WO2006058538A1 - Method for producing a denatured protein material - Google Patents

Method for producing a denatured protein material Download PDF

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Publication number
WO2006058538A1
WO2006058538A1 PCT/DK2005/000760 DK2005000760W WO2006058538A1 WO 2006058538 A1 WO2006058538 A1 WO 2006058538A1 DK 2005000760 W DK2005000760 W DK 2005000760W WO 2006058538 A1 WO2006058538 A1 WO 2006058538A1
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material
heating
protein
temperature
cooling
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PCT/DK2005/000760
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French (fr)
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Jesper Oldrup
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Cp Kelco Aps
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J3/00Working-up of proteins for foodstuffs
    • A23J3/14Vegetable proteins
    • A23J3/16Vegetable proteins from soybean
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J3/00Working-up of proteins for foodstuffs
    • A23J3/04Animal proteins
    • A23J3/08Dairy proteins
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A23B - A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/20Reducing nutritive value; Dietetic products with reduced nutritive value
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; THEIR TREATMENT, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

A process and a plant for the preparation of a microparticulated denatured protein material, such as microparticulated whey protein, with a means particle size of between a 0.1µm and 5µm in diameter. An aqueous solution or colloidal dispersion of a soluble or dispersible protein material is degassed, pre-heated to a temperature below 69.5°C, further heated by use of mechanical energy to a temperature (T) between 70 and 120°C in a period of time (td) between 5 and 300 seconds under mixing, and then quench cooled to a temperature below 55°C within a period of time (tq) of less than 30 seconds. The quench cooling ensures a desirable small particle size without aggregation or subsequent homogenization ensuring a microparticulated product with excellent or ganoleptic qualities with a non-gritty appearance, a suitable opacity, a homogeneous texture and a desirable viscosity in aqueous dispersion and a fat-like mouthfeel. The microparticulated protein is suitable as a texturing and water binding additive for use in both food products and non-food products including pharmaceutics and cosmetics. Thus the denatured protein can be used in attractive products endowed with a desirable appearance, texture and skinfeel or mouthfeel with a good consumers appeal.

Description

Microparticulated whey

Title: Method for producing a denatured protein material.

Technical field

The present invention relates to a process and a plant for the preparation of a microparticulated denatured protein material having a mean particle size of between 0.1 μm and 5μm in diameter, whereby an aqueous solution or colloidal dispersion, containing a suitable amount of a soluble or dispersible protein material is degassed, heated to a temperature above 70 0C and then cooled to a temperature below 55 0C. The invention also relates to a microparticulated denatured protein obtainable by the process and having excellent organoleptic characteristics and a food or beverage including a denatured protein material prepared by the process.

Technical background

The modern way of life with less physical activity has increased the demand of low calorie foods and beverages and especially such products having a low fat content. Unfortunately the fat component of foods and beverages is often very important for the organoleptic characters and therefore it can be difficult to provide low fat substitutes with acceptable organoleptic characters such as good taste and mouthfeel.

A possible way to compensate for the low fat content is addition of protein. In order to protect public health foods and beverages should often be subjected to a heat treatment to reduce microorganisms. By such heat treatment the proteins are denatured and the consistency or texture may be changed. Thus it can be desirable to denature the protein before it is added to the food or beverage as the consistency of the food or beverage in that case can be better maintained during a subsequent heat treatment.

The relationship between the particle size of denatured protein material and its or- ganoleptic properties has already been investigated extensively. All studies concur on the following correlation between particle size and organoleptic properties:

A mean particle size of 0.1 - 2 μm gives a desirable creamy mouthfeel, 2 - 6 μm gives a powdery texture whereas larger particles from 6 to 9 μm gives a chalky mouthfeel and particles larger than 9 μm are gritty. U.S. Pat. No. 4,734,287 (Singer et al.) discloses a product comprising a proteinaceous, water-dispersible, macrocolloid comprising substantially non-aggregated particles of dairy whey protein coagulate having mean diameter particle size distributions, when dried, ranging from about 0.1 μm to about 2.0 μm, with less than about 2 per cent of the total number of particles exceeding 3.0 μm in diameter, whereby the colloid has a substantially smooth, emulsion-like organoleptic character when hydrated. The product is produced by concentrating undenatured whey protein, forming an aqueous solution or colloidal dispersion of the undenatured whey protein containing 45%-55%, on a dry weight basis, of the undenatured whey protein, and then applying shear, in the pres- ence of heat, in an acidic environment. The proteinaceous, water-dispersible, macro- colloids produced are thereby denatured. The shear condition is provided with a cylindrical rotator inside a heated tube with a gab of 2 mm. The rotator is driven with a speed of about 1000 rpm providing a shear of about 500,000 min'1. In this gab the protein material is heat denatured at 90 - 120 0C in between 15 minutes and 3 seconds under high shear. This combined heat and high shear treatment requires a complex and expensive equipment and is difficult to control.

