ACID STABLE BEVERAGES COMPRISING BIXIN

Abstract

The present invention is directed to an acid-stable bixin form, wherein the bixin is microencapsulated in a matrix of a hydrocolloid, preferably in a matrix of modified food starch. This bixin form can be in the form of an emulsion, a suspension or in form of a powder. The present invention is further directed to a process for the manufacture of such forms, as well as to beverages containing them. These yellow-orange to red-orange beverages are physically stable and color stable.

Claims

1.-19. (canceled)

20. A beverage comprising a bixin form, wherein the bixin in the bixin form is microencapsulated in a matrix of a hydrocolloid, characterized in that the beverage is physically stable at a pH in the range of from 2 to 5, preferably at a pH in the range of from 2.5 to 4, more preferably at a pH in the range of from 2.8 to 3.6, for a period of time of at least 3 months, preferably for a period of time of at least 6 months.

21. The beverage according to claim 20, wherein the beverage is color stable.

22. The beverage according to claim 20, wherein the hydrocolloid is at least one modified food starch so that the bixin in the bixin form is microencapsulated in a matrix of at least one modified food starch, and/or wherein the matrix further comprises a saccharide.

23. The beverage according to claim 20, wherein the bixin form upon re-dispersion in water provides a yellow-orange to red-orange color hue at high color strength characterized by an E1/1 value of at least 400, preferably an E1/1 value in the range of from 500 to 1800.

24. The beverage according to claim 20, wherein the amount of bixin in the beverage is in the range of from 1 ppm to 50 ppm, preferably in the range of from 2 to 30 ppm, more preferably in the range of from 3 to 25 ppm, based on the total weight of the beverage.

25. The beverage according to claim 20, wherein the beverage is selected from the group consisting of soft drinks, flavored waters, fortified waters, sports drinks, mineral drinks, carbonated beverages, fruit juices, fruit-juice containing soft drinks, fruit punches, alcoholic beverages, sugar-containing beverages and diet beverages.

26. A bixin form, wherein the bixin is microencapsulated in a matrix of a hydrocolloid.

27. The bixin form according to claim 26, wherein the bixin form upon re-dispersion in water provides a yellow-orange to red-orange color hue at high color strength characterized by an E1/1 value of at least 400, preferably an E1/1 value in the range of from 500 to 1800.

28. The bixin form according to claim 26, wherein the average particle size of the inner phase of the bixin form measured by Photon Correlation Spectroscopy (Beckman Coulter N4 Plus Submicron Particle Sizer) is in the range of from 100 to 400 nm.

29. The bixin form according to claim 26 being a powder or a dispersion.

30. The bixin form according to claim 26, wherein the bixin is microencapsulated in a matrix of at least one modified food starch, and/or wherein the matrix further comprises a saccharide.

31. The bixin form according to claim 26, wherein the bixin is microencapsulated in a matrix which does not comprise conjugates of plant gums and modified food starch, and/or wherein the bixin is microencapsulated in a matrix which does not comprise octenyl-succinic anhydride-modified gum Acacia, and/or wherein the bixin is microencapsulated in a matrix which does not comprise beet pectin, chicory pectin, Jerusalem artichoke pectin or other pectin types having a high degree of acetylation.

32. A process for the manufacture of a bixin dispersion or a bixin powder according to claim 29 comprising the following steps: a) forming a solution of the bixin in an organic solvent, optionally adding a fat-soluble antioxidant and/or optionally adding an oil and/or optionally adding middle-chain triglycerides; b) providing a matrix of modified food starch and optionally a saccharide and/or a water-soluble antioxidant in water; c) emulsifying the solution obtained in step a) into the matrix obtained in step b) to obtain a dispersion; d) removing the organic solvent from the dispersion obtained in step c) to obtain a bixin dispersion; e) optionally drying the bixin dispersion obtained in step d) to obtain a bixin powder.

33. Use of a bixin form, wherein the bixin is microencapsulated in a matrix of a hydrocolloid, and whereby preferably the average particle size of the inner phase of the bixin form measured by Photon Correlation Spectroscopy (Beckman Coulter N4 Plus Submicron Particle Sizer) is in the range of from 100 to 400 nm, for coloring beverages.

