PREPARATIONS COMPRISING A FLAVORING AND TEA EXTRACT

Abstract

The present invention primarily relates to a process for producing a preparation for nourishment or pleasure, preferably a beverage or a convenience food, such as a soup, a sauce or a snack, or semi-finished product for the production of a preparation for nourishment or pleasure, preferably a beverage or a convenience food, such as a soup, a sauce or a snack, the process comprising preparing a dispersion, in particular an emulsion, by mixing a functional agent, preferably flavoring, a tea extract and water with each other, and optionally drying the emulsion. The present further relates to related processes, products and uses.

Claims

1. A process for producing a preparation for nourishment or pleasure comprising: (a) providing a functional agent, a tea extract, and water; (b) preparing a dispersion by mixing the functional agent, the tea extract, and the water; and (c) optionally, drying the dispersion.

2. The process of claim 1, wherein the functional agent forms an emulsion with the tea extract and the water.

3. The process of claim 1, wherein the tea extract is selected from an extract from black tea, white tea, green tea, or mixtures thereof.

4. The process of claim 1 comprising (c) drying the dispersion, wherein the drying is carried out by spray drying.

5. The process of claim 1, wherein the dispersion is prepared by dispersing, sonicating, and/or homogenizing the functional agent, the tea extract, and the water.

6. The process of claim 1, wherein the tea extract is provided as a dry powder in (a) and mixed with the water in (b) in a weight ratio of 1:10 to 10:1 (tea extract:water) or the tea extract is provided as a paste in (a) and mixed with the water in (b) in a weight ratio of from 1:1 to 100:1 (tea extract:water).

7. The process of claim 1, wherein the functional agent is in an amount of from 0.1 to 150 wt. %, relative to a dry mass of the tea extract.

8. The process of claim 4, wherein the dried dispersion comprises particles having a mean diameter of 50 nm to 2 mm.

9. The process of claim 1 wherein the preparation is free of a matrix or carrier material other than the tea extract.

10. A preparation for nourishment or pleasure prepared according to the process of claim 1.

11. The preparation of claim 10, wherein the preparation is provided in the form of a dried dispersion.

12. The preparation of claim 10, wherein the preparation is a powder or agglomerates of powder.

13. The process of claim 1, further comprising: (d) packaging the dispersion.

14. (canceled)

15. (canceled)

16. A process for producing an edible composition comprising: (a) providing a flavoring, a tea extract, and water; (b) preparing an emulsion by mixing the flavoring, the tea extract, and the water; and (c) drying the emulsion.

17. The process of claim 16, wherein the tea extract is selected from an extract from black tea, white tea, green tea, or mixtures thereof.

18. The process of claim 16, wherein the emulsion is spray dried in (c).

19. The process of claim 16, wherein the emulsion is formed by homogenizing the flavoring, the tea extract, and the water in (b).

20. The process of claim 16, wherein the tea extract is provided as a dry powder in (a) and mixed with the water in (b) in a weight ratio of 0.5:1 to 1:1 (tea extract:water) or the tea extract is provided as a paste in (a) and mixed with the water in (b) in a weight ratio of from 2:1 to 50:1 (tea extract:water).

21. The process of claim 16, wherein the flavoring is in an amount of 1 to 100 wt. %, relative to a dry mass of the tea extract.

22. The process of claim 16, wherein the dried emulsion comprises droplets having a mean diameter of 0.1 to 1 ?m.

Description

[0046] The drawings show:

[0047] FIG. 1 Droplet size distribution of black tea extract water phase before (BTE3) and after (BTE1-LF-E-3) emulsification of lemon-lime flavoring.

[0048] FIG. 2 Formation of lemon-lime flavor emulsions: Hydrolyzed starch/modified starch combination vs. black tea extract. Droplet size measurement after 0 h.

[0049] FIG. 3 Stability of lemon-lime flavor emulsions: Hydrolyzed starch/modified starch combination vs. black tea extract. Droplet size measurement after 24 h storage at room temperature.

[0050] FIG. 4A Emulsification of functional agent (plant oil) by means of dry tea extract BTE2: Variation of the weight ratio of the tea extract to the water (=tea extract-water-ratio). Amount of plant oil in emulsion kept constant. Comparison of mean droplet sizes (triangles) and viscosities measured at a shear rate of 2000/s (dots).

