Patent Description:
<CIT> granted to Wild GmbH & Co KG discloses a composition with a phycocyanin content of <NUM>,<NUM> w% to <NUM> w% based on the total composition. The Spirulina extract can be stabilized with sucrose and invert sugar. The concentrate can then be mixed with a carrier material, such as dried glucose syrup, and spray-dried. However, no dried glucose syrup formulation is exemplified. Finally, this document does not show any liquid composition comprising Spirulina extract, sucrose, and dried glucose syrup.

<CIT> to Krafts discloses in Example <NUM>, Formula <NUM>, Table <NUM> a pelletized colorant comprising <NUM> Spirulina, <NUM> com syrup and <NUM> sucrose. According to paragraph [<NUM>] th pelletized colorant had a slower dissolution rate than the pelletized colorant formed from Formula <NUM>. Formula <NUM> consists of a com syrup of a dextrose equivalent DE <NUM> in an amount of <NUM>, Spirulina in an amount of <NUM> ad sucrose in an amount of <NUM>. But this document does not disclose a liquid natural blue coloring composition comprising spirulina extract, sucrose and a starch-based compound with a Dextrose Equivalent (DE) between <NUM> and <NUM>, wherein the concentration of the starch-based compound is from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.

<CIT> discloses in Example <NUM> a method for making a chewing gum consisting of <NUM> w% gum base, <NUM> w% sugar,<NUM> w% starch syrup and <NUM> w% phycocyanin composition as well as <NUM> w% flavor. However, this document does not specify which mono or disaccharide is used as a sugar. Further, this document does not describe the Dextrose Equivalent of the starch syrup.

However, the coloring performance and stability are still a challenge. Therefore, there still is a need for stable and heat-resistant natural blue colouring compositions for homogenous coloration of food applications, in particular for confectionary, such as panned confectionary or ice cream.

The inventors surprisingly found that the combination of sucrose and dried glucose syrup stabilizes liquid Spirulina-based coloring compositions and improves the blue coloring of panned confectionary products as compared to trehalose-based Spirulina compositions.

The step order of the manufacturing process unexpectedly improves the coloring performance. Consequently, the present combination of sugars as stabilizers for a Spirulina-based coloring compositions shows improved performance.

Effects as compared to a Spirulina-based coloring composition comprising trehalose, glycerol, trisodium citrate, acetic acid or invert sugar or combinations thereof concern:.

Accordingly, a first aspect of the present invention is a liquid natural blue coloring composition comprising a phycocyanin-containing extract, in particular a Spirulina extract, starch-based compound with a Dextrose Equivalent (DE) between <NUM> and <NUM>, preferably <NUM>, and sucrose.

In one embodiment the natural blue coloring composition consists of the phycocyanin-containing extract, in particular the Spirulina extract, the starch-based compound with a DE between <NUM> and <NUM>, preferably <NUM>, and sucrose.

The natural blue coloring composition is liquid.

In another aspect, the natural blue coloring composition does not comprise any trehalose, trisodium citrate, acetic acid or glycerol or combinations thereof.

In another aspect, the concentration of the phycocyanin-containing extract, in particular the Spirulina extract, is from <NUM> w% to <NUM> w%, preferably from <NUM>,<NUM> w% to <NUM>,<NUM> w%, preferably from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.

In another aspect, the phycocyanin-containing extract, in particular the natural blue coloring composition, has a color strength E10% from <NUM> CU/kg to <NUM> CU/kg, preferably from <NUM> CU/kg to <NUM> CU/kg, even more preferably from <NUM> CU/kg to <NUM> CU/kg as measured by a spectrophotometer Shimadzu UV <NUM> or <NUM> with phosphate buffer pH <NUM>,<NUM>.

In another aspect, the concentration of starch-based compound with a DE between <NUM> and <NUM>, preferably <NUM>, is from <NUM> w% to <NUM> w%, preferably from <NUM>,<NUM> w% to <NUM>,<NUM> w%, preferably from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.

In another aspect, the natural blue coloring composition further comprises antifoaming agents, pH adjuster such as citric acid and/or salts such as sodium chloride.

In another aspect, the pH of the natural blue coloring composition is between <NUM> and <NUM>, preferably between <NUM> and <NUM>.

Another aspect of the present invention is the use of the natural blue coloring composition according to any one of the preceding claims for coloring food products, preferably confectionary products, even more preferably panned confectionary, jelly gum or ice cream.

Another aspect of the present invention is a method for producing the natural blue coloring composition of any one of the preceding claims wherein the step order is:.

In another aspect, the Spirulina extract, the starch-based compound with a DE between <NUM> and <NUM>, preferably <NUM>, and the sucrose are evenly dispersed and dissolved preferably by an overhead stirrer or a powder/liquid mixer involving high-shear mixing.