34. The use according to claim 33, wherein the bixin in the bixin form is microencapsulated in a matrix of modified food starch, and wherein the matrix optionally further comprises a saccharide.

Description

EXAMPLES

Examples 1-7: Manufacture of Powders According to the Present Invention

[0117] The examples were carried out according to the following general procedure with the amounts of compounds (bixin, middle-chain triglycerides, modified food starch, saccharide, antioxidants, water) and the process parameters as given in detail in Table 1. As solvent an organic solvent selected from the group consisting of dimethyl carbonate, ethyl formate, ethyl acetate, isopropyl acetate, methyl tert-butyl ether and methylene chloride was used. The amount of the solvent and the dissolution temperature were chosen so as to dissolve the bixin and the fat-soluble antioxidant and the MCT, if present, completely.

[0118] The bixin used was the commercially available AlcabixP (from AICA-Color, Peru).

[0119] General Procedure

[0120] Bixin, the fat-soluble antioxidant and the middle-chain triglycerides (MCTs) (amounts as given in Table 1) are dispersed in an organic solvent as mentioned above. The resulting suspension is then heated up to a temperature as given in Table 1 to dissolve the whole amount of bixin. The resulting solution is then held at the temperature as given in Table 1 in a holding vessel.

[0121] The matrix phase consisting of the modified food starch (=OSA starch), the saccharide and the water-soluble antioxidant as given in Table 1 is dissolved in the amount of water as given in Table 1 at the temperature as given in Table 1.

[0122] The emulsification process consists of two steps and is carried out under pressure.

[0123] Both phases are continuously fed to a rotor stator device where the solution is emulsified into the matrix phase. The rotation speed is 5000 rpm (revolutions per minute) and the mixing temperature is as given in Table 1. The next step entails a second micronisation step and consists of a sapphire orifice. The orifice diameter is as given in Table 1 and the applied pressure drop over the orifice is as given in Table 1 at the temperature as given in Table 1.

[0124] Then the organic solvent is removed from the emulsion by using a thin film evaporator cascade. After that the solvent-free emulsion is sprayed into a fluidized corn starch bed where the particles are dried.

[0125] The results of the examples are summarized below. The average particle size of the inner phase was measured by Photon Correlation Spectroscopy (Beckman Coulter N4 Plus Submicron Particle Sizer).

[0126] The color intensity E1/1 is the absorbance of a 1% solution and a thickness of 1 cm and is calculated as follows: E1/1=(AmaxA650)*dilution factor/(weight of sample*content of product form in %).

[0127] (AmaxA650) means the value you get when you subtract the Adsorption value measured at 650 nm (A650) wavelength from the value (Amax) that was measured at the maximum Adsorption in the UV-Spectrophotometer.

[0128] * means multiplied with.

[0129] dilution factor=the factor by which the solution has been diluted.

[0130] weight of sample=the amount/weight of the formulation that was used in [g]

[0131] content of product form in %=the amount of bixin in the powder in % (detected via UV spectrophotometer) which is in the range of from 4.5 to 9.7% in the following examples.

Example 1

[0132] The final product has a bixin content of 4.5%, E1/1=1355 and a particle size of the inner phase of 226 nm.

Example 2

[0133] The final product has a bixin content of 9.0%, E1/1=710 and a particle size of the inner phase of 306 nm.

Example 3

[0134] The final product has a bixin content of 7.1%, E1/1=992 and a particle size of the inner phase of 282 nm.

Example 4

[0135] The final product has a bixin content of 9.7%, E1/1=621, a particle size of the inner phase of 352 nm and a turbidity of 196 NTU (measured in a pasteurized soft drink (6 ppm) as prepared according to the instruction below). Such turbidity adds to the juicy appearance of a fruit juice when added to it and is in this application advantageous.