[0051] FIG. 4B Emulsification of functional agent (plant oil) by means of pasty tea extract BTE3 as emulsifier: Variation of the weight ratio of the tea extract to the water (=tea extract-water-ratio). Amount of plant oil in emulsion kept constant. Comparison of mean droplet sizes (triangles) and viscosities measured at a shear rate of 2000/s (dots).

[0052] FIG. 4C Emulsification of functional agent (plant oil) by means of dry tea extract BTE2 as emulsifier: Variation of the amount of functional agent relative to the dry mass of the tea extract (=oil-tea extract-ratios) in the emulsions. Weight ratio of the tea extract to the water kept constant (Tea extract-water-ratio=0.86). Comparison of mean droplet sizes (triangles) and viscosities measured at a shear rate of 2000/s (dots).

[0053] FIG. 4D Effect of tea extract-water-ratio and flavor loading on emulsification of lemon-lime flavoring: Droplet size measurement after 0 h.

[0054] FIG. 5A Dispersing different types of flavorings using black tea extracts: Grapefruit (BTE1-GF-E-1), lemon-lime (BTE1-LF-E-3), peach (BTE3-PF-E-2). Droplet size measurement after 0 h.

[0055] FIGS. 5B,5C Emulsification of plant oil by using BTE2 as emulsifier: Changes of viscosity, temperature (A) and droplet size distribution (B) during emulsion preparation, as a function of dispersing time (0 s-240 s). Formulation: BTE2-PO-E-2.

[0056] FIG. 6 Stability of plant oil emulsions using different types of tea extracts: Black tea extract (BTE1-PO-E-1), green tea extract (GTE1-PO-E-1), white tea extract (WTE2-PO-E-1). Droplet size measurement after 0 h.

[0057] FIG. 7 Emulsification of plant oil using different types of tea extracts: Black tea extract (BTE1-PO-E-1), green tea extract (GTE1-PO-E-1), white tea extract (WTE2-PO-E-1). Droplet size measurement after 24 h.

[0058] FIG. 8 Spray-drying of lemon-lime-flavoring on black tea extracts. Comparison of different inlet air temperatures: 175? C. (dashed line) and 190? C. (solid line). Particle size measurements of powders after 0 h. Raw material (black tea extract BTE1) as reference (dashed-dotted line).

[0059] FIG. 9 Spray-drying of different flavoringstea extractcombinations. Particle size measurements of powders after 0 h. Spray-drying formulation M/C-LF-SD-1 included as a reference.

[0060] FIG. 10 Spray-drying of lemon-lime flavoring on modified starch/hydrolyzed starch M/C-LF-SD-1 (A), black tea extract BTE1-LF-SD-1 (B), and green tea extract GTE1-LF-SD-1 (C). Images of dried powders: digital microscope, magnification 200?.

[0061] FIG. 11A Spray-drying (SD) of lemon-lime flavoring on black tea extract: Aroma analysis by means of GC-MS after solvent extraction. (A) pure, liquid flavoring before emulsification and SD. (B) Flavoring after emulsification and SD on black tea extract (BTE1-LF-SD-1). Amount of pure flavoring adjusted to SD formula.

[0062] FIG. 11B Spray-drying of functional agents by means of dry tea extract BTE2 as emulsifier and carrier: Variation of the amount of functional agent relative to the dry mass of the tea extract (=flavoring-tea extract-ratios) in the pre-emulsions. Tested functional agents: y-decalactone and D-limonene. Weight ratio of the tea extract to the water (tea extract-water-ratio) in the pre-emulsions adjusted to viscosities of 150?3 mPas at a shear rate of 2000/s. Comparison of flavor retention (dots) and surface oil (triangles) measured by means of GC-MS.

[0063] FIG. 12 Spray-drying (SD) of grapefruit flavoring on black tea extracts: Comparison of particle size distribution before and after particle agglomeration by means of fluidized bed agglomeration (=simulation of spray-bed drying (SBD)). Particle size measurements of powders after 0 h.

[0064] FIG. 13 Microscopic comparison of spray-dried particles (A) and agglomerated, spray bed-dried particles (B). Formulation: BTE1-GF-SD-1. Images of dried powders: digital microscope, magnification 500?.