U. S. Patent 4,961 ,953 (Singer, et al.) discloses a similar denatured protein product. Suggested as suitable protein sources are animal, vegetable and microbial proteins in- eluding, egg and milk proteins, plant proteins, such as oilseed proteins obtained from cotton, palm, rape, safflower, cocoa, sunflower, sesame, soy, peanut, and the like, and microbial proteins such as yeast proteins and the so-called "single cell" proteins. Preferred are dairy whey protein, and "non-dairy-whey" proteins such as bovine serum albumin, egg white albumin, and vegetable whey proteins, such as soy protein. The de- naturing is obtained by a combined high shear and heat treatment at 5,080 rpm and 122 0C. The product is cooled during continued high shear to 40 0C within 2 minutes.

U.S. Pat. No. 6,605,311 (Villagran et al.) discloses a process for making non- aggregated macrocolloids of insoluble, denatured, heat-stable protein particles, with a degree of insolubility of at least 80%. The protein is denatured using a combination of heat and high shear. Once denatured the importance of rapid cooling of the particles during continued high shear mixing to a preferred temperature of less than about 700C is discussed. With rapid cooling is meant that the product preferably is cooled to this temperature in less than about 1 hour, more preferably in less than about 30 minutes. Cooling periods in the order of seconds, also termed quenching, are not suggested. U.S. Pat. No.5,171 ,603 (Singer et al.) discloses a process of producing a denatured protein material, which is shown to have a mean particle size of between 0.1 and 2.0 μm in diameter, which process comprise degassing, pre-heating, microcooking as well as 2 cooling steps. The microcooking is made under high shear conditions and the cooling in a scraped surface heat exchanger. The denaturing temperature is 200 0F (93.3 0C). In the first cooling step the material is cooled to 130 0F (54.4 0C) and in the second step 55 0F (12.8 0C). The starting material can be whey, casein micelles and/or egg white.

U.S. Pat. No. 5,350,590 (McCarthy et al.) discloses a water-dispersible, gravitational and heat-stable fat replacer composition for foods, which comprises co-formed agglomerates of at least partially denatured whey protein and desolubilized casein. The agglomerate is obtained by heating of an aqueous mixture of whey protein and casein with a pH of about 3.0 to 6.6 to at least partially denature the whey protein and cooling the mixture to a temperature below the whey protein denaturing temperature. The method requires presence of casein which does not give a denatured protein but is desolubilized and merely acts as a filler protecting against agglomeration to greater agglomerates. Without agitation the mean particle size of the agglomerate is 20 - 75 μm, and with conventional agitators (stirrers) the mean size will typically be about 15 μm. To obtain an optimum organoleptic size the mean agglomerate size should be less than about 7 μm, especially less than about 2.5 to 3 μm. To obtain such size it is necessary to use a suitable disruptive treatment during or immediately after denaturization, e.g. homogenization.

A further known process for the preparation of microparticulated denatured whey from whey protein concentrate comprises pre-heating to 70 °C in a tube heat exchanger, heating in a scraped surface heat exchanger to 82 - 85 0C, maintenance at this temperature and then cooling to below 60 °C in a further scraped surface heat exchanger.

The prior art as referred to above provides useful denatured protein materials from water soluble or colloidal dispersible proteins and with suitable organoleptic characters. However, the prior art processes uses complicated technical equipments with expensive and/or specially prepared components.

Accordingly, there was a demand for a less complicated process using less complicated and less expensive equipment for the preparation of the above type of micropar- ticulated denatured protein materials with the desired organoleptic characters. It is an object of the present invention to provide a process and a plant meeting this demand.

Brief description of the invention Accordingly the present invention relates to a process for the preparation of a denatured protein material having a mean particle size of between 0.1 μm and 5μm in diameter, whereby an aqueous solution or colloidal dispersion, containing a suitable amount of a soluble or dispersible protein material is degassed, heated to a temperature above 70 0C and then cooled to a temperature below 55 0C, characterized in, that the heating and cooling are carried out by a) pre-heating the material to a temperature below 69.5 0C, b) heating the material at a temperature (T) between 70 and 120 0C in a period of time (td) between 5 and 300 seconds under mixing, and c) cooling the material from step b) from the temperature T to a temperature below 55 0C within a period of time (tq) of less than 30 seconds.