Example 5

[0136] The final product has a bixin content of 5.1%, E1/1=1057, a particle size of the inner phase of 307 nm and a turbidity of 160 NTU (measured in a pasteurized soft drink (6 ppm) as prepared according to the instruction below).

Example 6

[0137] The final product has a bixin content of 4.8%, E1/1=1035, a particle size of the inner phase of 378 nm and a turbidity of 157 NTU (measured in a pasteurized soft drink (6 ppm) as prepared according to the instruction below).

Example 7

[0138] The final product has a bixin content of 5.6%, E1/1=834, a particle size of the inner phase of 331 nm and a turbidity of 209 NTU (measured in a pasteurized soft drink (6 ppm) as prepared according to the instruction below).

[0139] Application Trials with the Powders According to Examples 1-7

[0140] The powders according to examples 1-7 have been applied in soft drinks with a concentration of the bixin of 6 ppm. The objective of these trials was to evaluate the performance of these samples for their application in beverages. The powders have to provide a good color stability, good chemical stability and a good performance of appearance (no or less ringing, absence of or only few particles on the surface and (almost) no sedimentation).

[0141] Preparation of the Soft Drinks

[0142] The soft drinks had the following composition:

TABLE-US-00001 Ingredient Amount of ingredient 1 Potassium sorbate 0.2 g 2 Sugar syrup (64 Brix) 156.2 g Ascorbic acid 0.2 g Aqueous 50-weight-% 5.0 g citric acid Apricot flavor (water- 0.2 g soluble, Givaudan 78848-56) Pectin solution 2-weight-% 10 g Stock solution* 6 g (i.e. 6 ppm) 3 Water Filled up so that a total amount of the soft drink of 1000 ml results Total amount 1000 ml *From each powder according to examples 1 to 7 a stock solution was prepared, whereby the powder was diluted with water so that the stock solution had a concentration of the bixin of 0.1 weight-% (= 1000 ppm).

[0143] The soft drinks were prepared as follows:

[0144] Potassium sorbate 1) was dissolved in water, the other ingredients 2) were added one after the other while the mixture was gently stirred. Then the resulting soft drink syrup was diluted with drink water in such an amount to result in 1000 ml of the soft drink. The pH of the soft drinks was in the range of from 2.8 to 3.6.

[0145] The soft drinks were then filled in glass bottles and the bottles sealed with a metallic cap. Some of these bottles were pasteurized and some not. A tunnel pasteurizer from Miele was used for pasteurization with a holding temperature of 80 C. for 1 minute at a core of the bottle.

[0146] The bottles were stored at room temperature (temperature in the range of 18 to 27 C.) and under light exposure 12 hours per day with 800 Lux. Color measurements were performed directly after beverage preparation (time=0), as well as after a storage time of 2 weeks, 30 days, 60 days and 90 days.

[0147] Color Measurements

[0148] Color measurements for the application in food are performed with a colorimeter (Hunter Lab Ultra Scan Pro) which can other than a spectrophotometer express color values according to the psychophysical perception of color by human eye.

[0149] Color measurements are carried out after CIE guidelines (Commission International d'Eclairage). Values can be expressed either as planar coordinates L*a*b* with L* being the measuring value for lightness, with a*being the value on the red-green-axis and with b* being the value on the yellow-blue-axis.

[0150] Instrument settings: [0151] Color scale: CIE L*a*b*/L*C*h* [0152] Light source definition: D65 daylight equivalent [0153] Geometry: Diffuse/8 [0154] Wavelengths: scan 350 to 1050 nm in 5 nm optical resolution [0155] Sample measurement area diameter: 19 mm (large) [0156] Calibration mode: Transmission/white tile

[0157] The Chroma (C*) sometimes called saturation describes the vividness or dullness of a color which can be calculated as followed:

C*=(a*.sup.2+b*.sup.2)

[0158] The angle called hue (h) describes how we perceive an object's color and can be calculated as followed:

h=tan(b/a).sup.(1)

[0159] The color difference DE* is calculated using the following equation:

DE*={square root over ((L*).sup.2+(a*).sup.2+(b*).sup.2)}

[0160] whereby L=lightness, a=red value, and b=yellow value

[0161] L*=L.sub.x*L.sub.0*; 0=initial value; x=time of measuring

[0162] a*=a.sub.x*a.sub.0*; 0=initial value; x=time of measuring

[0163] b*=b.sub.x*b.sub.0*; 0=initial value; x=time of measuring

[0164] For a good color stability, DE* should be lower than 10 (DE*<10); this means that the color difference is acceptable and at DE*<3 cannot be seen by naked eyes, i.e. without the use of an apparatus such as a colorimeter.