EXAMPLES

1. Materials and Methods

[0065] Particle and droplet size distributions were determined with the laser diffraction analyser Mastersizer 2000 (Malvern Panalytical, United Kingdom) using the parameters summarized in Table 1. Viscosity measurements of the emulsions and slurries were performed with a MCR 302 rheometer (Anton Paar, Austria) using a cone-plate system at a ramped shear rate program (1-2000 m/s) and 25? C. in combination with the Rheoplus software (Anton Paar). Details for the tea extracts used in the experiments can be found in Table 2. Tables 3 to 6 list the formulations tested.

[0066] For preparation of the emulsions, the tea extract powder or paste or/and other powders were first mixed with water and stirred for at least 15 min. The mixture was then dispersed using a rotor-stator system Ultra-Turrax (IKA, Germany), while the non-polar flavoring or oil was added dropwise. The total disperging time was adjusted to the sample volume (e.g. 2 min for 60-150 mL; 15 min for 500-1000 mL).

[0067] For preparation of the slurries, the tea extract powder or paste, the water, and the polar flavoring were mixed and stirred for at least 15 min.

[0068] The resulting homogenous emulsions and slurries were then used as such, e.g. for analytical purposes, or spray-dried. Single-stage spray-drying of the emulsions or slurries was carried at an inlet air temperature of 190? C. and outlet air temperature of 70? C., if not indicated otherwise.

[0069] Microscopic images were obtained with the digital microscope VHX (Keyence, Japan) equipped with an universal zoom lens VH-Z100UR (Keyence).

TABLE-US-00001 TABLE 1 Measurement of particle and droplet size distributions by means of Malvern Mastersizer 2000. Used system parameters: Particle Particle Disper- Dispersant refractive absorption sant refractive Dispersion index index name index unit Powder 0 0 1 Scirocco 2000 (dry) Emulsion 1.45 0.01 Water 1.33 Hydro 2000S (wet)

TABLE-US-00002 TABLE 2 Used tea extracts and nomenclature Dry Matter Nomen- Content Labeling Form clature (measured) TEA BLACK EXTRACT POWDER BTE1 92.7% TEA BLACK EXTRACT POWDER BTE2 96.2% TEA BLACK EXTRACT DARK PASTE BTE3 34.0% TEA BLACK EXTRACT POWDER BTE4 93.0% TEA GREEN EXTRACT POWDER GTE1 94.0% ORGANIC TEA GREEN EXTRACT POWDER GTE2 93.6% TEA GREEN EXTRACT POWDER GTE3 94.3% ORGANIC TEA WHITE EXTRACT POWDER WTE1 95.1% TEA WHITE EXTRACT POWDER WTE2 93.7%

TABLE-US-00003 TABLE 3 Tested Formulations: Starch/Tea extract - lemon flavoring - emulsions M/C- BTE1/C- BTE1- BTE1- BTE1- BTE1- LF-E-1 LF-E-2 LF-E-1 LF-E-2 LF-E-3 LF-E-4 Lemon-Lime-Flavoring 11.5 11.7 11.8 11.7 12.2 17.7 (LF) Maltodextrin 78.1 OSA-modified starch 9.6 9.8 BTE1 80.7 80.5 100.9 90.4 87.7 Water 100.7 100.1 100.7 80.4 90.4 87.7

TABLE-US-00004 TABLE 4 Tested Formulations: Tea extract - plant oil - emulsions BTE1- BTE4- GTE1- WTE2- BTE3- BTE3- BTE2- BTE2- GTE2- WTE1- PO- PO- PO- PO- PO- PO- PO- PO- PO- PO- E-1 E-1 E-1 E-1 E-1 E-2 E-1 E-2 E-1 E-2 GTE2 60 WTE1 60 Plant Oil 8 8 8 8 8 8 8 8 8 8 Triglyceride Palmfree (PO) GTE1 60 BTE3 105 110 BTE4 60 BTE1 60 BTE2 60 50 WTE2 60 Water 60 60 60 60 15 10 60 58 60 60

TABLE-US-00005 TABLE 5 Tested Formulations: Tea extract - grapefruit flavoring - emulsions BTE1-GF- BTE4-GF- GTE1-GF- WTE2-GF- E-1 E-1 E-1 E-1 Grapefruit Flavor 8 8 8 4 Concentrate (GF) GTE1 60 BTE4 60 BTE1 60 WTE2 60 Water 60 60 60 60

