (SWM) containing cGMP (casein glycomacropeptide). Also disclosed is a method for producing a protein material having a target tryptophan / threonine (Trp / Thr) ratio from SWM cGMP.

Description

[0001] This application is a divisional application of PCT application PCT / EP2016 / 052174, filed on February 2, 2016, entitled "Method for processing sweet whey material containing CGMP and related methods for producing protein material with a target tryptophan / threonine ratio". The date of entry into the Chinese national phase of the PCT application was August 3, 2017, and the application number was 201680008543.5. Technical Field

[0002] This invention relates to a method for processing sweet whey material containing cGMP (casein glycomacropeptide), and a related method for producing protein material from sweet whey material containing cGMP (casein glycomacropeptide), said protein material having a target tryptophan / threonine ratio. Background Technology

[0003] US Patent 687158 relates to a method for extracting glycomacropeptides or casein glycomacropeptides (“cGMP”) from lactic acid raw materials. cGMP is a phosphorylated and partially sialylated macropeptide formed by the action of a protease (e.g., rennet) on mammalian milk k-casein. cGMP accounts for approximately 20% by weight of the protein in sweet whey obtained after casein separation during cheese making.

[0004] The method includes the following steps: removing cations from a lactic acid raw material for a sufficient duration to obtain a substantially deionized lactic acid raw material having a pH of about 1 to 4.5; contacting the substantially deionized lactic acid raw material with an anion exchange resin having a hydrophobic matrix at a sufficient temperature for a sufficient duration to remove cGMP from the substantially deionized lactic acid raw material and obtain a treated liquid material; separating the resin from the treated liquid material; and rinsing the resin to obtain cGMP therefrom. The actual removal of cGMP is in the range of 85% to 91% of the initial cGMP.

[0005] The processed liquid material obtained from sweet whey has a reduced threonine content and is rich in aromatic amino acids such as tryptophan. It can be used as a protein source or raw material in infant or dietary products, in pharmaceutical compositions used in combination with antithrombotic agents, antidiarrheal agents, or antibacterial agents, or as an emulsifier, foaming agent, or gelling agent in food compositions.

[0006] However, its amino acid composition, particularly the content of tryptophan and threonine, makes the treated liquid not always suitable for hypoallergenic formulations, and manufacturers have to mix it with at least one different protein source and / or add selected amino acids.

[0007] Furthermore, the duration of the treatment, as well as the amounts of resin and treated liquid, are selected based on the composition of the starting materials and the amount of cGMP to be removed. In practice, this can be achieved through experiments in field operations, but there are no clear theoretical rules to guide the implementation of this treatment.

[0008] Therefore, one object of the present invention is to provide a method for processing sweet whey materials containing cGMP based on a simple and effective setting, or at least to provide a useful alternative.

[0009] Another related object of the present invention is to provide a method for producing protein materials from sweet whey materials containing cGMP, said protein materials having a target tryptophan and threonine content obtained by using said method, or at least providing a useful alternative. Summary of the Invention

[0010] In a first aspect of the invention, a method for processing sweet whey material containing cGMP (casein glycomacropeptide) is provided, the method comprising the following steps: - Decation of sweet whey materials to obtain sweet whey with a pH value of 1 to 4.5; - The sweet whey is treated in a fluidized bed reactor containing a specific volume of anion exchange resin at a temperature between 10 and 18°C, wherein the sweet whey contacts the resin such that the resin absorbs between 0% and 100% of the cGMP present in the sweet whey; and - Recycle protein materials; The treatment is carried out for a sufficient time to allow the resin to absorb 30 to 42 g / L, preferably between 35 and 42 g / L, and more preferably between 39 and 41 g / L of cGMP present in sweet whey.

[0011] The inventors have discovered, surprisingly, that this method possesses a key parameter corresponding to the maximum cGMP absorption in the resin, which remains essentially constant regardless of the method employed. This maximum value is reached after a sufficient period of time. This allows the method of the present invention to be implemented in a simple and efficient manner.