[0165] Physical stability is measured by human eye according to an evaluation matrix. Parameter recorded for soft drink beverages are: [0166] Ring formation/Neck ring in bottles in score 6 to 1 with 6 representing no ring, and 1 representing very strong ring. [0167] Surface particles in score 6 to 1 with 6 representing no particles/no covering and 1 representing more than half of surface covered with particles/more than two third of surface covered with film other than particles. [0168] Sediment on the bottom of packaging as fine film, individual particles or ring-formation in score 6 to 1 with 6 representing either no particles, no film or no ring and 1 representing either more than half of bottom covered with particles, bottom covered with strong film or very strong ring visible.

[0169] Turbidity Measurements

[0170] Suspended solids (or particles) are responsible for the turbid appearance of beverages containing juice. This turbid appearance can be evaluated by turbidity measurements. Turbidity depends on the light-scattering properties of such particles: their size, their shape and their refractive index.

[0171] In this work turbidity measurements were conducted using a Turbidimeter (Hach 2100N IS, USA) and turbidity values were given in NTU (nephelometric turbidity units). Neophelometer measures the light scattered by a sample in 90 from the incident light path (s. FIG. 1).

[0172] FIG. 1 illustrates the principle of the nephelometric turbidity measurement Instrument settings: Light source: 86010 nm LED

[0173] Results Concerning the Soft Drinks Containing Bixin (Powders According to Examples 1-7)

[0174] a) Color Difference

[0175] The results concerning the measurement of the color difference during storage are shown in FIGS. 2 and 3.

[0176] FIG. 2 shows the color difference (DE*) in non-pasteurized soft drinks during a storage time of up to 3 months.

[0177] x-axis: Storage time in days; y-axis: Color difference (DE*) (dimensionless);

[0178] =soft drink containing a powder according to example 4;

[0179] x=soft drink containing a powder according to example 6;

[0180] .circle-solid.=soft drink containing a powder according to example 7.

[0181] All samples showed acceptable (DE*10) and similar color stability.

[0182] FIG. 3 shows the color difference (DE*) in pasteurized soft drinks during a storage time of up to 3 months.

[0183] x-axis: Storage time in days; y-axis: Color difference (DE*) (dimensionless);

[0184] =soft drink containing a powder according to example 4;

[0185] x=soft drink containing a powder according to example 6;

[0186] .circle-solid.=soft drink containing a powder according to example 7.

[0187] All samples showed very good (DE*<10) and similar color stability.

[0188] FIG. 4 shows the chemical stability (% recovery) in pasteurized soft drinks during a storage time of up to 3 months.

[0189] x-axis: Storage time in days; y-axis: Chemical stability (% recovery) CS (dimensionless),

[0190] =soft drink containing a powder according to example 4;

[0191] x=soft drink containing a powder according to example 6;

[0192] .circle-solid.=soft drink containing a powder according to example 7.

[0193] All samples showed good chemical stability (% recovery <15).