TABLE-US-00006 TABLE 6 Tested Formulations: composition/slurries used for spray-drying experiments M/C- BTE1- BTE2- GTE3- GTE1- BTE1- BTE3- BTE3- BTE3- LF- LF- LF- LF- LF- GF- PF- PF- CF- SD-1 SD-1 SD-1 SD-1 SD-1 SD-1 SD-1 SD-2 SD-1 Lemon-Lime- 30.0 68.8 85.0 40.0 50.0 Flavoring (LF) Cola Flavoring 36.5 (CF) Grapefruit 153.0 Flavor Concentrate (GF) Maltodextrin 205.0 Peach 55.7 60.1 Flavoring (PF) OSA-modified 25.0 starch GTE1 300.0 GTE3 300.0 BTE3 743.6 600.0 468.8 BTE1 445.0 918.1 BTE2 445.0 Vanilla 1.0 Flavoring Water 265.0 492.2 491.3 350.0 350.0 1020.0 67.4 81.0 93.8 FLAVOUR 11.5% 13.4% 16.0% 11.8% 14.3% 16.7% 17.6% 22.3% 18.6% LOADING (theoretical) Weight ratio 0.90.sup.a 0.91.sup.a 0.86.sup.a 0.86.sup.a 0.90.sup.a 11.03.sup.b 7.41.sup.b 5.00.sup.b of tea extract to water BTE1- BTE1- M/C- GTE1- BTE1- M/C- GTE3- BTE2- ChF- BF- ChF- ChF- BF- L- L- L- SD-1 SD-1 SD-1 SD-1- SD-1 SD-1 SD-1 SD-1 Chicken 75 100 100 Flavoring (ChF) Natural Beef 55 121 121 121 Flavoring (BF) BTE1 500 375 55 Water 550 410 800 327 FLAVOUR 9.8% 9.8% 12.8% LOADING (theoretical) Weight ratio of 0.86.sup.a 0.91.sup.a tea extract to water BTE1-PF- BTE2-PF- BTE6-PF- GTE2-LO- BTE6-LO- SD-1 SD-1 SD-1 SD-1 SD-1 Lemon Oil (LO) 259.0 270.3 Peach Flavoring (PF) 81.9 81.9 81.9 GTE2 1036.1 BTE1 426.2 BTE2 426.3 BTE6 432.1 1081.1 Water 460.0 498.0 470.9 1103.8 1223.0 FLAVOUR LOADING 16.1% 16.1% 15.9% 20.0% 20.0% (theoretical) Weight ratio of tea 0.93 0.86 0.92 0.94 0.88 extract to water .sup.atea extract provided as a dry powder .sup.btea extract provided in pasty form

2. Results

2.1. Emulsification of Flavorings Using Tea Extracts

2.1.1. Formulation Optimization

[0070] The particle size distribution was determined before (BTE3) and after (BTE1-LF-E-3) emulsification of a lemon-lime flavoring. It was observed that the black tea extract itself contained nano-aggregates smaller than 100 nm and undefined particles bigger than 1000 nm. After emulsification, droplets having a particle size ranging from 200 nm to 1000 nm were formed in addition (cf. FIG. 1).

[0071] Droplet size distribution of lemon-lime flavor emulsions based on hydrolyzed starch/modified starch combination (as reference) vs. tea extract are shown in FIG. 2. The samples were prepared by solubilization of solids under stirring and addition of the oil phase while dispersing by means of rotor-stator system. Droplet size measurements were conducted after 0 h. It was found that emulsification of the flavoring in the presence of the tea extracts resulted in droplet sizes <1 ?m, and was similar to the reference hydrolyzed starch/modified starch combination. A comparison of FIGS. 1 and 2 suggests that the additionally measured particles <100 nm derived from the tea extracts themselves.

[0072] All samples were then stored for 24 h at room temperature. Then, 24 h after emulsification, the droplet size distribution was re-determined. After 24 h storage, the droplet sizes of the emulsions containing OSA-modified starch significantly increased, suggesting a low emulsion stability. By contrast, no differences in the droplet size distribution occurred for the emulsion stabilized by black tea extract suggesting that the emulsion stabilized by the tea extract was more stable than the reference formulation (FIG. 3).