[0012] This method advantageously makes protein materials suitable for use in hypoallergenic infant formula. It eliminates the need to remove high levels (85% to 91% by weight) of cGMP as previously done, resulting in a treated material that is substantially cGMP-free. The treated liquid is mixed with at least one different protein source and / or amino acid source for suitability for infant formula. In other words, cGMP may still be partially present in the protein material.

[0013] Furthermore, surprisingly, regardless of the resin's cGMP uptake level, the resin absorbs undesirable products such as anions (typically present in whey) during the processing according to the invention, such that these products are present in the protein material at acceptable levels (trace impurities), regardless of the percentage of cGMP uptake in the resin.

[0014] In a second aspect of the invention, a method is provided for producing a protein material from a sweet whey material containing cGMP (casein glycomacropeptide), said protein material having a target tryptophan / threonine ratio, wherein said method comprises the following steps: - The method according to the invention is applied to sweet whey material, wherein a resin absorbs a percentage of cGMP present in sweet whey (P1 percentage) to obtain a first protein material, and the contents of tryptophan (Trp) and threonine (Thr) in the first protein material are measured to obtain the ratio Trp / Thr1. - The method according to the invention is applied to sweet whey material, wherein the resin absorbs cGMP present in the sweet whey at a P2 percentage, to obtain a second protein material, and the contents of tryptophan (Trp) and threonine (Thr) in the second protein material are measured to obtain the ratio Trp / Thr2. - By positioning the points (Trp / Thr1; P1) and (Trp / Thr2; P2) on the coordinate graph and drawing a line through these two points, a linear calibration curve is plotted on the coordinate graph that provides the percentage of cGMP absorbed by the resin as a ratio of Trp / Thr. - By using the plotted linear calibration curve, the specific proportion of cGMP present in sweet whey that the resin should absorb relative to the target tryptophan / threonine ratio was determined; and - Applying the method according to the invention to sweet whey material, wherein the resin absorbs a specific proportion of cGMP present in the sweet whey to obtain a protein material having a target tryptophan / threonine ratio.

[0015] This method advantageously allows for the adjustment of the method according to the invention for each sweet whey protein material to meet the target tryptophan / threonine ratio of the protein material. The tryptophan / threonine ratio is generally selected based on the suitability of the protein material in infant formula, preferably in hypoallergenic infant formula.

[0016] Without being bound by any theory, it is believed that the linear calibration curve can be plotted by utilizing the fact that the resin absorbs 30 to 42 g / L of cGMP for a sufficient time according to the method of the present invention. Attached Figure Description

[0017] Figure 1This is a schematic diagram of the device used in the method of the present invention.

[0018] Figure 2 This is a graph showing the tryptophan (Trp) content relative to the threonine (Thr) content for the sweet whey material WPC 31.5, indicating the corresponding percentage of cGMP removal (see double arrow).

[0019] Figure 3 The graph shows two calibration curves. One calibration curve provides the cGMP removal (in percentage) of sweet whey material WP 31.5 relative to the Trp / Thr ratio, and the other calibration curve provides the cGMP removal (in percentage) of sweet whey material WP 80 relative to the Trp / Thr ratio. Detailed Implementation

[0020] To fully understand the invention and its advantages, reference is made to the following detailed description of the invention.

[0021] It should be understood that the various embodiments of the present invention can be combined with other embodiments of the present invention, and are merely examples of specific ways of preparing and using the present invention, and do not limit the scope of the present invention when considered in light of the claims and the following detailed description.

[0022] The following terms are defined in this specification and should be taken into consideration when reading and interpreting the specification, embodiments, and claims.

[0023] The following terms and expressions are used in this article and have the following meanings.

[0024] The term "suitable for infant formula" means that the product can be used directly in infant formula without any modifications. This means that it is not necessary to mix the product with at least one different protein source and / or add selected amino acids.