In another aspect, the temperature is in the case of.

Another aspect of the present invention is a food product, preferably confectionary product, even more preferably a panned confectionary product, jelly gum or ice cream comprising the natural blue coloring composition of any one of the preceding claims or obtained through the process of any one of the preceding claims.

The invention is now described in further detail without, however, limiting its scope.

Phycocyanin-containing extract can be any extract from an organism, preferably microalga, that produces phycocyanin. A preferred phycocyanin-containing extract is Spirulina extract.

Spirulina extract describes an extract of the Spirulina algae, e.g., Spirulina platensis or Arthrospira platensis. This blue-green microalga is known both as a food supplement and as a raw material for food coloring. The pigments mainly found in Spirulina are two blue water-soluble biliproteins, c-phycocyanin and allophycocyanin, grouped under the term phycocyanin, green chlorophylls and yellow xantophylls.

In one embodiment, the Spirulina extract has a color strength E10% from <NUM> CU/kg to <NUM> CU/kg as measured by a spectrophotometer Shimadzu UV <NUM> or <NUM> with phosphate buffer pH <NUM>,<NUM>.

In one embodiment, the concentration of the Spirulina extract is from <NUM> w% to <NUM> w%, preferably from <NUM>,<NUM> w% to <NUM>,<NUM> w%, preferably from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.

In one embodiment, the natural blue coloring composition has a color strength E10% from <NUM> CU/kg to <NUM> CU/kg, preferably from <NUM> CU/kg to <NUM> CU/kg, even more preferably from <NUM> CU/kg to <NUM> CU/kg as measured by a spectrophotometer Shimadzu UV <NUM> or <NUM> with phosphate buffer pH <NUM>,<NUM>.

In one embodiment, the color strength is measured with a spectrophotometer Shimadzu UV <NUM> or <NUM>. The sample preparation is made with phosphate buffer pH <NUM>,<NUM>.

Preferably, the phosphate buffer is prepared as follows:.

Preferably, the sample preparation is prepared as follows:.

The Color Units (CU) (corresponding to E10% <NUM> at maximal absorbance wavelength) are calculated using the following formula:.

In one embodiment, measurements are performed in transmission mode with a spectrocolorimeter Datacolor <NUM> or <NUM> (illuminant D65/<NUM>°, include mode). The sample is poured into a <NUM> quartz cell placed in the position closest to the detector. The sample is diluted with phosphate buffer pH <NUM>,<NUM> (same preparation as for color strength) in order to reach a lightness comprised between <NUM>,<NUM> and <NUM>,<NUM>. Once the correct lightness is obtained, the chroma and hue of the sample are recorded.

Preferably, the natural blue coloring composition has a color strength comprised between <NUM> to <NUM> CU/kg.

Preferably, at L70, the chroma (C*) is between <NUM> - <NUM>, preferably between <NUM> and <NUM>.

Preferably at L70, and a chroma (C*) is between <NUM> - <NUM>, preferably between <NUM> and <NUM> and the hue (h*) is between <NUM> - <NUM>.

In one embodiment, the stability is minimum <NUM> months in frozen conditions (<-<NUM>).

In one embodiment, the stability is minimum <NUM> months in cold conditions (<NUM> - <NUM>).

In one embodiment, the stability is assessed by measuring the color strength, the LCh parameters, as well as the Brix, pH and water activity (direct reading).

In one embodiment, the high content of sugar allows the water activity to stay below <NUM>,<NUM> in order to protect the product against micro-organisms.

In the absence of a salt, the concentration of sucrose is from <NUM> w% to <NUM> w%, preferably from <NUM> w% to <NUM> w%, preferably from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.

In the presence of a salt, the concentration of sucrose is from <NUM> w% to <NUM> w%, preferably from <NUM> w% to <NUM> w%, preferably from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.

The starch-based compound with a DE between <NUM> and <NUM>, preferably <NUM>, preferably is dried glucose syrup or maltodextrin.

The concentration of starch-based compound with a DE between <NUM> and <NUM>, is from <NUM> w% to <NUM> w%, preferably from <NUM>,<NUM> w% to <NUM>,<NUM> w%, preferably from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.

In one embodiment, the starch-based compound is a dried glucose syrup having a DE comprised between <NUM> and <NUM>, preferably a DE of <NUM>.

In one embodiment, the starch-based compound is a maltodextrin having a DE comprised between <NUM> and <NUM>.

The natural blue coloring composition may be used for coloring food products, preferably confectionary products, even more preferably panned confectionary, jelly gum or ice cream, water ice.