[0073] Then, the ratios between black tea extract and water as well as the ratios between flavoring and dry mass content of the emulsion, expressed as flavor loading, were varied. The extract-water-ratio had a substantial effect on the viscosity and has to be finely tuned to facilitate technical operations such as pumping or spray-drying. The desired ranges of viscosity are typically 100-150 mPas. An increase of the flavor loading from 13.5% to 20.2% did not alter the viscosity significantly (Table 7, FIGS. 4A-4C). By contrast, varying the extract-water-ratio had only a slight effect on the mean diameters of the droplet size distributions (FIG. 4D).

TABLE-US-00007 TABLE 7 Effect of tea extract-water-ratio and flavor loading on emulsification of lemon-lime flavoring: Tested formulations and viscosity measurement by means of rheometer (Anton Paar). BTE1-LF- BTE1-LF- BTE1-LF- BTE1-LF- E-1 E-2 E-3 E-4 Lemon-Lime-Flavoring 11.8 11.7 12.2 17.7 Black Tea Extract 80.5 100.9 90.4 87.7 BTE1 Water 100.7 80.4 90.4 87.7 Total in g (3 Parts): 193 193 193 193 Flavor Loading 14.6% 11.6% 13.5% 20.2% (calculated) Viscosity (2000 1/s) 45 mPas 440 mPas 140 mPas 141 mPas

2.1.2. Variation of Flavorings

[0074] The effect of the flavoring on the particle size distribution is shown in FIG. 5A. The emulsification of the non-polar citrus flavorings lemon-lime and grapefruit by means of black tea extracts resulted in similar oil droplet size distributions. The more polar peach flavoring was almost completely water soluble so that a slurry rather than an emulsion was formed (as expected). Notably, the peaks at 200 nm and about 1 ?m do not indicated emulsion droplets but are presumably due to nano-aggregates present in the black tea extract (cf. FIG. 1).

2.1.3. Emulsification Properties

[0075] The emulsion preparation process was optimized with respect to the disperging time at hand of the example plant oil and BTE2 as emulsifier. The changes of viscosity, temperature and droplet size distribution during emulsion preparation, as a function of disperging time, is illustrated in FIGS. 5B and 5C.

2.1.4. Variation of Tea Extracts

[0076] The effect of the different tea extracts on the particle size distribution is shown in FIG. 6. In these experiments, plant oil was used as an inert model for a non-polar flavoring. It was observed that the emulsification of a plant oil differed substantially between the types of tea extracts used as emulsifiers. Notably, black tea extracts resulted in the lowest oil droplet sizes by far (<1000 nm).

[0077] The emulsion stability was evaluated by measuring the droplet size distribution 24 h after emulsification and storage at room temperature. Despite the differences in the droplet size distributions, all the tested plant oil-tea extract-emulsions remained stable after 24 h (FIG. 7). The results demonstrate the tea extracts' in particular the black tea extracts' suitability as emulsifiers.

[0078] The trend reported in FIG. 6 was confirmed by further experimental results summarized in Table 8, in which different qualities of black, green, and white tea extracts were compared.

[0079] The same trend was also observed in further experimental results, in which a grapefruit flavoring was used as a non-polar functional agent instead of the plant oil (formulations in Table 5, results not shown).

TABLE-US-00008 TABLE 8 Emulsification of plant oil using different types of tea extracts. Droplet size measurement after 0 h. Emulsifier Formulation D [4.3] Uniformity D [3.2] d (0.1) d (0.5) d (0.9) Black Tea BTE1-PO-E-1 0.73 0.46 0.56 0.32 0.64 1.26 Extracts BTE4-PO-E-1 1.51 3.02 0.28 0.12 0.43 4.38 BTE3-PO-E-1 0.80 0.47 0.62 0.36 0.69 1.41 BTE3-PO-E-2 0.79 0.49 0.60 0.34 0.67 1.42 BTE2-PO-E-1 0.90 0.37 0.74 0.45 0.83 1.45 MEAN 0.94 0.96 0.56 0.32 0.65 1.98 Green GTE1-PO-E-1 3.29 0.93 1.80 0.91 2.12 6.76 Tea GTE2-PO-E-1 3.40 0.52 2.37 1.23 2.98 6.15 Extracts MEAN 3.35 0.72 2.09 1.07 2.55 6.46 White Tea WTE2-PO-E-1 3.61 0.22 3.37 2.50 3.47 4.88 Extracts WTE1-PO-E-1 5.76 0.42 4.31 2.57 5.29 9.63 MEAN 4.68 0.32 3.84 2.53 4.38 7.25