[0025] The term "compound removal" refers to the process by which compounds present in a product are absorbed into the resin, resulting in a product with a lower content of that compound. The corresponding percentage is the percentage of compounds removed from the product through resin absorption.

[0026] The term "infant" refers to a child under 12 months of age.

[0027] The term "infant formula" refers to food specifically designed to provide nutrition for infants aged 4 to 6 months and which meets the diverse nutritional needs of these infants (in accordance with Article 1.2 of European Commission Directive 91 / 321 / EEC of 14 May 1991 concerning infant formula and follow-up formula). See also the exemptions for that EU directive.

[0028] The terms “including,” “contains,” and similar words used in this specification should not be construed as exclusive or exhaustive. In other words, these terms are used to mean “including but not limited to.”

[0029] Any references to prior art documents in this specification should not be construed as an admission that such prior art is well-known or constitutes part of common general knowledge in the art.

[0030] In a preferred embodiment of the method according to the invention, the treatment is carried out for a sufficient time so that the resin absorbs between 10% and 90% of the cGMP present in the sweet whey.

[0031] Advantageously, the resin absorbs at least 90% of the anions present in sweet whey. The anions are typically selected from chloride, phosphorus, citrate, sulfate, and lactate. Specifically, the resin advantageously absorbs at least 90% of the chloride and phosphorus present in sweet whey.

[0032] In a preferred embodiment of the method according to the invention, the treatment of sweet whey in a fluidized bed reactor is carried out at a protein-to-resin ratio of 0.10 to 0.35, preferably 0.20 to 0.35 kg protein / L resin.

[0033] In a preferred embodiment of the method according to the invention, the treatment of sweet whey in a fluidized bed reactor is carried out at a ratio of 0.25 to 1.25 kg dry matter / L resin.

[0034] In a preferred embodiment of the method according to the invention, P1 is 55% and P2 is 90%.

[0035] The decation step essentially does not alter the anion or cGMP content in the sweet whey material. Therefore, the resin's absorption of cGMP and anions may be related to their content in the sweet whey material, or vice versa. Here, we choose to refer to their content in the sweet whey.

[0036] The cGMP quantity relative to the resin quantity makes the process and method according to the invention suitable for any fluidized bed reactor, since the cGMP quantity represents the sweet whey material and the resin quantity represents the reactor design.

[0037] The maximum cGMP value that the resin can bind helps users determine the amount of sweet whey material to be treated after knowing the resin volume.

[0038] The cGMP content of the liquid in the fluidized bed reactor can be checked by HPLC analysis, thereby monitoring the reaction duration. The reaction duration can also be monitored by measuring the pH of the liquid: the reaction ends once the pH reaches a certain constant. However, HPLC analysis is preferred because it is more accurate.

[0039] cGMP can be initially measured in sweet whey material, or roughly estimated as 20% of the protein content of sweet whey material. According to the present invention, initial cGMP measurement by HPLC is preferred.

[0040] According to the present invention, the sweet whey material may be one of the following: sweet whey obtained after separation of casein coagulated with rennet; sweet whey concentrate; sweet whey or whey demineralized by electrodialysis, ion exchange, reverse osmosis, electrodeionization, or a combination of these processes; sweet whey concentrate demineralized by electrodialysis, ion exchange, reverse osmosis, electrodeionization, or a combination of these processes; protein concentrate of substantially lactose-free sweet whey obtained by ultrafiltration followed by perfiltration (with washing); mother liquor from which lactose crystallizes from sweet whey; permeate from sweet whey ultrafiltration; a product of hydrolysis of natural casein obtained by skim milk by acidification with inorganic acids or by bio-acidification, or by microfiltration of skim milk, under the action of proteases; or a product of hydrolysis of caseinate salts under the action of proteases. Preferably, the sweet whey has a solids content of about 6% to 30% by weight after decationization.

[0041] Sweet whey materials are typically liquids that can be obtained by dispersing and / or dissolving solid whey powder in a liquid.