The present invention also relates to a denatured protein material obtainable by the inventive process having a mean particle size of between 0.1 μm and 5μm in diameter, and a degree of denaturing between 50 and 100 % by weight of the protein material.

According to a preferred embodiment the microparticulated denatured protein material is obtained with a mean particle size of between 1.0 μm and 1.6 μm in diameter, preferably with at distribution of particle size having a single and narrow peak.

Furthermore the invention relates to a plant for the preparation of a denatured protein material having a mean particle size of between 0.1 μm and 5μm in diameter, from a degassed aqueous solution or colloidal dispersion, containing a suitable amount of a soluble protein material including a heating unit (8) and a cooling unit (24), characterized by comprising in the flow direction a) a conventional heating unit (4) pre-heating the material to a temperature below

69.5 0C, b) a heating unit (8) heating the material at a temperature (T) between 70 and 120 0C in a period of time (td) between 5 and 300 seconds, which heating unit is provided with a means for mixing (10, 12; 34) the material during the heating, whereby the mayor portion of or the entire heating energy supplied to in heating unit (8) is the mechanical energy, and c) a cooling unit (24) cooling the material from being under mixing at the temperature T to a temperature below 55 °C within a period of time (tq) of less than 30 seconds.

The present invention is based on the surprising finding that the desired particle size of the denatured protein can be obtained without the complicated simultaneous use of high shear and high temperature and/or subsequent homogenization as taught by the prior art if the protein after denaturing at the "denaturing temperature" T is quickly cooled (quenched) to a temperature below 55 0C within less than 30 seconds, if neces- sary less than 20 or 10 seconds, preferably less than 3 seconds, more preferred less than 1 second. It has surprisingly turned out that when this quenching time (tq) is sufficiently short aggregation of the denatured protein particles can be avoided.

Such quench cooling may be obtained by leading the hot material to a vessel having a large volume of the material cooled to a temperature well below 55 0C. Alternatively, the hot material can be lead to a cooling loop with circulating cooled material. In both cases the hot material is mixed with the cooled material almost instantly forming a mixture having a temperature below 55 0C. With such cooling arrangements the process and the plant will be substantially less complicated and less expensive in comparison with the prior art processes and plants.

The term "mean particle size" as used in the present specification and claims is the volumetric median D(50) particle size as measured in an aqueous dispersion by means of laser diffraction using Malvern 2000 (Malvern Instruments Limited, Malvern, Worces- tershire, United Kingdom). The dried sample is suspended in demineralised water for 3 hours prior to analysis. Air bubbles are removed and the sample is dispersed with the built-in ultrasound probe until steady particle size reading is achieved.

The extent of applicability of the invention appears from the following detailed descrip- tion. It should, however, be understood that the detailed description and the specific examples are merely included to illustrate the preferred embodiments, and that various alterations and modifications within the scope of protection will be obvious to persons skilled in the art on the basis of the detailed description.

Detailed description of the invention The starting material to be processed by the inventive process may be a solution of whey or any other type of soluble proteins. It will be appreciated that the term "solution" is often used in the whey protein art as a synonym for what is in fact a true colloidal dispersion of undenatured whey proteins. In the present specification the terms "solu- ble" and "solution" are intended to cover this broader meaning also including colloidal dispersible proteins and colloidal protein dispersions as well.

Examples of useful proteins are animal proteins, such as sweet or acid whey protein, bovine serum albumin, egg white albumin and fish proteins, plant proteins, such as oil- seed proteins obtained from cotton, palm, rape, safflower, cocoa, sunflower, sesame, soy, and peanut, and microbial proteins such as yeast proteins and the so-called "single cell" proteins.

The protein solution is first degassed in a conventional way. This may be done simply by allowing the solution to rest in a desired period of time prior to further treatment. Alternatively, a commercially available degasser can be used.

Prior to the denaturing step the degassed solution is pre-heated to a temperature below the "denaturing temperature" (T) under gentle conditions ensuring a minimal de- gree of denaturing during the pre-heating. The pre-heating temperature should be below 69.5 0C. Typical pre-heating temperatures are 50 - 69 0C, preferably 55 - 65 0C. For the gentle pre-heating a plate heat exchanger is suitable.