[0080] While all tea extract emulsions remained stable for at least 24 h (FIG. 6), a differential picture was observed after longer storage times. Here, significant differences occurred between the types of tea extracts after 2 months of storage at room temperature. According to visual inspection, the black tea extract emulsions remained homogeneously stable, with no observable sedimentation or creaming. By contrast, creaming layers were formed on top of the emulsions based on white tea extracts and green tea extracts. Also, visible sedimentations occurred in these extracts (data not shown). These data reaffirm the stability of emulsions based on black tea extract.

2.2. Analyses of Raw Materials

[0081] It was hypothesized that the high stability of emulsions based on black tea extract is related to surface-active ingredients such as saponins, also referred to as triterpene glycosides. The amphipathic nature of saponins gives them activity as surfactants. Therefore, the tea extracts were subject of a screening for non-volatile compounds by means of LC-MS/UV (VION). The analytical screening for potentially surface-active compounds revealed significant differences between the types of tea extracts. Surprisingly, no saponins could be found in any tested black tea extract (BTE1, BTE2, BTE3 and BTE4) despite best emulsion formation and stability induced by the black tea extracts, whereas different saponins (e.g. theasaponins, foliatheasaponins, chakasaponins) were detected in both green tea extracts (GTE1, GTE2) and white tea extracts (WTE1, WTE2) (data not shown), which performed worse than the black tea extracts.

2.3. Spray-Drying of Flavorings on Tea Extracts

2.3.1. Spray-Drying Process Development

[0082] Spray-drying of the flavoring emulsion stabilized by black tea extract under typical conditions could be performed without any technical problems. Homogenous powder particles having particle sizes typical for spray-drying (<50 ?m) were obtained (FIG. 8).

[0083] Spray-drying of different flavoringtea extractcombinations was conducted and the particle size distributions were measured directly after spray drying (0 h). The spray-drying formulation M/C-LF-SD-1 was included as a reference. Spray-drying of all tested combinations resulted in homogenous powder particle distributions, comparable to the hydrolyzed starch/modified starchcombination (reference). Images of the dried powders are depicted in FIG. 10.

[0084] Aroma analyses of pure, liquid lemon-lime flavoring (before emulsification and spray-drying) as compared to spray-dried lemon-lime flavoringblack tea extractemulsion by GC-MS revealed that the obtained gas chromatograms were quantitatively and qualitatively comparable. This indicated that no systematic losses of volatile fractions occurred during the spray-drying process (FIG. 11). The same observation was made with peach flavoring spray-dried on a pasty black tea extract (data not shown).

[0085] These results demonstrate the suitability of tea extracts as (dry) carriers of flavorings.

[0086] Additional analytical data, investigating the upper limits of flavor loadings for the spray-drying process on tea extracts as compared to non-polar flavor compound (limonene) and rather polar flavor compound (y-decalactone), are shown in FIG. 11B.

[0087] Different tea extracts for encapsulation of flavorings were evaluated. The results are summarized in Tables 9 and 10.

TABLE-US-00009 TABLE 9 Spray-drying of flavorings by using tea extracts as emulsifiers and carriers: Comparison of different tea extracts for encapsulation of peach flavoring (PF) or lemon oil (LO). Physical characterization and flavor analyses of powders. BTE1-PF- BTE2-PF- BTE6-PF- GTE2-LO- BTE6-LO- SD-1 SD-1 SD-1 SD-1 SD-1 Powder Dry Matter 96.5% 96.7% 95.3% 94.5% 97.7% Apparent Density 528 560 400 508 504 (bulk density) [g/L] Powder Yield 44.31% 39.65% 44.27% 47.4% 46.0% Flavour Retention 84.2% 89.1% 91.3% 97.7% 100.5% Surface Oil 0.05% 0.08% 0.07% 0.05% 0.09%

TABLE-US-00010 TABLE 10 Spray-drying of functional agent by using different emulsifier/carrier systems: Comparison of tea extract GTE1 and reference combination (OSA-modified starch/maltodextrin) for encapsulation of a chicken flavoring (ChF). M/C-ChF-SD-1 GTE1-ChF-SD-1 Flavour Loading (theoretical) 9.80 9.80 [%] Flavour Loading (measured) 9.27 9.74 [%] Flavour Retention [%] 94.59 99.38 Surface Oil [%] 0.05 0.12