[0042] Advantageously, the resin is treated with an alkaline material before contact with sweet whey. Preferably, the sweet whey is contacted with the resin in a gently stirred reactor at a temperature below 50°C for one to ten hours to adsorb a suitable amount of cGMP onto the resin. A suitable resin is alkaline and exists in the form of a macroporous or macrocrosslinked gel. The sweet whey is typically contacted with the resin until the treated liquid material reaches a constant pH between about 4.2 and about 5.8, indicating that the reaction has been completed. Advantageously, the sweet whey and resin are present in a volume ratio of 1:1 to 30:1, preferably 1:2 to 1:10.

[0043] The protein materials obtained by the method according to the invention are protein sources intended for human use, particularly for infants, and especially for infant formula. The term "intended for use" means that they are particularly suited to the nutritional needs of the target population. In addition to the protein materials according to the invention, those skilled in the art also know of ingredients that can be used in such nutritional compositions to make them suitable as supplements or nutritionally complete compositions.

[0044] These nutritional foods meet all dietary and / or regulatory requirements, meaning that in addition to the protein source, they contain additional components such as available carbohydrate sources and lipid sources.

[0045] The chlorine content of the protein material is typically between 1 mg / 100g, preferably between 5 and 80 mg / 100g, and / or the phosphorus content of the protein material is between 50 and 150 mg / 100g, preferably between 90 and 160 mg / 100g.

[0046] The ratio of tryptophan to threonine in protein materials is generally between 0.240 and 0.450, and more preferably between 0.300 and 0.430.

[0047] The accuracy of analytical methods for measuring the amino acid content of protein materials is generally + / - 8.5% to 11% (by weight). The accuracy of analytical methods for measuring the threonine content of protein materials is generally + / - 8.5%. The accuracy of analytical methods for measuring the tryptophan content of protein materials is generally + / - 11%.

[0048] The protein material is preferably suitable for producing hypoallergenic infant formula. Generally, the protein material is subjected to a hydrolysis step before being incorporated into the infant formula. This hydrolysis step is well known to those skilled in the art. This hydrolysis does not alter the amino acid composition, particularly the Trp / Thr ratio. More generally, several steps may be performed on the protein material before incorporating it into the infant formula, as long as this does not alter the amino acid composition, particularly the Trp / Thr ratio. Advantageously, according to the invention, no other protein source or amino acid is added to the protein material obtained by the method according to the invention.

[0049] Figure 1 The apparatus used in the method of the present invention is shown. Reactor 1 has a main tank 2 connected to a lower section in its upper part, the lower part having a compartment 3 with a diameter smaller than that of tank 2. Tank 2 has a flushing liquid inlet channel 4, an inlet 5 allowing pressurized gas to enter, and a safety valve 6 for regulating the gas pressure in reactor 1. Near the base of tank 2, there are filters 7 and channels 8 for discharging liquid.

[0050] The reactor connected to compartment 3 has a pH meter 9, a gas inlet 10, a three-way valve 11 connected to an inlet channel 12 for the liquid to be treated, and a discharge channel 13 for removing the treated liquid. The base of compartment 3 has a mesh or perforated plate 14 for collecting resin microspheres 15. Below the mesh 14, discharge channel 16 removes liquid to a buffer tank 18 via pump 17, which has a level control device 19. Channel 20 removes liquid from buffer tank 18 via pump 21. Channel 20 is connected to channel 12 or to a discharge overflow 22.

[0051] A method of using the device is now described, which is implemented in the following embodiments.