In the next step the material is heated to a "denaturing temperature", T, defined as a temperature at which the proteins are substantially denatured, typically between 70 and 120 0C in a period of time ("denaturing time"; td) between 5 and 300 seconds. During this heating step which may also be termed a "denaturing step" the material is subjected to mixing with sufficient shear to prevent aggregation. However, this shear treatment need not to be a high shear as suggested in US 4,734,287.

The degree of denaturing calculated as the percentage by weight of denatured protein based on the total weight of protein in the obtained product depends on the protein in question as well as the relation between the heating temperature (denaturing temperature; T) and the heating time (denaturing time; td) in the heating step (step a). The re- quired degree of denaturing depends on the end use of the denatured protein product and especially the conditions of any further processing the denatured protein product will be subjected to for such end use. Thus in case the end application does not involve further heat treatment above the denaturing level a low degree of denaturing down to 50 % by weight will be acceptable. On the other hand, in case the end application requires a high temperature treatment such as UHT treatment the degree of denaturing obtained by the inventive process should be in the upper range such as 70 - 98 % by weight. Thus an important feature is that further denaturing after the inventive process is avoided.

The "degree of denaturing" as referred to in the present specification and claims is de- termined by centrifugation of a 5 % by weight solution of the protein material, such as a solution of whey, in 0.1 M NaCI and adjusted to pH 6.6 at 9,000 rpm for 30 min in a Sorvall® RC5B refrigerated superspeed centrifuge with a Sorvall® GS-3 insert (available from Kendro Laboratory Products, Asheville, NC. USA). Using an approximate calculation based on the assumption that the volume of the initial protein solution and the volume of the supernatant are approximately the same the degree of denaturing is calculated as the difference in protein concentration of the initial solution and that of the clear supernatant divided by the initial protein concentration:

Degree of denaturing = (Ci - Cc)/Ci x 100 % wherein

Ci = initial protein concentration

Cc = protein concentration in clear supernatant.

Total protein content is determined as nitrogen content multiplied with 6.38 (based on the normal nitrogen content of milk proteins). The total nitrogen is determined by Kjeldahl or by an equivalent method.

Total dry matter is determined by drying at 105 0C to constant weight.

According to the invention the material is first pre-heated to a temperature below 69.5 0C (step a). Thereafter the material is heated to the temperature T in the heating or denaturing step (b) which heating is provided by use of mechanical energy as the major or the sole heating source. Such mechanical heating may be provided by pumps or other mechanical means. To ensure that the material reaches a temperature close to T almost instantly the heating can be provided in a heating loop with one or more pumps providing both heating and circulation of the material. A suitable velocity for this circu- lating flow is selected to give the desired denaturing temperature T and the desired denaturing time td. As an example a circulation velocity 20 - 75 fold the velocity of the material flow fed to the heating loop may be used. The pumps providing the heating energy as mechanical energy need not to be high shear devices and are exemplified by conventional centrifugal pumps. Alternatively the mixing in the denaturing step can be carried out in a scraped surface heat exchanger in which case supplementary heat optionally may be supplied by injection of steam.

The next step (step c) is an important feature of the present invention and may be termed a quenching, that is a quick cooling of the material from being under mixing at the denaturing temperature T to a temperature below 55 °C within a period of time ("quenching time"; tq) of less than 30 seconds, if necessary less thaniO seconds, preferably within 3 seconds, most preferred within 1 second.

In the present specification the term "quenching time" (tq) is defined at the time in seconds from the material being under mixing at the denaturing temperature, T, until it has been cooled to a temperature below 55 0C. The necessary short quenching time depends in practise of the level of the denaturing temperature T.

Experiments have shown that a denaturing temperature T = 90 °C requires a quenching time (tq) below 3 seconds. A higher T requires a shorter quenching time whereas a longer quenching time can be accepted with a lower T. Based on the results with T = 90 0C it can be expected that T = 80, 100 or 120 0C would require a quenching time (tq) shorter than about 10, 1 or 0.5 seconds, respectively.

This rapid cooling is an essential step in the process according to the invention. Thus it was found that a sufficiently short quenching time ensures that aggregation of the denatured protein particles can be avoided, whereby the desirably small particle size obtained during the denaturing step will be maintained.

In one embodiment this quenching may be carried out in a cooling loop with a cooler and one or more pumps circulating the flow. Typically the flow will be of the same or preferably a higher velocity than the processing flow velocity, preferably a velocity 2.5 - 10 fold the velocity of the material flow being processed. In another embodiment the hot flow of denatured protein can be quenched in a large volume of cooled material.

