CREATINE-PROTEIN MATRIX AND METHOD FOR PRODUCING SAID MATRIX

Abstract

The invention relates to a powdery creatine-protein matrix comprising a protein component and a creatine-component for use as a food supplement for athletes and to a method for producing said creatine protein matrix. Said matrix has an improved solution behaviour compared to powder mixtures with the same composition.

Claims

1.-16. (canceled)

17. A creatine protein matrix comprising: i) at least one protein component selected from the group consisting of whey protein concentrates, whey protein isolates, whey protein hydrolysates and mixtures thereof, having a protein content in dry matter of at least 55 wt. %; and, ii) at least one creatine component selected from the group consisting of creatine, a salt thereof, creatine monohydrate and mixtures thereof, wherein the creatine protein matrix is in the form of a powder having a mean particle size of from 10 to 250 m, and at least 50% of the powder contains particles wherein each individual particle comprises both the creatine component and the protein component.

18. The creatine protein matrix of claim 17, wherein the creatine protein matrix further comprises iii) at least one mineral component selected from the group consisting of alkali or alkaline earth salts of phosphoric acid, diphosphoric acid, triphosphoric acid, citric acid, lactic acid, gluconic acid, double salts and mixtures thereof, wherein the creatine component and the mineral component are dispersed in the protein component.

19. The creatine protein matrix of claim 17, wherein the creatine protein matrix comprises: i) from 50 to 95 wt. % of the protein component; ii) from 5 to 40 wt. % of the creatine component; and, iii) not more than 10 wt. % water.

20. The creatine protein matrix of claim 18, wherein the creatine protein matrix comprises: i) from 50 to 95 wt. % of the protein component; ii) from 5 to 40 wt. % of the creatine component; iii) from 0 to 10 wt. % of the mineral component; and, iv) not more than 10 wt. % water.

21. The creatine protein matrix of claim 17, wherein the creatine protein matrix or the protein component is lactose-free.

22. The creatine protein matrix of claim 17, wherein the protein component is a whey protein concentrate, a whey protein isolate or a whey protein hydrolysate having a protein content of at least 75 wt. % protein.

23. The creatine protein matrix of claim 17, wherein the creatine protein matrix or the protein component comprises not more than 10 wt. % fats and/or not more than 10 wt. % water.

24. The creatine protein matrix of claim 18, wherein the alkali or alkaline earth salt of phosphoric acid, diphosphoric acid, triphosphoric acid, citric acid, lactic acid or gluconic acid is selected from the group consisting of sodium dihydrogen phosphate, disodium hydrogen phosphate, trisodium phosphate, calcium hydrogen phosphate, tricalcium phosphate, dicalcium dihydrogen phosphate, calcium tetrahydrogen phosphate, sodium dihydrogen citrate, disodium hydrogen citrate, trisodium citrate, calcium citrate, tricalcium dicitrate, sodium lactate, calcium lactate, sodium gluconate and calcium gluconate.

25. The creatine protein matrix of claim 17, wherein the creatine protein matrix is in the form of a powder having a mean particle size of from 10 to 100 m.

26. The creatine protein matrix of claim 17, wherein the creatine protein matrix or the protein component establishes a pH of pH 7.0 to 8.0 in water.

27. The creatine protein matrix of claim 17, wherein the creatine protein matrix or the protein component establishes a pH of pH 7.1 to 7.8 in water.

28. The creatine protein matrix of claim 17, wherein the creatine protein matrix has a calorific value of from 700 to 1700 kJ/100 g.

29. A food supplement for athletes, comprising the creatine protein matrix of claim 17.

30. A method for producing a creatine protein matrix in powder form, comprising: a) providing an aqueous, pasteurised solution or suspension Lq1 comprising at least one protein component selected from the group consisting of whey protein concentrates, whey protein isolates, whey protein hydrolysates and mixtures thereof, having a protein content in dry matter of at least 55 wt. %; b) preparing a solution or suspension Lq2 by adding at least one creatine component selected from the group consisting of creatine or a salt thereof, creatine monohydrate or mixtures thereof, and optionally at least one mineral component selected from the group consisting of alkali or alkaline earth salts of phosphoric acid, diphosphoric acid, triphosphoric acid, citric acid, lactic acid, gluconic acid and mixtures thereof, simultaneously or in succession to the solution or suspension Lq1 provided; and, c) drying the prepared solution or suspension Lq2 by means of spray drying, thin layer evaporation or roller drying methods.