[0194] c) Physical Appearance

[0195] After 3 months of storage the non-pasteurized and pasteurized soft drinks were evaluated visually concerning their physical appearance. Hereby the samples were examined visually whether they show a ring in the bottle neck, whether they show particles on the surface and whether they show white sediments. The following schedule of notes was applied:

[0196] Ring in Bottle Neck:

[0197] 6=no ring

[0198] 5=hardly noticeable ring

[0199] 4=recognizable ring

[0200] 3=clear fine ring recognizable

[0201] 2=strong ring recognizable

[0202] 1=broad ring recognizable

[0203] Particles on Surface:

[0204] 6=no particles

[0205] 5=1 to 10 particles

[0206] 4=more than 10 particles

[0207] 3=not countable anymore

[0208] 2=half of the surface covered

[0209] 1=more than half of the surface covered

[0210] Sediment:

[0211] 6=no sediment

[0212] 5=slight matt glimmer

[0213] 4=fine matt sediment

[0214] 3=matt sediment

[0215] 2=strong matt sediment

[0216] 1=very strong matt sediment

[0217] For a good performance, scores should be 3.

[0218] Tab. 2 shows the results obtained for the appearance evaluation of a non-pasteurized soft drink.

TABLE-US-00002 Soft drink containing a powder according to Ring in bottle Particles on the example neck surface White sediment 4 4 6 4

[0219] The sample showed a very good performance with respect to its appearance attributes.

[0220] Tab. 3 shows the results obtained for the appearance evaluation of a pasteurized soft drink.

TABLE-US-00003 Soft drink containing a powder according to Ring in bottle Particles on the example neck surface White sediment 4 4 6 5

[0221] Also in pasteurized drinks, the sample showed a very good performance with respect to its appearance attributes.

Comparison Example

[0222] The commercial available product CapColor A-8-WSS-145 from Christian Hansen, Denmark, was further analyzed. It is a dark reddish brown liquid or gel, produced by extraction of annatto pigments from the seeds of the annatto tree (Bixa Orellana L.). The pigments are dispersed in an aqueous solution of vegetable hydrocolloid (Gum Arabic). CapColor A-8-WSS-145 comprises 7.5 to 8.5% of bixin as major coloring principle.

[0223] The E1/1 corrected in water is only 226 (430 nm) and therefore, much lower than the E1/1 of the bixin forms according to the present invention.

TABLE-US-00004 TABLE 1 Example 1 2 3 4 5 6 7 Amount of bixin [g] 62 60 60 62 48 56 54 Fat-soluble Antioxidant D D D D D D D Amount of fat-soluble 9 8 9 9 2.6 3 4.3 antioxidant [g] Amount of MCT [g] 28 27 4.5 12.8 15 21.4 Modified food starch H H H H H/Q C/P C/P Amount of modified 218 231 211 218 189/11.3 113/110 127/56.3 food starch [g] Saccharide and amount 21 g of 21 g of 5.3 g of dextrose 4 g of dextrose 32.8 g of maltodextrin maltodextrin monohydrate + monohydrate + sucrose + (DE2023) (DE2023) 24.7 g of 8 g of 23.4 g of maltodextrin maltodextrin maltodextrin (DE2023) (DE2023) (DE2023) Water-soluble antioxidant none none none none S S none Amount of water-soluble 5.3 3 antioxidant [g] Amount of water [g] 720 693 696 720 946 913 718 Temperature at which the 65 C. 65 C. 67 C. 64 C. 50 C. 50 C. 50 C. hydrocolloid matrix is prepared Temperature to which the 105 C. 112 C. 116 C. 113 C. 106 C. 104 C. 106 C. suspension is heated up Temperature at which the 120 C. 117 C. 116 C. 120 C. 110 C. 108 C. 114 C. solution is held Mixing temperature 68 C. 66 C. 77 C. 66 C. 71 C. 71 C. 90 C. Orifice diameter [.sup.m] 170 230 230 230 170 170 200 Applied pressure drop at 215 bar 56 bar 64 bar 48 bar 188 bar 180 bar 175 bar temperature given at 68 C. at 66 C. at 69 C. at 66 C. at 66 C. at 70 C. at 75 C. In this table D = dl--tocopherol; H = HiCap 100; Q = Q-Naturale 200 (Quillaja - a mixture of triterpenic saponins, commercially e.g. provided by Desert King International, San Diego, US); C = ClearGum Co03 (an OSA starch); P = Purity Gum Ultra (an OSA starch); MCT = middle chain triglycerides (commercially available as Bergabest 60/40); S = Sodium ascorbate.