Composition and method for manufacturing clear beverages comprising nanoemulsions with <i>Quillaja saponins</i>

Abstract

A method of making a clear beverage concentrate, which contains a nanoemulsion of a liquid flavour oil in an aqueous phase, including the emulsification of the flavour oil into water in the presence of an emulsifier, which emulsifier consists of at least 5% by weight Quillaja saponins, optionally containing at least one other emulsifier, characterised in that, prior to emulsification, the pH of the aqueous phase is adjusted to 4.0 maximum. The method allows the preparation of beverages that not only are crystal-clear, but which also have substantially more of the full flavour of the original flavour oil.

Claims

1. A method of making a clear beverage concentrate, which comprises a nanoemulsion of a liquid flavor oil in an aqueous phase, comprising: adjusting the pH of the aqueous phase to 4.0 maximum prior to emulsification of the liquid flavor oil into the aqueous phase; and emulsifying the flavor oil into the aqueous phase in the presence of an emulsifier, wherein the emulsifier is at least 5% by weight Quillaja saponins, wherein the weight ratio of the Quillaja saponins to the liquid flavor oil is about 0.1 to about 3.0, wherein the nanoemulsion comprises particles with a hydrodynamic diameter in the range of 100 nm to 122 nm, and optionally containing at least one other emulsifier.

2. The method according to claim 1, in which the pH is adjusted by addition of food-approved acid.

3. The method according to claim 2, wherein the food approved acid is selected from the group consisting of citric acid, malic acid, acetic acid, lactic acid, ascorbic acid, tartaric acid, phosphoric acid and combinations thereof.

4. The method according to claim 1, in which the proportion of Quillaja a saponins in the emulsifier is 25% by weight.

5. A method of making a solid-form clear beverage concentrate, comprising adding a carrier to the concentrate according to claim 1 and spray-drying, the carrier comprising gum Arabic of molecular weight greater than 100 kDa.

6. A solid-form clear beverage concentrate, prepared by the method according to claim 5.

7. The method according to claim 1, in which the proportion of Quillaja saponins in the emulsifier is 50% by weight.

8. The method according to claim 1, in which the proportion of Quillaja saponins in the emulsifier is 75% by weight.

9. The method according to claim 1, in which the proportion of Quillaja saponins in the emulsifier is 100% by weight.

Description

COMPARATIVE EXAMPLE 1

(1) A nanoemulsion (Comparative Example 1) with a composition given in Table 1 was prepared by blending deionised water, propylene glycol, glycerine and sugar syrup until homogeneous. Quillaja extract was added and the blend was again stirred until homogeneous. Under high shear using a Polytron PT6100 system equipped with a PT-DA 3030-6060 dispersing aggregate the Orange flavour base was added to the water phase. High shear blending was continued at 18000 rpm for 5 minutes. The resulting coarse emulsion was processed through an APV60 high pressure homogeniser at 400/50 bars (5600/700 psi) 3 times. The hydrodynamic diameter was determined on a Zetasizer HSA (Malvern Instruments) using the instrument as per the instructions. Values given are averages of three measurements.

(2) pH of the emulsion: 4.8

(3) hydrodynamic diameter after three homogenisation passes: 134 nm

(4) TABLE-US-00001 TABLE 1 Comparative Ingredient Name Example 1 g/kg Deionised water  27.5 Propylene glycol 150.0 Glycerine 99.5% 200.0 Quillaja extract*  50.0 Sugar syrup 65Brix 538.5 Orange flavour base**  34.0 *Q-Naturale ™ 200 (National Starch Food Innovation) **Product code 96584505 (Givaudan)

Examples 1-4

(5) Nanoemulsions were prepared according to the process described for Comparative Example 1 with the only difference that the amount of citric acid given in Table 2 was first dissolved in deionised water before solvents and sugar syrup were added. The amount of acid added is subtracted from the amount of water given in Comparative Example 1. pH values and hydrodynamic diameters are given in Table 2. All hydrodynamic diameters are significantly lower than that in Comparative Example 1 without acid added before homogenisation. The lower the pH, the smaller is the size of the nanoemulsion droplets.