31. The method of claim 30, wherein the solution or suspension Lq1 is lactose-free and/or comprises a whey protein concentrate, a whey protein isolate or a whey protein hydrolysate having a protein content of at least 55 wt. % (in dry substance).

32. The method of claim 30, wherein the solution or suspension Lq1 contains at least 30 wt. % dry matter.

33. The method of claim 30, wherein the solution Lq2, after addition of the creatine component and optionally the mineral component, is adjusted to a pH of pH 7.0 to 8.0 with a base.

34. The method of claim 30, wherein the solution Lq2, after addition of the creatine component and optionally the mineral component, is adjusted to a pH of pH 7.1 to 7.8 with a base.

35. An industrially produced creatine protein matrix in powder form comprising: i) at least one protein component selected from the group consisting of whey protein concentrates, whey protein isolates, whey protein hydrolysates and mixtures thereof, having a protein content in dry matter of at least 55 wt. %; and, ii) at least one creatine component selected from the group consisting of creatine, a salt thereof, creatine monohydrate and mixtures thereof, wherein the creatine protein matrix is in the form of a powder having a mean particle size of from 10 to 250 m and at least 50% of the powder contains particles wherein each individual particle comprises both the creatine component and the protein component, wherein the industrially produced creatine protein matrix in powder form is produced by the method of claim 30.

Description

[0092] The present invention will be explained in the following by means of examples, but the invention is not to be understood as being limited to the examples. In fact, any combination of preferred embodiments is likewise included in the present invention. In the figures

[0093] FIG. 1 shows a comparison of the powder diffractograms of a matrix according to the invention and crystalline creatine monohydrate.

EXAMPLES

[0094] The whey protein retentates or solutions used in the following examples formally yield, depending on the preceding treatment, either whey protein concentrates (WPC), whey protein isolates (WPI) or whey protein hydrolysates (WPH). This is to be understood as meaning that, if the solution Lq1 were to be dried without adding further ingredients, the particular product mentioned, specifically a whey protein concentrate, isolate or hydrolysate, would be formed.

Test Methods

1) Segregation

[0095] The homogeneity of the creatine protein matrix can be tested by means of a segregation test. In this test, the creatine protein matrix and a simple mixture (blend) of the three constituents are compared with one another. Both formulations are again mixed thoroughly before the test. For the test, the test mixture is placed in a funnel. The product is allowed to flow from the funnel onto a conveyor belt, which transports the product to a cylindrical receiving container. A cone of test material builds up in said receiving container, the fine material accumulating in the inner portion of the cone while the coarse material rolls along the outside edges. The inner portion of the cone can be removed from the receiving vessel through a central opening, while the outer portion of the cone remains in the vessel. The composition of the fractions thus obtained can then be tested. The homogeneity is determined by means of the covariance CV=SD100/mean, the mean being determined over all the analysis results (cone core and outside edges). If CV is <30%, the mixture can be assumed to be homogeneous with a low tendency to demixing; if CV is between 30 and 40%, a moderate tendency to demixing can be assumed, and at CV>40% a high tendency to demixing can be assumed.

2) Particle Size Distribution

[0096] The particle size distribution of the product is determined by means of laser diffraction. This procedure is suitable in particular for powders having a particle size <1000 m. Requirements and information regarding the design of the apparatus, system verification, sampling, sample measurement and the models for calculating the particle size distribution from the light scattering pattern can be found in ISO 13320:2009.

[0097] For the measurement, 10 g of sample are introduced via a transport chute into the sample chamber, through which a laser shines. The incoming particles cause refraction or deflection of the laser beam, depending on the particle size. The data can be converted into a particle size distribution by means of Fourier transformation. The mean particle size (x50 value) in m can be read off from the particle size distribution.

3) Bulk Density

[0098] For the bulk density, 200 g of sample are introduced in a free-flowing manner into a measuring cylinder via a funnel. The measuring cylinder containing the sample is allowed to stand for 10 minutes, and the volume is then read off. The bulk density is given in g/l.

4) Ingredients

[0099] Creatine and creatinine are determined by HPLC.

[0100] For determining the protein content, the nitrogen content is first determined by means of the Dumas or the Kjeldahl method. Via a conversion factor (N6.38 or N6.25), the protein content can be calculated, which must be corrected by the proportion of creatine present. Na, K, Ca and Mg are determined by means of atomic absorption spectroscopy.