[0052] The initial sweet whey material (a dispersion of whey powder in water) was previously decationized via a cationic resin column in the following sequential order: weak / strong / strong. The resulting sweet whey was introduced into reactor 1 via channel 12. Air was introduced into compartment 3 via one-way valve 23 through inlet 10 through the base bubble flow. A fluidized bed of resin microspheres 15 was established, which contained a weak anionic resin (IMAC HP 661, Rohm & Haas) based on a hydrophobic polystyrene matrix. - (Form regeneration). The resin microspheres 15 are stirred for 4 hours, and due to the turbulence generated by fluidization, these resin microspheres come into contact with the dispersion. The pH of the liquid is constantly controlled by pH meter 9. Constant analysis of sweet whey by high performance liquid chromatography (“HPLC”) (not shown) indicates when the reaction removes 55% of the cGMP present in the sweet whey. At this point, due to the removal of the desired amount of cGMP, the air supply at inlet 10 is cut off, and air is introduced above liquid level 24 through inlet 5 at the top of the reactor. The liquid is pressurized, and the resin microspheres settle in the lower part of compartment 3 of reactor 2, where they are trapped by grid 14. The treated liquid material is discharged by gravity and / or pumped through channel 8 and through channel 16 toward buffer tank 18 by means of pump 17. The treated liquid material is then discharged through channel 20 by means of pump 21 and guided to the outlet by channels 12 and 13.

[0053] The treated liquid material is standardized and pH adjusted, concentrated by evaporation or nanofiltration, and the concentrate is spray-dried in a drying tower.

[0054] cGMP recycling is optional. However, this is in... Figure 1As shown in the diagram. To recover cGMP, the reactor and resin are washed with deionized water introduced via valve 26 through inlet channel 25 and through inlet channel 4, and flushed through channels 12 and 13. cGMP is eluted twice with a 2% NaOH aqueous solution introduced via channel 27 and valve 28 through the same loop, and flushed with 30 L of deionized water. After combining the eluent and wash volumes, the volume is concentrated by ultrafiltration or nanofiltration using a membrane with a nominal molecular weight cutoff of 3000 Daltons to obtain effluent and filtrate. The effluent is then freeze-dried.

[0055] Once the volume equivalent to 10 volumes of resin bed has been processed, the resin can be periodically regenerated acidically after alkaline regeneration. After eluting cGMP with the alkaline solution described above, the resin is washed with a concentrated HCl aqueous solution supplied by channel 29 and valve 30, and then washed with water supplied by channel 25 and valve 26. The resin is converted to OH- by passing a concentrated NaOH aqueous solution supplied by channel 27 into channel 4, followed by passing water from channel 25 into channel 4. - The solution is removed from reactor 1 via channel 16 and transferred to buffer tank 18 via pump 17. The solution is then removed from buffer tank 18 via pump 21 and discharged through channel 20 and overflow 22 for effluent treatment. After this operation, the resin is ready for the next processing cycle.

[0056] The treated liquid is removed and used as a protein material according to the invention.

[0057] The invention will now be further described with reference to the following embodiments. It should be understood that the invention protected by the claims is not intended to be limited in any way to these embodiments.

[0058] Example

[0059] Example 1 (according to the present invention): A method for removing different percentages of cGMP from sweet whey material WPC 31.5 And to produce proteins with a target Trp / Thr ratio using sweet whey material containing cGMP WPC 31.5 and WPC 80 as raw materials. Methods for high-quality materials

[0060] The sweet whey material was whey concentrate WPC 31.5. It was decationized using a weak / strong / strong cation exchange resin. The weak resin was IMAC HP 336, and the strong resin was IMAC 1110Na, both sold by Dow Chemical (formerly Rohm and Haas). This sweet whey had a protein content of approximately 31.5% DM (dry matter), a total solids content of 18%, and a pH of 1.75. 4420 kg of this sweet whey was pumped into reactor 1 containing 7500 L of weak anion exchange resin (HP 661 food grade). The entire volume of sweet whey was brought into contact with the resin. The resin and sweet whey were suspended together at 15–18°C for 4 hours. The pH increased from 1.75 to a final pH of 5.1–5.3 within the 4-hour reaction time. cGMP removal was monitored by HPLC.

[0061] After a 4-hour reaction time, the resulting demineralized and cGMP-free whey is pumped out of the reactor. This protein material is discharged, and the resin is washed with water to minimize protein and dry matter loss. cGMP is recovered through a combined elution and regeneration with 4% NaOH. After regeneration, the NaOH is discharged with water, and the reactor is washed until the pH reaches approximately 10.5. Once this pH is reached, the reactor is ready for the next production run. After standard neutralization with NaOH and KOH, the product is heat-treated, evaporated, and spray-dried.