2.3.2. Agglomeration of Loaded Particles

[0088] Small powder particle sizes are related to technical drawbacks such as blocking or health risks for the operator. Therefore, larger particle sizes are preferred. To increase the particle size, agglomeration by means of fluidized bed agglomeration (=simulation of spray-bed drying (SBD)) has been conducted. The agglomeration of a grapefruit-black tea-powder by means of fluidized bed agglomeration resulted in large particle sizes (FIG. 12), without any technical problems.

[0089] Microscopic pictures of spray-dried particles and agglomerated, spray bed-dried particles are shown in FIG. 13.

2.3.3. Shelf Life Studies of Loaded Powders

[0090] Accelerated shelf-life studies of the loaded powders were carried out using Symager? technology, which allowed to study the oxidative stability throughout the simulated storage time. In place of the Symager? technology, the oxipres apparatus (Mikrolab, Aarhus, Denmark) can be equally used. After incubation, the taste of the aged samples was compared to the non-aged samples by means of sensory triangular tests. If no statistically significant difference was perceived, the sample was considered to be stable from a sensory perspective throughout the tested shelf-life time. Referring to the results presented in Table 11 below, the lemon-lime flavoring (as an exemplary citrus flavoring known to be susceptible to oxidation) spray-dried on a combination of hydrolyzed starch and modified starch was significantly different after being stressed for 12 months and attributed with off-flavors by the panelists. The results illustrate well that in formulations based on starches, typically additional antioxidants are required. By contrast, no statistical sensory differences were measurable for the flavorings spray-dried on black tea extracts. Despite knowing that tea extract has a certain antioxidative potential, it was surprising that it was capable to completely inhibit the chemical deterioration of the susceptible flavorings during storage.

TABLE-US-00011 TABLE 11 Accelerated Shelf Life Study of lemon-lime flavorings spray- dried on different carriers. Accelerated ageing by means of SYMAGER? technology to simulate different storage times. Sensory triangular test to analyze statistical differences between non-aged reference and accelerated aged sample. # Formulation 1 Carrier Emulsifier Flavoring Drying Code 2 Black tea extract Lemon-lime SD BTE1-LF-SD-1 3 Black tea extract (Paste) Peach SD BTE3-PF-SD-1 4 Black tea extract Lemon-lime SD BTE2-LF-SD-1 5 Black tea extract Grapefruit SBD BTE1-GF-SD-1 6 Hydrolyzed Modified Lemon-lime SD M/C-LF-SD-1 7 starch starch # Sensory triangular test (a) 1 Simulated still Statis- storage Correct acceptable tical Descriptors time answers (b) difference 2 12 months 5 3 no 3 12 months 3 3 no 4 12 months 2 0 no 5 12 months 2 0 no 6 6 months 6 2 no 7 12 months 9 2 yes Strong off- note, bitter, oxidized (a) Laboratory expert panel. Number of panelists n = 10. Reference sample ambient stored. Dosage of reference or accelerated powders: 0.25 g/L. Significance level 95%. (b) Among correct answers: taste still acceptable

[0091] Results of an aroma analysis by means of Headspace-SPME-GC-MS (not shown) were in accordance to the sensory data. The gas chromatograms obtained from the starch-based samples significantly changed during the simulated 12 months of storage, which indicated the chemical changes in the composition of volatiles. In contrast thereto, the gas chromatograms obtained from the tea-extract-based samples did not significantly change during the simulated 12 months of storage.

[0092] Additional analytical data, supporting the better shelf-life stability of tea extracts (black and green) compared to reference emulsifier/carrier systems are summarized in Table 12 below. Flavour analyses of non-aged powders (0 m) were found to be comparable regarding retention and flavour composition for both tea extract and the reference carrier systems. After 12 months of simulated ageing in Oxipress, a significant decline of flavour retention and concentration of limonene in reference carrier system was observed. At the same time, chemical oxidation products (e.g. carveols, limonene epoxides) responsible for non-desirable off-flavours were formed. By contrast, no significant changes of flavour profiles of both tea extract carrier systems could be determined. In summary, the flavour analyses demonstrated that the chemical stability of d-limonene increased, if it was encapsulated by either black tea extract or green tea extract compared to the reference carrier system based on maltodextrin.

