SPRAY DRYING

Abstract

A method of preparing spray-dried flavor-containing particles, comprising the addition of flavor to an aqueous, sugar-free matrix and spray-drying the resulting blend, the matrix comprising an emulsifier, a film former and at least one metal salt, selected from the ferrous, alkali metal and alkaline earth metal salts of citric, gluconic and tartaric acids. The method allows the preparation of highly-stable, oxidation- and moisture resistant flavor particles.

Claims

1. A method of preparing spray-dried flavor-containing particles, comprising adding flavor to an aqueous, sugar-free matrix to form a blend and spray-drying the resulting blend, the matrix comprising an emulsifier, a film former and at least one metal salt, selected from the ferrous, alkali metal and alkaline earth metal salts of citric, gluconic and tartaric acids.

2. The method according to claim 1, in which the salt is selected from potassium gluconate, tripotassium citrate, potassium bitartrate, sodium gluconate, magnesium gluconate and ferrous gluconate.

3. The method according to claim 1, in which the at least one salt is present at a concentration of from 10-30% by weight of the non-flavor particle constituents.

4. The method according to claim 3, in which the weight proportions of individual salts are selected as follows: Potassium Gluconate 20-30%, Magnesium Gluconate 25%, Ferrous Gluconate 25%, Potassium Bitartarate 25%, Tripotassium Citrate 10-25%, or Magnesium Citrate 20-30%.

5. The method according to claim 1, in which more than one metal salt is used.

6. The method according to claim 5, in which the more than one salt is selected from one of the following combinations: tripotassium citrate and potassium gluconate, tripotassium citrate and potassium bitartrate, or potassium gluconate, tripotassium citrate and potassium bitartrate.

7. The method according to claim 6, in which the following weight proportions of salt are used: Potassium Gluconate & Tripotassium Citrate (1:2) at 30%, Potassium Gluconate & Magnesium Citrate (1:2) at 30%, Potassium Gluconate & Tripotassium Citrate (1:1) at 20%, Potassium Bitartarate & Tripotassium Citrate (1:1) at 20%, or Potassium Gluconate, Potassium Bitartarate & Tripotassium Citrate (1:1:1) at 30%.

8. The method according to claim 1, in which flavor is present at a proportion of up to 15% by weight of the particle.

9. The method according to claim 1, in which the matrix comprises from 10-90% by weight of the particle.

10. A spray-dried, flavor-containing particle comprising flavor in a sugar-free matrix, the matrix comprising an emulsifier, a film former and at least one metal salt, selected from the ferrous, alkali metal and alkaline earth metal salts of citric, gluconic and tartaric acids.

11. The spray-dried, flavor-containing particle according to claim 10, in which the flavor content is up to 15% by weight of the particle.

12. The spray-dried, flavor-containing particle according to claim 10, in which the matrix comprises from 10-90% by weight of the particle.

13. The spray-dried, flavor-containing particle according to claim 10, in which the salt is selected from potassium gluconate, tripotassium citrate, potassium bitartrate, sodium gluconate, magnesium gluconate and ferrous gluconate.

14. The spray-dried, flavor-containing particle according to claim 10, in which the at least one salt is present at a concentration of from 10-30% by weight of the non-flavor particle constituents.

15. The spray-dried, flavor-containing particle according to claim 14, in which the weight proportions of individual salts are selected as follows: Potassium Gluconate 20-30%, Magnesium Gluconate 25%, Ferrous Gluconate 25%, Potassium Bitartarate 25%, Tripotassium Citrate 10-25%, or Magnesium Citrate 20-30%.

16. The spray-dried, flavor-containing particle according to claim 10, in which more than one metal salt is present.

17. The spray-dried, flavor-containing particle according to claim 16, in which the more than one salt is selected from one of the following combinations: tripotassium citrate and potassium gluconate, tripotassium citrate and potassium bitartrate, or potassium gluconate, tripotassium citrate and potassium bitartrate.

18. The spray-dried, flavor-containing particle according to claim 17, in which the following weight proportions of salt are used: Potassium Gluconate & Tripotassium Citrate (1:2) at 30%, Potassium Gluconate & Magnesium Citrate (1:2) at 30%, Potassium Gluconate & Tripotassium Citrate (1:1) at 20%, Potassium Bitartarate & Tripotassium Citrate (1:1) at 20%, or Potassium Gluconate, Potassium Bitartarate & Tripotassium Citrate (1:1:1) at 30%.

Description

EXAMPLE 1

Preparation of Test Matrix

[0033] A test matrix was prepared by blending Capsul 1450, a sodium octenyl succinate-modified starch, and 25 DE maltodextrin in the weight proportion of 10:90. This is used as a control. When salts were added, the proportion of maltodextrin is reduced by the proportion of salt added. The salts are shown in table 1.

TABLE-US-00001 TABLE 1 Overview of salt samples Sample No. Salt/Level 1 Tripotassium Citrate 25%, Sugar 25% 2 Tripotassium Citrate 20% 3 Tripotassium Citrate 20% & Potassium Gluconate 10% 4 Magnesium Citrate 10%, Mannitol 20% 5 Magnesium Citrate 20% & Potassium Gluconate 10% 6 Potassium Gluconate 25% 7 Magnesium Gluconate 25% 8 Ferrous Gluconate 25% 9 Tripotassium Citrate 25% 10 Magnesium Citrate 25% 11 Calcium Citrate 25% 12 Calcium Magnesium Citrate 25% 13 Calcium Lactate 25% 14 Magnesium Lactate 25% 15 Calcium Fumarate 25% 16 Potassium Bitartrate 25% 17 Sodium Chloride 25% 18 Potassium Chloride 25% 19 Potassium Gluconate 10% & Tripotassium Citrate 10% 20 Potassium Gluconate 10% & Potassium Bitartrate 10% 21 Tripotassium Citrate 10% & Potassium Bitartrate 10% 22 Potassium Gluconate 10%, Tripotassium Citrate 10% & Potassium Bitartrate 10% 23 CONTROL SAMPLE (no salt) 24 Sodium Gluconate 25%

[0034] The loading in all cases was an addition to the matrix+salt of D-limonene at a rate of 15% of the matrix+salt.