As a result of the rapid cooling giving a short or even ultra short transition time, at which the temperature of protein material shift from being at a temperature T with a substantial denaturing rate down to a temperature without noticeable denaturing, in practice below 55 0C, it was found possible to obtain a mean particle size (D50) of 0.1

- 5 μm, preferably 0.7 - 3 μm, more preferred between 1.0 and 1.6 μm in diameter.

Furthermore the obtained distribution of particle size shows a single narrow peak which is preferred among persons skilled in the art .

The exposure of protein material containing considerable amounts of undenatured protein particles to high sterilisation temperatures may cause continued aggregation of the proteins resulting in that the mean particle size of the protein material increase and thus deviate from the organoleptically acceptable particle size range, which is from about 0.1 μm to about 5.0 μm. Thus, as already explained above it is an important feature that a sufficient degree of denaturing depending on any expected subsequent treatments, especially heat treatments, is obtained by the inventive process.

It has further been found that the process according the invention is not limited to the treatment of protein solutions having a relatively low content of proteins on dry matter basis. Thus the starting aqueous solution or colloidal dispersion may contain from 25 and up to about 100 % by weight of protein on dry matter basis. Thus even purified whey protein such as whey protein isolate (WPI) from which lactose and fat have been removed can be processed according to the present invention without aggregation of the protein particles. This is surprising as the lactose contained in whey is considered to have a protecting effect avoiding aggregation of the protein particles.

Accordingly, the starting aqueous solution or colloidal dispersion of protein may be any of the standard protein products available on the market such as standard whey protein product obtainable from a dairy plant. Typically standard whey products have a protein content on dry matter basis of 30 to 40 % by weight, 50 to 60 % by weight, 75 to 85 % by weight or 85 to 95 % by weight. The possibility of using aqueous solutions containing the above protein concentrations in a simple denaturation process according to the invention offers a range of new possibilities in the production of protein based consumable additives.

The protein material produced according to the present invention may suitable be used as a fat replacer and/or nutritive protein additive in the production of consumables such as foodstuff, beverage products or the like, especially produced for human consumption. Non-limiting examples of such consumables include milk or milk-based products, cheese, coffee-white ner, ready to use drinks, and dried food supplements.

The organoleptic qualities of the obtained protein product are excellent with a non-gritty appearance, a suitable opacity, a homogeneous texture and a desirably viscosity in aqueous dispersion and a fat-like mouthfeel.

The pH of the solution may be adjusted at any step prior to denaturing. A pH in the range of from about 5.5 to about 7.5 is preferred. A pH in the range of from about 6.1 to about 6.3 is especially preferred. The pH of the solution can be adjusted using any food grade base or acid.

According to a preferred embodiment of the present invention the heating and cooling can be carried out as a continuous process.

The quench cooling down to a temperature below 55 °C is essential to avoid aggregation. In practice the material will often be cooled to a temperature far below this tem- perature such as below 45 0C or even below 30 0C in order to reduce or avoid growth of microorganisms.

Once the suspension of the denatured protein has been cooled it can be dried, preferably by spray drying, or stored as a suspension for use at a later time. Alternatively, the suspension could be utilized directly in the manufacture of food and beverage products, for example in dairy products.

The denatured protein is suitable as a texturing and water binding additive for use in both food products and non-food products including pharmaceutics and cosmetics. Thus the denatured protein can be used in attractive products endowed with a desirable appearance, texture and skinfeel or mouthfeel with a good consumers appeal. Brief description of the drawing

Fig. 1 is a schematic diagram illustrating the principle of the method and plant according to the invention. Fig. 2 is a schematic diagram illustrating a modified embodiment of the method and plant shown in Fig. 1.

The principle of the method and the plant according to the invention is shown schematic in Fig. 1. An aqueous solution, containing a suitable amount of a soluble protein material is first degassed in a conventional way and then fed by a feed pump 1 pressurising the system to about 0.1 - 1 MPa (1 - 10 bar) such as 0.2 MPa through an inlet 2 to a heater, which in the shown embodiment can be exemplified with a conventional plate heat exchanger 4. In the plate heat exchanger the degassed protein solution is pre-heated to a temperature below the temperature level at which perceptible denatur- ing takes place, normally 50 - 63 0C, under gentle conditions ensuring a minimum level of denaturing.