TABLE-US-00012 TABLE 12 Simulated ageing of limonene-loaded powders based on different emulsifier/carrier systems: Comparison of overall flavor retentions and flavor compound profiles. Pre-emulsions with 27.5 weight-% D-limonene relative to the dry mass of the emulsifier and carrier. Viscosities of pre-emulsions adjusted to 150 ? 3 mPa .Math. s. Simulated ageing of powders by means of Oxipress. Code BTE2-L-SD-1 GTE3-L-SD-1 Emulsifier/Carrier BTE2 GTE3 Storage Time (simulated) [months] 0 12 0 12 Flavor Retention [%] Flavor compounds [ppm] .sup.a RI .sup.b 97.5 95.3 99.4 96.9 Limonene 1212 221467.6 257757.7 225803.7 254092.3 trans-Limonene-1,2-epoxide 1462 54.4 62.7 44.4 57.9 cis-Limonene-1,2-epoxide 1475 34.9 28.0 30.7 36.3 Limonene-8,9-epoxide 1572 n.d. n.d n.d. n.d. trans-p-2,8-Menthadien-1-ol 1639 86.8 81.7 67.7 72.6 cis-p-2,8-Menthadien-1-ol 1681 72.4 64.9 63.6 62.5 Carvone 1756 n.d. 122.9 n.d. 114.1 trans-p-Mentha-1(7),8-dien-2- 1809 n.d. n.d n.d. n.d. ol trans-Carveol 1846 131.1 64.2 119.3 77.5 cis-Carveol 1878 74.6 46.6 72.9 42.6 cis-p-Mentha-1(7),8-dien-2-ol 1901 n.d. n.d n.d. n.d. 8,9-Carveol epoxide 2097 53.3 n.d. 42.9 n.d. Code M/C-L-SD-1 Emulsifier/Carrier OSA-modified starch/ Maltodextrin (reference) Storage Time (simulated) [months] 0 12 Flavor Retention [%] Flavor compounds [ppm] .sup.a RI .sup.b 99.8 44.2 Limonene 1212 266406.2 115807.3 trans-Limonene-1,2-epoxide 1462 n.d. .sup.c 5057.4 cis-Limonene-1,2-epoxide 1475 34.5 4048.0 Limonene-8,9-epoxide 1572 n.d. 1403.1 trans-p-2,8-Menthadien-1-ol 1639 135.7 673.2 cis-p-2,8-Menthadien-1-ol 1681 121.2 525.9 Carvone 1756 359.8 5360.5 trans-p-Mentha-1(7),8-dien-2- 1809 n.d. 601.5 ol trans-Carveol 1846 91.0 3057.7 cis-Carveol 1878 64.6 820.2 cis-p-Mentha-1(7),8-dien-2-ol 1901 n.d. 111.9 8,9-Carveol epoxide 2097 n.d. 37.0 .sup.a Aroma molecules analyzed by means of GC-MS/FID. Molecule identification based on comparison of mass spectra and retention indices with internal data bases. Quantitation by using internal standard 2-nonanol. .sup.b Retention indices measured on polar GC-column (WAX). .sup.c Compound not detected.

2.3.4. Application Tests

[0093] Spray-dried lemon-lime flavoring powders were applied on beverage test bases using dosage of 0.25 g/L and the beverage was visually and sensory evaluated.

[0094] It was observed that the flavoring spray-dried on tea extract lead to a beverage that was clear and did not result in sedimentations, similar to the reference beverage obtained from the hydrolyzed starch/modified starch combination. Moreover, the taste of the beverage was identical to the reference beverage.

TABLE-US-00013 TABLE 13 Application of D-limonene-loaded powders based on different emulsifier/carrier systems: Turbidity measurements of powders in buffered aqueous solutions (pH 3, pH 5, pH 7). Concentrations of powders adjusted to 0.1 g limonene per litre of solution. Code BTE2-L-SD-1 GTE3-L-SD-1 M/C-L-SD-1 Emulsifier/Carrier OSA-modified starch/ Turbidity Maltodextrin (FNU) BTE2 GTE3 (reference) pH 3 36.2 20.9 18.4 pH 5 33.2 24.6 18.8 pH 7 33.1 22.7 19.7