[0062] Data related to this method is summarized in Table 1 below. .

[0063]

[0064] Repeat this method several times to obtain the composition. Figure 2 The coordinate graph disclosed herein provides the tryptophan (Trp) content relative to the threonine (Thr) content for the sweet whey material WPC 31.5. Each point of the curve data corresponds to the Trp and Thr values ​​measured for the protein material obtained by the processing method according to the invention, performed at a given cGMP value. The corresponding percentage of cGMP removal is shown in the figure. Figure 2 The figure is roughly indicated (see double arrow). The curve shows a linear relationship between Trp content and Thr content.

[0065] Depend on Figure 2 The conclusion is Figure 3The calibration curve for sweet whey material WPC 31.5 is provided. This calibration curve provides the cGMP removal (expressed as a percentage) of sweet whey material WP 31.5 relative to the Trp / Thr ratio. The curve shows a linear relationship between the percentage of cGMP removal and the Trp / Thr ratio. Similarly, another linear calibration curve is plotted by drawing a line through the two points, based on the values ​​for sweet whey material WP 80 seen in Examples 4 (point (0.411; 90%)) and 5 (point (0.36; 55%)).

[0066] According to the present invention Figure 3 The calibration curve determines the specific proportion of cGMP to be removed from a given sweet whey material containing cGMP (in this example, WPC 31.5 or WPC 80) in order to obtain protein material with a target tryptophan / threonine ratio.

[0067] Example 2 (according to the present invention): Method for removing 90% of cGMP from sweet whey material according to the present invention

[0068] This example is based on the same WPC 31.5 with 90% cGMP removal as in Example 1. However, the reactor is different, and the pretreatment of the whey material is also different.

[0069] The sweet whey material was whey concentrate WPC 31.5. It was subjected to electrodialysis, followed by decation with a weak / strong / strong cation exchange resin, and then ultrafiltration. The weak resin was IMAC HP 336, and the strong resin was IMAC 1110Na, both sold by Dow Chemical (formerly Rohm and Haas). This sweet whey had a protein content of approximately 31.5% DM (dry matter), a total solids content of 18%, and a pH of 1.85. 5900 kg of this sweet whey was pumped into a reactor containing 8,500 L of weak anion exchange resin (HP 661 food grade). The entire volume of sweet whey was brought into contact with the resin. The resin and sweet whey were suspended together at 15–18°C for 4 hours. The pH increased from 1.85 to a final pH of 5.25 within the 4-hour reaction time. cGMP removal was monitored by HPLC.

[0070] After a 4-hour reaction time, the resulting demineralized cGMP sweet whey decreased by 55%, and the protein material was pumped out of the reactor. The protein material was discharged, and the resin was washed with water to minimize protein and dry matter loss. cGMP was recovered through a combined elution and regeneration with 4% NaOH. After regeneration, the NaOH was discharged with water, and the reactor was washed until the pH reached approximately 10.5. Once this pH was reached, the reactor was ready for the next production run. After standard neutralization with NaOH and KOH, the product was heat-treated, evaporated, and spray-dried.

[0071] Data related to this method are summarized in Table 2 below. .

[0072]

[0073] Considering measurement accuracy, the Trp / Thr ratio is the same as the result obtained in Example 1.

[0074] Example 3 (according to the present invention): Method for removing 55% cGMP from sweet whey material according to the present invention

[0075] The sweet whey material was whey concentrate WPC 31.5. It was decationized using a weak / strong / strong cation exchange resin. The weak resin was IMAC HP 336, and the strong resin was IMAC 1110Na, both sold by Dow Chemical (formerly Rohm and Haas). This sweet whey had a protein content of approximately 31.5% DM (dry matter), a total solids content of 18%, and a pH of 1.75. 6785 kg of this sweet whey was pumped into a reactor containing 8,500 liters of weak anion exchange resin (HP 661 food grade). The entire volume of sweet whey was brought into contact with the resin. The resin and sweet whey were suspended together at 15–18°C for 4 hours. The pH increased from 1.75 to a final pH of 4.90 within the 4-hour reaction time. cGMP removal was monitored by HPLC.