The pre-heated protein solution is lead through a conduct 6 to a heating unit, which in the shown embodiment is a heating loop 8, provided with pumps 10 and 12 ensuring a sufficiently high flow velocity of the material as shown with arrows 14 and 16. The material circulating in the loop 8 is heated by the mechanical energy provided by the pumps 10 and 12 to a temperature T at which substantial denaturing occurs, normally between 70 and 120 0C depending on the proteins contained in the material. The circulation in the loop 8 ensures that the pre-heated protein solution entering through the conduct 6 almost instantly reaches the temperature T at which substantial denaturing occurs. The circulation provided with the pumps 10 and 12 ensure a sufficient mixing during the denaturing. Only a relative moderate shear is necessary to avoid aggregation during the denaturing step. Suitable pumps for this mixing are conventional centrifugal pumps. From the heating loop 8 the denatured protein containing material is lead out through a conduct 18.

The relative velocities of the flows in conduct 6, the loop 8 and the conduct 18 are adapted to provide a heat treatment at the temperature T for a period of time (td) between 5 and 300 seconds. The heat energy supplied to the material flowing in the loop 8 may be monitored by monitoring the energy supplied to the pumps 10 and 12. The effect delivered to the material in the loop 8 can be regulated by means of valves 20 and 22, by changing the size of the pump wheel and/or by changing speed of the pump.

The denatured protein containing material in the conduct 18 is lead to a cooling loop 24 including a cooling means which in the shown embodiment is a plate heat exchanger 26 and a pump 28 circulating the material flow in the loop 24. The direction of the circulating flow may be in the direction shown with an arrow 30 but it is also possible with a circulation in the opposite direction. The hot material from the conduct 18 meets in a quenching point 32 with the cold flow circulating in the cooling loop 24 and practically instantly the temperature drops to a temperature where no further denaturing takes place. In this way the denatured protein containing material leaving the heating loop through the conduct 18 will be cooled from the "denaturing temperature", T, to a temperature below 55 0C within a period of time of less than 30 seconds. After cooling the denatured material leaves the plant through a valve 33.

The period of time from the material being under mixing at the temperature T in the heating loop 8 until the material reaches a temperature below 55 0C is termed the quenching time (tq).

In practice, provided the velocity of the circulation in the cooling loop 24 is sufficiently high, the quenching time (tq) will be the period of time from leaving the heating loop 8 until reaching the quenching point 32.

The distance in the conduct 18 from the heating loop 8 to the quenching point 32 is preferably as short as possible in order to obtain a short quenching time. In this way it is possible to obtain quenching times below 3 seconds or even below 1 second.

Fig. 2 shows a modified embodiment of the method and plant according to the invention wherein the heating unit is a pump 34. The effect delivered to the material can be regulated by means of valve 36, by changing the size of the pump wheel and/or by changing speed of the pump. The remaining parts of the plant shown in Fig. 2 are similar to those of the plant shown in Fig. 1 and similar parts has been given the same reference number.

The following examples further describe and demonstrate embodiments within the scope of the present invention. These examples are given solely for the purpose of il- lustration and are not to be construed as a limitation of the present invention, as many variations thereof are possible without departing from the invention's spirit and scope.

EXAMPLES

Example 1

The inventive method can be carried out on the plant shown in Fig. 1. A whey protein material containing 53 % by weight of whey proteins on dry mater basis is fed as an aqueous solution having a dry matter content of 35 % by weight with a velocity of 2 m3/h at a pressure of 0.2 MPa through the conduct 2. The pre-heated material leaves the plate heat exchanger 4 at 60 °C. The flow velocity in the heating loop is approximately 75 m3/h and the temperature in the loop is about 93 0C and the average holding time at 93 0C is about 60 seconds. The pumps 10 and 12 each provide a pressure of about 0.5 MPa and operates at a pump efficiency of approximately 0.27 (27%). The flow velocity in the cooling loop is 10 m3/h and the temperature after the plate heat exchanger is 12 0C. The mixture of the recycled material after the pump 28 and the hot material from the conduct 18 will be about 28 0C. The hot material will be quenched to 28 0C within 2.5 seconds after leaving the heating loop 8 through a 25.4 mm (1 inch) pipe (conduct 18).

The mean particle size D(50) was 1.3 μm (Malvern 2000). The degree of denaturing was 65 % by weight. The organoleptic character was estimated by a tasting panel of 4 people to be creamy.

Example 2

In this example the method was carried out in the same way as in example 1 with the exception that the hot material was quenched from 93 0C to 28 0C within 1.7 seconds after leaving the heating loop 8 through a 50.8 mm (2 inch) pipe. The mean particle size D(50) was 1.3 μm (Malvern 2000). The degree of denaturing was 67 % by weight. The organoleptic character was estimated by a tasting panel of 4 people to be creamy.