Example 1

a) Production of the Creatine Protein Matrix in Powder Form

[0101] 1400 kg of ultrafiltered whey protein retentate (lactose-free (max. 0.1% i.d.m.), 40% dry matter, protein content 81% i.d.m., pH: 7.0 to 7.4) are placed, after being pasteurised, in a storage container which is adjusted to a temperature of 30 C. The retentate is stirred constantly. 108 kg of creatine MH (creatine monohydrate) are metered into the container, followed by 14 kg of tricalcium orthophosphate (solid metering). The mixture is stirred vigorously for 30 minutes until a homogeneous, cloudy solution is present. The pH is then checked and optionally adjusted to 7.2 to 7.4 with aqueous NaOH. The cloudy solution thus obtained is passed onto the spray tower via a heat maintenance section (80 C., 65 seconds) and spray dried. The air inlet temperature is 160 C., while a temperature of 78 C. prevails in the spray tower. Approximately 650 kg of a white to light-beige powder are obtained.

b) Characterisation of the Creatine Protein Matrix in Powder Form

[0102] The powder has the following composition: 81 wt. % whey protein concentrate, 14 wt. % creatine, 2 wt. % tricalcium orthophosphate, 3 wt. % water.

[0103] Lactose content: <0.1%

[0104] Creatinine content: <0.05%

[0105] Mean particle size: x50 value: 35 m

[0106] Bulk density: 400 g/l

[0107] Calorie content: 1300 kJ/100 g

[0108] Segregation test: CV<5%

[0109] The resulting creatine protein matrix according to Example 1 is an intimate mixture of the creatine component and the protein component, in which the components cannot be separated from one another. The creatine is present in homogeneously distributed and amorphous form in the protein matrix. The matrix produces a pH of 7.2 in water.

[0110] The amorphous state of creatine is shown in FIG. 1.

[0111] The figure shows a comparison between crystalline creatine monohydrate and a creatine protein matrix. The absolute intensities of the signals are plotted over the diffraction angle. It is clear from the comparison of the curves that only weak signals are recorded in the case of the co-processed mixture, which additionally cannot be correlated with creatine monohydrate. The absence of sharp diffraction reflections is an indication that the product contains scarcely any or no crystalline constituents; it is thus in amorphous form.

[0112] For the consumer, the creatine protein matrix represents a form of this food supplement which is easy to measure out. The product can, for example, easily be dispensed, provided with further ingredients (carbohydrates, fats, vitamins, sweeteners, etc.) or used as an ingredient for the preparation of foodstuffs, such as bars, for example. For direct consumption, the powder is advantageously flavoured and, under some circumstances, a colourant is added.

Example 2

a) Production

[0113] 1400 kg of partially hydrolysed whey protein retentate (40% dry matter, pH: 7.2 to 7.4, protein content 79% i.d.m.) are placed, after being pasteurised, in a storage container which is adjusted to a temperature of 30 C. 49 kg of creatine MH are metered into said container, followed by 10 kg of trimagnesium orthophosphate (solid metering). The mixture is stirred vigorously for 20 minutes until a slightly cloudy solution is present. The pH is then checked and optionally adjusted to 7.1 to 7.4 with NaOH. The suspension/paste thus obtained is dried on a roller dryer at 3.5 bar and a roller temperature of 120 C. Further conditions: roller speed 10 rpm. The resulting flakes are made into a powder by means of a powder mill. Approximately 610 kg of a white to light-beige powder are obtained.

b) Characterisation

[0114] The powder has the following composition: 90.4 wt. % whey protein hydrolysate, 7 wt. % creatine, 1.6 wt. % trimagnesium orthophosphate, 1 wt. % water.

[0115] Creatinine content: <0.05%

[0116] Bulk density: 250 g/l

[0117] Mean particle size: x50 value: 200 m

[0118] Calorie content: 1455 kJ/100 g

[0119] Segregation test: CV<5%

[0120] The resulting creatine protein matrix according to Example 2 is an intimate mixture of the creatine component and the protein component, in which the components cannot be separated from one another. The creatine is present in homogeneously distributed and amorphous form in the protein matrix. The matrix produces a pH of 7.3 in water.

Example 3

a) Production

[0121] 1400 kg of ultrafiltered whey protein retentate (50% dry matter, pH: 7.1 to 7.2, protein content 62% i.d.m.) are placed, after being pasteurised, in a storage container which is adjusted to a temperature of 35 C. 264 kg of creatine MH are metered into the container, followed by 46.6 kg of tricalcium dicitrate (solid metering). The mixture is stirred vigorously for 40 minutes until a homogeneous suspension/paste is present. The pH is then checked and optionally adjusted to 7.1 to 7.2 with KOH. The cloudy solution thus obtained is dried as in Example 1.

b) Characterisation

[0122] The powder has the following composition: 69 wt. % whey protein concentrate, 23 wt. % creatine, 5 wt. % tricalcium dicitrate, 3 wt. % water.