In one embodiment, the pH of the natural blue coloring composition is between <NUM> and <NUM>, preferably between <NUM> and <NUM>. The pH is preferably measured directly in the liquid.

the Method for producing the liquid natural blue coloring composition comprising the phycocyanin-containing extract, in particular the Spirulina extract, dried glucose syrup and sucrose is obtained by a method, wherein the step order is:.

The agitation is preferably performed until the phycocyanin-containing extract, in particular the Spirulina extract, the starch-based compound with a DE between <NUM> and <NUM>, preferably <NUM>, and the sucrose are evenly dispersed and dissolved, preferably by an overhead stirrer or a powder/liquid mixer involving high-shear mixing.

Furthermore, confectionary ingredients need to be heat stable, as they are usually heated or cooked. The coloring performance of the natural blue coloring compositions are surprisingly similar to those of confectionary after heat treatment.

Liquid: the natural blue coloring composition is a liquid.

The natural blue coloring composition may further comprise other ingredients, such as antifoaming agents, pH adjuster such as citric acid and/or salts such as sodium chloride.

The skilled person can choose the quantity of the further ingredients of the natural blue coloring composition of the present invention so that they add up to <NUM> w%.

The natural blue coloring composition may further comprise other pigments, such as yellow or red pigments to produce for example green or violet color shades.

The following examples illustrate the natural blue coloring compositions.

Following natural blue coloring compositions were tested:.

Several challenge tests were conducted on exemplary natural blue coloring compositions comprising Spirulina extract, dried glucose syrup and sucrose to prove the resistance of the formulation to microbial growth in case of contamination.

A challenge test is a study where the microbiological stability is investigated at <NUM>, <NUM> and <NUM> by adding potential spoilage organisms to the product at levels somewhat over the acceptable limit (ca. <NUM>,<NUM>-<NUM>,<NUM> x <NUM><NUM> cfu/g). Then the survival/growth of the micro-organisms is monitored over time. A negative control (without added micro-organisms) is also monitored at <NUM>.

<FIG> shows the microbiological stability over <NUM> weeks of an exemplary natural blue coloring composition consisting of <NUM>% spirulina extract, <NUM>% dried glucose syrup DE <NUM>, <NUM>% sucrose, <NUM>% antifoam and <NUM>% citric acid diluted in water.

<FIG> shows the microbiological stability in respect of yeast and mold at three different temperatures: <NUM>, <NUM> and <NUM>.

<FIG> shows the microbiological stability over <NUM> weeks of an exemplary natural blue coloring composition consisting of <NUM>% spirulina extract, <NUM>% dried glucose syrup DE <NUM>, <NUM>% sucrose, <NUM>% antifoam and <NUM>% citric acid diluted in water. <FIG> shows the microbiological stability in respect of yeast and mold at three different temperatures: <NUM>, <NUM> and <NUM>.

<FIG> shows the microbiological stability over <NUM> weeks of a comparative blue coloring composition comprising trehalose, trisodium citrate and invert sugar.

The results show a satisfactory stability of the formulation at <NUM> because the cell count for yeast and mold is either stable or decreasing. The results at <NUM> and <NUM> show that the formulation is very sensitive to the storage temperature and should be kept below <NUM> for microbiological safety.

These results are similar to what is observed with a standard Spirulina liquid formulation containing trehalose, trisodium citrate and invert sugar (cf. <FIG> below). The yeast and mold levels at <NUM> remain stable throughout the <NUM> weeks of the challenge test.

Hard panning was carried out following the recipe and procedure below:.

The panning process comprised the following steps:.

The natural blue coloring composition comprising Spirulina extract, dried glucose syrup and sucrose shows excellent panning performance due to the sugar combination used (sucrose and dried glucose syrup, no trehalose, no invert sugar).

<FIG> show a comparison in panning of a natural blue coloring composition composed of <NUM>% Spirulina extract, <NUM>% dried glucose syrup DE <NUM>, <NUM>% sucrose, <NUM>% antifoam and <NUM>% citric acid diluted in water (sample B). The comparative example is also a liquid formulation containing Spirulina, trehalose, trisodium citrate and invert sugar, with a similar color strength (sample A).

The dragees panned with the formulation of the invention showed an even and smooth surface as shown in <FIG>. The color was evenly spread on the surface on the dragée. The comparative example (<FIG>) shows a washed-off surface, which is indicated through an inhomogeneous color on the dragees.

The good covering abilities are confirmed by a roll-out test performed with the roll-out stick shown in <FIG>, where the difference in color appearance is clearly seen: the reference shows an inhomogeneous appearance contrary to the new formulation.

Both the panning syrup roll out as well as the panned dragees clearly show that the natural blue coloring composition comprising Spirulina extract, dried glucose syrup and sucrose has superior panning behavior. It results in an evenly distribution of the color and almost no white spots on the surface in comparison to a standard Spirulina formulation.