[0076] After a 4-hour reaction time, the resulting demineralized cGMP sweet whey decreased by 55%, and the protein material was pumped out of the reactor. The protein material was discharged, and the resin was washed with water to minimize protein and dry matter loss. cGMP was recovered through a combined elution and regeneration with 4% NaOH. After regeneration, the NaOH was discharged with water, and the reactor was washed until the pH reached approximately 10.5. Once this pH was reached, the reactor was ready for the next production run. After standard neutralization with NaOH and KOH, the product was heat-treated, evaporated, and spray-dried.

[0077] Data related to this method are summarized in Table 3 below. .

[0078]

[0079] Example 4 (according to the present invention): Method for removing 90% of cGMP from sweet whey material according to the present invention

[0080] The sweet whey material was whey concentrate WPC 80. It was decationized using a weak / strong / strong cation exchange resin. The weak resin was IMAC HP 336, and the strong resin was IMAC 1110Na, both sold by Dow Chemical (formerly Rohm and Haas). This sweet whey had a protein content of approximately 82% DM (dry matter), a total solids content of 12%, and a pH of 3.40. 3100 kg of this sweet whey was pumped into a reactor containing 11,600 liters of weak anion exchange resin (HP 661 food grade). The entire volume of sweet whey was brought into contact with the resin. The resin and sweet whey were suspended together at 15–18°C for 4 hours. The pH increased from 3.40 to a final pH of 5.1–5.3 within the 4-hour reaction time. cGMP removal was monitored by HPLC.

[0081] After a 4-hour reaction time, the resulting demineralized cGMP sweet whey decreased by 55%, and the protein material was pumped out of the reactor. The protein material was discharged, and the resin was washed with water to minimize protein and dry matter loss. cGMP was recovered through a combined elution and regeneration with 4% NaOH. After regeneration, the NaOH was discharged with water, and the reactor was washed until the pH reached approximately 10.5. Once this pH was reached, the reactor was ready for the next production run. After standard neutralization with NaOH and KOH, the product was heat-treated, evaporated, and spray-dried.

[0082] Data related to this method is summarized in Table 4 below. .

[0083]

[0084] Therefore, the protein material obtained by the method according to the invention with 55% cGMP removed surprisingly exhibits the same mineral composition as the 90% removal method, making the protein material suitable as a protein source for hypoallergenic infant formula.

[0085] Example 5 (according to the present invention): Method for removing 55% cGMP from sweet whey material according to the present invention

[0086] The sweet whey material was whey concentrate WPC 80. It was decationized using a weak / strong / strong cation exchange resin. The weak resin was IMAC HP 336, and the strong resin was IMAC 1110Na, both sold by Dow Chemical (formerly Rohm and Haas). This sweet whey had a protein content of approximately 82% DM (dry matter), a total solids content of 12%, and a pH of 3.40. 4235 kg of this sweet whey was pumped into a reactor containing 11,600 liters of weak anion exchange resin (HP 661 food grade). The entire volume of sweet whey was brought into contact with the resin. The resin and sweet whey were suspended together at 15–18°C for 4 hours. The pH increased from 3.40 to a final pH of 4.80 within the 4-hour reaction time. cGMP removal was monitored by HPLC.

[0087] After a 4-hour reaction time, the resulting demineralized cGMP sweet whey decreased by 55%, and the sweet whey was pumped out of the reactor. The sweet whey was discharged, and the resin was washed with water to minimize protein and dry matter loss. cGMP was recovered through a combined elution and regeneration with 4% NaOH. After regeneration, the NaOH was discharged with water, and the reactor was washed until the pH reached approximately 10.5. Once this pH was reached, the reactor was ready for the next production run. After standard neutralization with NaOH and KOH, the product was heat-treated, evaporated, and spray-dried.