[0123] Creatinine content: <0.05%

[0124] Mean particle size: x50 value: 55 m

[0125] Bulk density: 280 g/l

[0126] Calorie content: 940 kJ/100 g

[0127] Segregation test: CV <5%

[0128] The resulting creatine protein matrix according to Example 3 is an intimate mixture of the creatine component and the protein component, in which the components cannot be separated from one another. The creatine is present in homogeneously distributed and amorphous form in the protein matrix. The matrix produces a pH of 7.2 in water.

Example 4

a) Production

[0129] 2500 kg of whey protein solution (40% dry matter, pH: 7.1 to 7.4, protein content 93% i.d.m.) are placed, after being pasteurised, in a storage container which is adjusted to a temperature of 50 C. In a second container, 800 kg of creatine MH are suspended in 1000 l of water at 20 C. The retentate and the creatine suspension are mixed with one another continuously and highly vigorously in a third container and then immediately passed onto the spray tower via a heat maintenance section (temperature: 85 C., 45 seconds) and spray dried. The air inlet temperature is 170 C., the spray tower temperature is 85 C. Approximately 1660 kg of a white to light-beige powder are obtained.

b) Characterisation

[0130] The powder has the following composition: 56.9 wt. % whey protein isolate, 40.0 wt. % creatine, 3 wt. % water.

[0131] Creatinine content: <0.05%

[0132] Mean particle size: x50 value: 40 m

[0133] Bulk density: 420 g/l

[0134] Calorie content: 940 kJ/100 g

[0135] Segregation test: CV<5%

[0136] The resulting creatine protein matrix according to Example 4 is an intimate mixture of the creatine component and the protein component, in which the components cannot be separated from one another. The creatine is present in homogeneously distributed and amorphous form in the protein matrix. The matrix produces a pH of 7.1 in water.

Example 5

a) Production

[0137] 236 kg of creatine MH and 10 kg of calcium lactate are added to 2000 kg of ultrafiltered whey protein retentate (40% dry matter, pH: 7.1 to 7.3, protein content 79% i.d.m.) and the mixture is mixed thoroughly and pasteurised for 5 minutes at 62 C. The mixture is then cooled to 30 C. The cloudy solution thus obtained is passed onto the spray tower via a heat maintenance section (90 C., 30 seconds) and spray dried. Approximately 1005 kg of a white to light-beige powder are obtained.

b) Characterisation

[0138] The powder has the following composition: 75.5 wt. % whey protein concentrate, 18.6 wt. % creatine, 1.0 wt. % calcium lactate, 4 wt. % water.

[0139] Creatinine content: 0.9%

[0140] Calorie content: 1190 kJ/100 g

[0141] Segregation test: CV <5%

Example 6

a) Production of the Creatine Protein Matrix in Powder Form

[0142] 1990 kg of ultrafiltered whey protein retentate (lactose-free (max. 0.1% i.d.m.), 40% dry matter, protein content 80% i.d.m., pH: 7.0 to 7.4) are placed, after being pasteurised, in a storage container which is adjusted to a temperature of 30 C. The retentate is stirred constantly. 205 kg of creatine MH (creatine monohydrate) are metered into the container (solid metering). The mixture is stirred vigorously for 30 minutes until a homogeneous, cloudy solution is present. The pH is then checked and optionally adjusted to 7.2 to 7.4 with aqueous NaOH. The cloudy solution thus obtained is passed onto the spray tower via a heat maintenance section (80 C., 70 seconds) and spray dried. The air inlet temperature is 160 C., while a temperature of 75 C. prevails in the spray tower. Approximately 990 kg of a white to light-beige powder are obtained.

b) Characterisation of the Creatine Protein Matrix in Powder Form

[0143] The powder has the following composition: 79 wt. % whey protein concentrate, 18 wt. % creatine, 3 wt. % water.

[0144] Lactose content: <0.1%

[0145] Creatinine content: <0.05%

[0146] Mean particle size: x50 value: 45 m

[0147] Bulk density: 420 g/l

[0148] Calorie content: 1220 kJ/100 g

[0149] Segregation test: CV<5%

Example 7

[0150] As Example 1, but calcium citrate is used instead of tricalcium orthophosphate.