[0035] The particles were prepared by blending the modified starch, maltodextrin and (where applicable) salt/salt mixture into warm water (40 C.). To this, the D-limonene was added, and the mixture subjected to high shear mixing to emulsify the mixture to a mean particle size of less than 1.0 micron as measured by a laser diffraction particle size analyzer.

[0036] The emulsion was then spray-dried using an Anhydro PSD55 spray drying unit equipped with a rotary atomizer and a peristaltic delivery pump. Inlet and outlet temperatures were respectively 170 C. (5 C.) and 95 C. (3 C.). The powder was recovered by means of a cyclone separator.

EXAMPLE 2

Testing of Oxidative Stability

[0037] The various particles were tested for oxidative stability by determining the proportion of D-limonene remaining after various periods of storage. The samples were stored at 40 C. and 30% relative humidity in LDPE bags of a type that did not provide a barrier to moisture absorption. Samples were analyzed by GC and MS. In addition to the control sample, there were also included two particles made using the same matrix and made using the same conditions and equipment, but with sugar in place of the salts, one with 50% sugar, the other with 40% sugar. These were designated S1 and S2, respectively.

[0038] The results are shown in Tables 2 and 3. Table 2 shows the proportion of D-limonene remaining and Table 3 shows the proportion of oxidation by-products present. An acceptable D-limonene loss was less than 10% of the original proportion (i.e. a limonene content of greater than 13.5%), or when the oxidation by-product proportion exceeded 2.5% of the original limonene proportion (at which level the sample fails organoleptically), no further measurements were taken.

TABLE-US-00002 TABLE 2 Stability Study Results for sample D-Limonene assay values Stability-Limonene Levels Sam- 4- 8- 12- 16- 18- 24- ple No. Initial Weeks Weeks Weeks Weeks Weeks Weeks 1 14.18 13.51 12.83 11.99 11.40 2 15.69 14.67 13.78 12.74 11.87 3 13.91 13.73 13.53 13.26 13.08 12.92 4 14.44 14.33 14.22 14.10 13.96 13.94 5 14.59 14.52 14.41 14.26 14.18 14.33 6 14.75 14.46 14.27 13.86 7 14.58 14.19 13.88 13.60 8 14.79 14.09 13.89 13.25 9 14.66 14.37 13.88 13.82 10 13.45 12.64 11.96 11.34 11 14.04 12.99 12.23 11.61 12 13.78 12.66 11.85 11.28 13 14.64 13.29 12.59 12.04 14 14.11 13.40 12.84 12.50 15 16.76 15.91 15.21 14.67 16 14.82 14.22 13.50 13.04 17 14.52 14.20 13.79 13.35 12.87 12.54 18 14.82 14.44 13.98 13.55 13.16 12.86 19 14.67 14.41 14.31 14.10 13.98 13.92 20 14.68 14.46 14.10 13.87 13.13 13.01 21 14.91 14.62 14.48 14.20 14.16 14.03 22 14.85 14.60 14.55 14.01 13.82 13.70 23 14.38 13.67 13.25 12.71 (control) 24 14.57 14.26 14.18 14.09 S1 13.56 13.47 13.37 12.91 12.50 S2 14.12 13.39 13.24 12.71

TABLE-US-00003 TABLE 3 Stability-Oxidation Products Levels Sample 4- 8- 12- 16- 18- 24- No. Initial Weeks Weeks Weeks Weeks Weeks Weeks 1 0.31 1.23 2.23 3.40 4.03 2 0.41 1.58 2.37 3.41 4.09 3 0.39 0.77 1.02 1.41 1.69 2.60 4 0.67 0.60 0.80 0.67 0.88 2.48 5 0.50 0.51 0.60 0.51 0.69 1.18 6 0.47 0.62 0.83 0.83 7 0.68 1.04 1.55 1.29 8 0.65 0.98 1.38 0.97 9 0.40 0.56 0.73 0.55 10 0.48 1.15 2.62 3.05 11 0.76 2.09 2.94 3.23 12 0.55 1.99 2.97 3.09 13 0.60 1.93 3.55 4.03 14 0.57 1.19 2.32 2.36 15 0.66 1.51 2.67 2.88 16 0.35 1.03 1.61 1.77 17 0.29 0.57 1.06 2.04 2.26 3.25 18 0.29 0.52 0.95 1.86 2.16 3.17 19 0.31 0.58 0.82 1.21 1.22 1.89 20 0.25 0.62 0.91 1.51 2.62 3.80 21 0.26 0.64 0.81 1.30 1.33 2.14 22 0.27 0.51 0.65 1.38 1.50 2.37 23 0.51 1.90 2.54 (control) 24 0.45 0.72 0.74

[0039] From the tables, it can be seen that [0040] (i) the control and the two sugar-containing samples failed early. [0041] (ii) especially good results were obtained from samples 4, 5, 19, 21 and 22, that is: [0042] Magnesium Citrate 10%, Mannitol 20% [0043] Magnesium Citrate 20% & Potassium Gluconate 10% [0044] Potassium Gluconate 10% & Tripotassium Citrate 10% [0045] Tripotassium Citrate 10% & Potassium Bitartrate 10% [0046] Potassium Gluconate 10%, Tripotassium Citrate 10% & Potassium Bitartrate 10%

[0047] Many of the other salts were acceptable for short duration storage times.