Example 3

In this example the method was carried out in the same way as in example 1 with the exception that the hot material was quenched from 93 0C to 28 0C within 10 seconds after leaving the heating loop 8 through a 50.8 mm (2 inch) pipe. The mean particle size D(50) was 5.4 μm (Malvern 2000). The degree of denaturing was 63 % by weight. The organoleptic character was estimated by a tasting panel of 4 people to be gritty.

Example 4 In this example the method was carried out in the same way as in example 1 with the exception that the starting material was a protein material containing 77 % by weight of proteins on dry mater basis which was fed as an aqueous solution having a dry matter content of only 24 % by weight. The mean particle size D(50) was 1.4 μm (Malvern 2000). The degree of denaturing was 63 % by weight. The organoleptic character was estimated by a tasting panel to be creamy.

Example 5

Commercially available 80 % by weight whey protein concentrate (WPC), Lacprodan® 80 from ArIa, Denmark, was used for the preparation of an aqueous 19.4 % by weight solution and the solution was left at 5 0C over night to remove air.

A laboratory plant simulating a plant as shown in Fig. 2 was used. In this laboratory plant the pump 34 and the valve 36 were replaced by a reaction vessel designed as a cup with a lid and provided on the lid with a mechanical shaft seal for a shaft with an impeller inside the cup and driven with a motor with variable speed drive (Ultra Turrax® T50 from IKA® Werke, Germany). In this reaction vessel the material will be subjected to conditions simulating the conditions in a centrifugal pump.

The whey solution was fed with a flow rate of 120 ml/min with a peristaltic pump (Mas- terflex® L/S Model 7518-00 with 6 - 600 pump drive LS Model 7553-79, equipped with a hose with inner diameter 6 mm, available from Cole-Parmer Instrument Co. LTD, United Kingdom) through a tubular heat exchanger to increase the temperature to 66 0C. Thereafter the material was lead to the above described reaction vessel. The speed of the impeller was adjusted to 10,000 rpm maintaining the temperature at 88 °C. The volume of the reaction vessel was 134 ml. Based on the flow rate and the vessel volume and average residence time (denaturing time td) in the vessel can be calculated to 67 seconds.

The length of the quenching pipe was 13 mm and the inner diameter 4 mm giving a quenching time tq of approximate 1 second before the denatured material meets a cooling loop. The cooling loop included a peristaltic pump (Jencons Perimatic GP) mounted with a flexible pipe and a cooling spiral in ice water. The flow rate was adjusted to give a temperature of approximately 33 0C at the quenching point 32. To control the flow out from the plant another peristaltic pump was used (FillMaster™ Type 311 ; Nordson Corporation, Ohio, USA).

The mean particle size D(50) was 1.48 μm (Malvern 2000). The degree of denaturing was 55.6 % by weight. The organoleptic character was estimated by a tasting panel to be creamy.

Example 6

Commercially available 60 % by weight whey protein concentrate (WPC), Lacprodan® 60 from ArIa, Denmark, was used for the preparation of an aqueous 26.7 % by weight solution and the solution was left at 5 0C over night to remove air.

Using a laboratory plant as described in example 5 the whey solution was fed with a flow rate of 110 ml/min through a tubular heat exchanger to increase the temperature to 66 0C. Thereafter the material was lead to the reaction vessel. The speed of the impeller was adjusted to 10,000 rpm maintaining the temperature at 88 0C. The volume of the reaction vessel was 110 ml. Based on the flow rate and the vessel volume and av- erage residence time (denaturing time td) in the vessel can be calculated to 60 seconds.

The length of the quenching pipe was 13 mm and the inner diameter 4 mm giving a quenching time tq of approximate 1 second before the denatured material meets a cooling loop. The cooling loop included a peristaltic pump (Jencons Perimatic GP) mounted with a flexible pipe and a cooling spiral in ice water. The flow rate was adjusted to give a temperature of approximately 15 °C at the quenching point 32. To control the flow out from the plant another peristaltic pump was used (FillMaster™ Type 311 ; Nordson Corporation, Ohio, USA).

The mean particle size D(50) was 1.53 μm (Malvern 2000). The organoleptic character was estimated by a tasting panel to be creamy.

Having now described several embodiments of the present invention it should be clear to those skilled in the art that the forgoing is illustrative only and not limiting, having been presented only by way of exemplification. Numerous other embodiments and modifications are contemplated as falling within the scope of the present invention as defined by the appended claims thereto.