<FIG> shows the panning results of Example <NUM>: the natural blue coloring composition of the invention comprising Spirulina extract, dried glucose syrup and sucrose is shown in <FIG> with a homogenous color appearance. The comparative liquid Spirulina formulation comprising trehalose, Spirulina extract, trisodium citrate and invert sugar is shown in <FIG>.

<FIG> shows a roll out comparison of the coloring abilities of Example <NUM>. The natural blue coloring composition of the invention comprising Spirulina extract, dried glucose syrup and sucrose is shown in <FIG> with a homogenous appearance resulting in an evenly distribution of the color and almost no white spots on the surface. The comparative liquid Spirulina formulation comprising trehalose, Spirulina extract, trehalose, trisodium citrate and invert sugar is shown in <FIG>. The comparative example shows an inhomogeneous appearance.

Both the panning syrup roll out as well as the panned dragees clearly show that the present Spirulina formulation has superior panning behavior (resulting in an evenly distribution of the color and almost no white spots on the surface) in comparison to the comparative example comprising trehalose, Spirulina extract, trisodium citrate and invert sugar.

Jelly gum trials were carried out following the recipe and procedure below:.

The jelly gums are stored at <NUM>-<NUM> in zipper bags.

Two parameters are critical for a color used in jelly: stability towards acid and stability towards heat. The tests are performed against a comparative liquid Spirulina containing trehalose, an ingredient known for its stabilizing properties.

Nevertheless, the present natural blue coloring composition comprising Spirulina extract, dried glucose syrup, sucrose without trehalose performed almost as good as the reference in acid test (see <FIG>).

In light stability test, our formulation proved just as stable as the reference (see <FIG>).

Procedure for heat-acid stability test of Spirulina in jelly gum (see also <FIG>):.

<FIG> shows a comparison of the coloring performance of Example <NUM> in jelly. The natural blue coloring composition of the invention comprising Spirulina extract, dried glucose syrup and sucrose is shown in in the top row of <FIG>. The comparative liquid Spirulina formulation comprising Spirulina extract, trehalose, trisodium citrate and invert sugar is shown in bottom row of <FIG>. Column A shows the performance of the colouring compositions without acid. Column B shows the performance of the colouring compositions with added acid. Column C shows the performance of the colouring compositions after <NUM> minutes of heat treatment at <NUM>. Column D shows the performance of the coloring compositions after <NUM> minutes of heat treatment at <NUM>. Column E shows the performance of the coloring compositions after <NUM> minutes of heat treatment at <NUM>.

In addition, the light stability of the compositions of example <NUM> is tested in jelly gum. An accelerated light stability test under the following conditions is used: Atlas Suntester XLS+, Xenon lamp 480W/m2, <NUM>, window glass filter. The evaluation is done both visually and with color measurement after <NUM>, <NUM>, <NUM>, <NUM> and <NUM> hours. The results are shown in <FIG>. Column A of <FIG> represents the comparative example, a liquid coloring composition comprising Spirulina extract, trehalose, trisodium citrate and invert sugar in jelly. Column B of <FIG> shows the coloring performance of the inventive natural blue coloring composition comprising Spirulina extract, dried glucose syrup, and sucrose in jelly. The new natural blue coloring composition has a comparable light stability than the standard sample.

Salt, such as sodium chloride, can be added to the formulation in order to reduce the sucrose content. The concentration of salt is from <NUM> w% to <NUM> w%, preferably from <NUM> w% to <NUM> w%.

A natural blue coloring composition is prepared with <NUM> w% Spirulina extract, <NUM> w% dried glucose syrup, <NUM> w% sucrose, <NUM> w% sodium chloride, <NUM> w% antifoam and <NUM> w% citric acid diluted in water.

Claim 1:
A liquid natural blue coloring composition comprising a phycocyanin-containing extract, in particular a Spirulina extract, further comprising:
▪ a starch-based compound with a Dextrose Equivalent (DE) between <NUM> and <NUM>, preferably <NUM>; and
▪ sucrose;
wherein the natural blue coloring composition is obtainable by a process wherein
the step order is:
<NUM>) Adding the phycocyanin-containing extract, in particular the Spirulina extract, to an aqueous solution, preferably water, under agitation to obtain a first solution;
<NUM>) Adding the starch-based compound with a DE between <NUM> and <NUM>, preferably <NUM>, under agitation to obtain a second solution; and
<NUM>) Adding sucrose under agitation to obtain the natural blue coloring composition.
wherein the concentration of the starch-based compound is from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition; and
wherein the concentration of sucrose is
▪ In the absence of a salt, from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition; or
▪ In the presence of a salt, from <NUM> w% to <NUM> w% as compared to the total weight of the natural blue coloring composition.