(6) TABLE-US-00002 TABLE 2 Amount of citric acid added Hydrodynamic Example (g/kg emulsion) pH diameter (nm) 1  1.65 3.8 111 2  4.00 3.2 109 3  6.34 2.9 105 4 12.00 2.6 100

Examples 5-12

(7) Nanoemulsions were prepared according to the process described for Comparative Example 1 with the only difference that the amount of organic acids given in Table 3 was first dissolved in deionised water before solvents and sugar syrup were added. The amount of acid added is subtracted from the amount of water given in Comparative Example 1. pH values and hydrodynamic diameters are given in Table 3. All hydrodynamic diameters are significantly lower than that in Comparative Example 1 without acid added before homogenisation. The stronger the acid, the smaller the amount of acid needed to achieve a particular pH.

(8) TABLE-US-00003 TABLE 3 Amount of acid added Hydrodynamic Example Acid used (g/kg emulsion) pH diameter (nm)  5 Ascorbic acid 12.00 3.6 110  6 Tartaric acid  1.65 3.4 112  7 Tartaric acid  4.00 2.9 105  8 Tartaric acid  6.34 2.7 103  9 Malic acid  1.65 3.6 119 10 Malic acid  4.00 3.2 110 11 Malic acid  8.00 3.0 103 12 Malic acid 12.00 2.8 100

Example 13

(9) A nanoemulsion was prepared according to the process described for Comparative Example 1 with the only difference that the amount of phosphoric acid given in Table 4 was first dissolved in deionised water before solvents and sugar syrup were added. The amount of acid added is subtracted from the amount of water given in Comparative Example 1. pH value and hydrodynamic diameter after three passes of high pressure homogenisation are given in Table 4. The hydrodynamic diameter is significantly lower than that in Comparative Example 1 without acid added before homogenisation.

(10) TABLE-US-00004 TABLE 4 Amount of acid added Hydrodynamic Example (g/kg emulsion) pH diameter (nm) 13 1.5 3.0 110

Comparative Examples 2-3 and Examples 14-16

(11) Nanoemulsions comparable to those described above were prepared using a different Orange and a Lemon flavour base. Table 5 displays flavour base, amounts of citric acid added and hydrodynamic diameters after three homogenisaton passes.

(12) TABLE-US-00005 TABLE 5 Amount of Flavour acid added Hydrodynamic Example base (g/kg emulsion) diameter (nm) CE2 Orange* 142 14 Orange* 3.00 (plus 1.50 117 sodium benzoate) 15 Orange* 1.65 118 CE3 Lemon** 148 16 Lemon** 1.65 122 *Product Code 96584506 (Givaudan) **Product Code 96584510 (Givaudan)

Comparative Example 4 and Example 17 (same as Example 1)

(13) A nanoemulsion (Comparative Example 4) was prepared according to the process described for Comparative Example 1. However, amounts of water, solvents and Quillaja extract were changed to allow dissolution of an additional emulsifier (gum arabic) in the water phase before homogenisation. The ratio of Quillaja extract and gum arabic was chosen according to examples disclosed in EP 2359702 to show that the combination with an emulsifying polymer as in EP 2359702 does not work to achieve sufficiently low diameters. For comparison, the compositions of Comparative Example 4 and Example 1 are given in Table 6 together with hydrodynamic diameters measured after one, two and three passes through a high pressure homogeniser. The combination of Quillaja extract and gum arabic results in significantly larger droplet diameters than in Comparative Example 1 (without acid) and in Example 1 (with acid) even in the presence of citric acid. It was further found that after two passes of high pressure homogenization the hydrodynamic diameter is not further reduced.

(14) TABLE-US-00006 TABLE 6 Comparative Example 1 Ingredient Name Example 4 (g/kg) (g/kg) Deionised water  55.20  25.85 Citric acid  1.65  1.65 Gum Arabic*  36.80 Propylene glycol 100.00 150.00 Glycerine 99.5% 193.85 200.00 Quillaja extract**  40.00  50.00 Sugar syrup 65Brix 538.50 538.50 Orange flavour base***  34.00  34.00 Hydrodynamic diameter (nm) After 1 pass 184   147   After 2 passes 163   119   After 3 passes 170   111   *Gum Arabic Instant AA (CNI) **Q-Naturale ™ 200 (National Starch Food Innovation) ***Product Code 96584505 (Givaudan)