[0088] Data related to this method are summarized in Table 5 below. .

[0089]

[0090] Therefore, the protein material obtained by the method according to the invention with 55% cGMP removed surprisingly exhibits the same mineral composition as the 90% removal method, making the protein material suitable as a protein source for hypoallergenic infant formula.

[0091] Although the invention has been described by way of example, it should be understood that variations and modifications may be made without departing from the scope of the invention as defined in the claims. Furthermore, if known equivalents exist for specific features, these equivalents should be introduced as expressly mentioned in this specification.

Claims

1. A method for processing sweet whey material containing cGMP (casein glycomacropeptide), the method comprising the following steps: - The sweet whey material is decationized to obtain sweet whey with a pH value of 1 to 4.5; - The sweet whey is treated in a fluidized bed reactor containing a specific volume of anion exchange resin at a temperature between 10°C and 18°C, wherein the sweet whey is contacted with the resin in the reactor such that the resin absorbs the cGMP present in the sweet whey at concentrations between 0% and 100%; and - Recycle protein materials; The treatment is carried out for a sufficient time to allow the resin to absorb 30 g / L to 45 g / L of the cGMP present in the sweet whey.

2. The method of claim 1, wherein the treatment is performed for a sufficient time to allow the resin to absorb between 10% and 90% of the cGMP present in the sweet whey.

3. The method according to any one of claims 1 and 2, wherein the resin absorbs 35 g / L to 42 g / L of the cGMP present in the sweet whey.

4. The method according to any one of claims 1 to 3, wherein the treatment is carried out for a sufficient time for the resin to absorb 39 g / L to 41 g / L of the cGMP present in the sweet whey.

5. The method according to any one of claims 1 to 4, wherein the treatment of the sweet whey in the fluidized bed reactor is carried out at a protein-to-resin ratio of 0.10 kg / L to 0.35 kg / L resin.

6. The method according to any one of claims 1 to 5, wherein the treatment of the sweet whey in the fluidized bed reactor is carried out at a protein-to-resin ratio of 0.20 kg / L to 0.35 kg / L resin.

7. The method according to any one of claims 1 to 6, wherein the treatment of the sweet whey in the fluidized bed reactor is carried out at a ratio of 0.25 kg to 1.25 kg dry matter / L resin.

8. A method for producing a protein material from sweet whey material containing cGMP (casein glycomacropeptide), said protein material having a target tryptophan / threonine ratio, said method comprising the following steps: - The method according to any one of claims 1 to 7 is applied to the sweet whey material, wherein the resin absorbs the cGMP present in the sweet whey at a P1 percentage to obtain a first protein material, and the contents of tryptophan (Trp) and threonine (Thr) in the first protein material are measured to obtain the ratio Trp / Thr1. - The sweet whey material is subjected to the method according to any one of claims 1 to 7, wherein the resin absorbs the cGMP present in the sweet whey at a P2 percentage, to obtain a second protein material, and the contents of tryptophan (Trp) and threonine (Thr) in the second protein material are measured to obtain the ratio Trp / Thr2. - A linear calibration curve is plotted on the coordinate graph that provides the percentage of cGMP absorbed by the resin relative to the Trp / Thr ratio by positioning the points (Trp / Thr1; P1) and (Trp / Thr2; P2) on the coordinate graph and drawing a line through these two points. - By using the plotted linear calibration curve, a specific proportion of cGMP present in the sweet whey that the resin should absorb relative to the target tryptophan / threonine ratio is determined; and - The sweet whey material is subjected to the method according to any one of claims 1 to 7, wherein the resin absorbs a specific proportion of cGMP present in the sweet whey to obtain the protein material having the target tryptophan / threonine ratio.

9. The method for producing protein materials according to claim 8, wherein P1 is 55% and P2 is 90%.

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