Claims

Claims
1. A process for the preparation of a denatured protein material having a mean particle size of between 0.1 μm and 5μm in diameter, whereby an aqueous solution or col- loidal dispersion, containing a suitable amount of a soluble or dispersible protein material is degassed, heated to a temperature above 70 0C and then cooled to a temperature below 55 0C, characterized in, that the heating and cooling are carried out by a) pre-heating the material to a temperature below 69.5 0C, b) heating the material at a temperature (T) between 70 and 120 0C in a period of time (td) between 5 and 300 seconds under mixing, and c) cooling the material from step b) from the temperature T to a temperature below 55 0C within a period of time (tq) of less than 30 seconds.
2. A process according to claim 1 , characterised in, that the heating in step (b) is provided by use of mechanical energy as the major or the sole heating source.
3. A process according to one of the claims 1 - 2, characterised by cooling the material from step (b) from the temperature T to a temperature below 55 0C within a period of time (tq) of less than 10 seconds.
4. A process according to one of the claims 3, characterised by cooling the material from step (b) from the temperature T to a temperature below 55 0C within a period of time (tq) of less than 3 seconds.
5. A process according to claim 4, characterised by cooling the material from step (b) from the temperature T to a temperature below 55 0C within a period of time of less than 1 second.
6. A process according to one of the preceding claims, characterised in, that the protein material is selected from the group consisting of whey protein, egg protein, fish protein, soy protein, and/or other proteins suitable for use in production of consumable products and/or mixtures thereof.
7. A process according to claim 6, characterised in, that the protein material in- eludes whey protein.
8. A process according to one of the preceding claims, characterised in, that the denatured protein material has a mean particle size of between 1 and 3 μm in diameter, preferably between 1 and 1.6 μm.
9. A process according to one of the preceding claims, characterised in, that the degree of denaturing of the obtained denatured protein material is from 50 to 100% by weight, particularly between 60 and 75% by weight.
10. A process according to one of the preceding claims, characterised in, that the starting aqueous solution or colloidal dispersion includes between 25 % and 95 % by weight of protein material based on dry matter.
11. A denatured protein material obtainable by the process of one of the above claims, having a mean particle size of between 0.1 μm and 5 μm in diameter, and a degree of denaturing between 50 and 100 % by weight of the protein material.
12. A denatured protein material according to claim 11 , having a mean particle size of between 1.0 μm and 1.6 μm in diameter.
13. A plant for the preparation of a denatured protein material having a mean particle size of between 0.1 μm and 5μm in diameter, from a degassed aqueous solution or colloidal dispersion, containing a suitable amount of a soluble protein material including a heating unit (8) and a cooling unit (24), characterized by comprising in the flow direction a) a conventional heating unit (4) pre-heating the material to a temperature below
69.5 0C, b) a heating unit (8) heating the material at a temperature (T) between 70 and 120 0C in a period of time (td) between 5 and 300 seconds, which heating unit is provided with a means for mixing (10, 12; 34) the material during the heating, whereby a mayor portion of or the entire heating energy supplied to in heating unit (8) is the mechanical energy, and c) a cooling unit (24) cooling the material from being under mixing at the temperature T to a temperature below 55 0C within a period of time (tq) of less than 30 seconds.
14. A plant as claimed in claim 13, characterized in, that the heating unit (8) comprises one or more pumps (10, 12; 34) and that the mayor portion of or the entire heating energy supplied to in heating unit (8) is the mechanical energy supplied by the pump(s) (10, 12: 34).
15. A plant as claimed in claim 14, characterized in, that the heating unit (8) is a heating loop with one or more pumps (10, 12) circulating the flow, and that the mayor portion of or the entire heating energy supplied to the heating unit (8) is the mechanical energy supplied by the pump(s) (10, 12).
16. A plant as claimed in claim 13, 14 or 15, characterized in, that the cooling unit (24) is a cooling loop with cooler (26) and one or more pumps (28) circulating the flow.
17. A food or beverage including a denatured protein material prepared by the proc- ess as claimed in one of the claims 1 - 10 or a denatured protein material according to one of the claims 11 - 12.
18. A pharmaceutical or cosmetical composition including a denatured protein material prepared by the process as claimed in one of the claims 1 - 10 or a denatured pro- tein material according to one of the claims 11 - 12.
PCT/DK2005/000760 2004-11-30 2005-11-29 Method for producing a denatured protein material WO2006058538A1 (en)

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