PARTICULATE PRODUCTS AND METHOD FOR PRODUCTION THEREOF

Abstract

The present invention relates to a process for the production of an agglomerated particulate product containing one or more flavorant(s) and/or odorant(s). By spraying with certain binders, the storage stability of the particulate product is significantly improved, and the flavorant(s) and/or odorant(s) are protected, in particular, from oxidation. The present invention also relates to particulate products containing one or more flavorant(s) and/or odorant(s), preferably produced by a process according to the invention, and to the use of certain substances for improving the storage stability of particulate products containing one or more flavorant(s) and/or odorant(s).

Claims

1-15. (canceled)

16. A process for producing a particulate product comprising one or more flavorants and/or odorants, the process comprising: (i) producing particles comprising or consisting of the one or more flavorants and/or colorants and one or more carriers by spray drying in a drying chamber of a spray drying apparatus; (ii) spraying the particles in a fluidized bed which is integrated into the drying chamber with an aqueous solution that is free from flavorants and/or colorants but comprises 10 to 30 vol % of one or more binders selected from mono or polysaccharides with reducing groups, sugar alcohols, and a mixture thereof, wherein (i) and (ii) occur simultaneously and the particles are kept in motion and agglomerated in the drying chamber.

17. The process of claim 16, wherein the one or more binders are selected from glucose, mannose, galactose, maltose, lactose, cellobiose, maltodextrin, gum arabic, traganth, gum ghatti, agar, carrageenan, guar flour, carubin, and combinations thereof.

18. The process of claim 16, wherein the one or more flavorants and/or odorants are selected from fruit aromas, meat aromas, vegetable aromas, spice aromas, meat extracts, vegetable extracts, spice extracts, and a mixture thereof.

19. The process of claim 16, wherein the one or more carriers are chosen from maltodextrins, dextrins, starches, flours, and fibrous materials.

20. The process of claim 16, wherein the particles produced by spray drying in (i) are produced by spray drying an emulsion comprising the one or more flavorants and/or odorants, the one or more carriers, and one or more emulsifiers; and the one or more flavorants and/or odorants and the one or more emulsifiers are in a weight ratio of 2:1 to 1:2 (one or more flavorants and/or odorants: one or more emulsifiers).

21. The process of claim 20, wherein the one or more emulsifiers are selected from gum arabic, modified starches, proteins, native and modified pectins, and soluble fractions of soy polysaccharides.

22. The process of claim 20, wherein the emulsion of (i) and the aqueous solution of (ii) are combined in a volume ratio of 5:1 to 15:1 (emulsion of (i):aqueous solution of (ii)) or solids of the emulsion of (i) and solids of the aqueous solution of (ii) are combined in a weight ratio of 30:1 to 70:1 (solids of (i):solids of (ii)).

23. A particulate product produced by the process of claim 16.

24. The particulate product of claim 23, wherein the one or more binders are selected from glucose, mannose, galactose, maltose, lactose, cellobiose, maltodextrin, gum arabic, traganth, gum ghatti, agar, carrageenan, guar flour, carubin, and combinations thereof.

25. The particulate product of claim 23 comprising or consisting of 2 to 35 wt. % of the one or more flavorants and/or the one or more odorants; and 65 to 98 wt. % of the one or more carriers, the one or more binders, and the one or more emulsifier; provided that if one or more of the one or more binders are not the same as one or more of the one or more carriers and/or the one or more emulsifiers, the product comprises 1 to 10 wt. % of one or more binders, in each case based on the total weight of the product.

26. The particulate product of claim 23, wherein the one or more carriers are selected from maltodextrins, dextrins, starches, flours, and fibrous materials and the one or more emulsifiers are selected from gum arabic, modified starches, proteins, native or modified pectins, and soluble fractions of soy polysaccharides.

27. The particulate product of claim 23, wherein the one or more odorants and/or flavorants are selected from fruit aromas, meat aromas, vegetable aromas, spice aromas, meat extracts, vegetable extracts, spice extracts, and a mixture thereof.

28. A product comprising a particulate product of claim 23 selected from food and beverage products, fruit and vegetable juice preparations, instant beverages, meat products, egg products, dairy products, products made from soy protein and other vegetable protein sources, fat- and oil-based products or emulsions thereof, fruit and vegetable preparations, snack foods, baked goods, confectionery, soups, sauces, spices and seasoning blends, instant products, ready meals, semi-finished goods, oral care products, pet food, and food supplements.

29. A method for improving oxidation stability one or more flavorants and/or odorants, the method comprising: (i) producing particles comprising or consisting of the one or more flavorants and/or colorants and one or more carriers by spray drying in a drying chamber of a spray drying apparatus; (ii) spraying the particles in a fluidized bed which is integrated into the drying chamber with an aqueous solution that is free from flavorants and/or colorants but comprises 10 to 30 vol % of one or more binders selected from mono or polysaccharides with reducing groups, sugar alcohols, and a mixture thereof, wherein (i) and (ii) occur simultaneously and the particles are kept in motion and agglomerated in the drying chamber.

30. The method of claim 29, wherein the one or more binders are selected from glucose, mannose, galactose, maltose, lactose, cellobiose, maltodextrin, gum arabic, traganth, gum ghatti, agar, carrageenan, guar flour, carubin, and combinations thereof.

31. The method of claim 16, wherein the one or more binders are selected from gum arabic, traganth, gum ghatti, agar, carrageenan, guar flour, carubin, and combinations thereof.

32. The particulate of claim 24, wherein the one or more binders are selected from gum arabic, traganth, gum ghatti, agar, carrageenan, guar flour, carubin, and combinations thereof.

Description

BRIEF DESCRIPTION OF THE FIGURES

[0072] FIG. 1 shows a spray drying agglomeration apparatus as described in EP3117720. (Z2) is the nozzle or atomizer construction, (H) is the weir (with the cap G) and (B) is the fluidized bed.

[0073] FIG. 2 shows spray-dried particles with lemon aroma that have not been agglomerated.

[0074] FIG. 3 shows spray-dried particles with lemon aroma agglomerated with water.

[0075] FIG. 4 shows spray-dried particles with lemon aroma agglomerated with 10% gum arabic.

[0076] FIG. 5 shows spray-dried particles with lemon aroma agglomerated with 30% maltodextrin DE8.

[0077] FIG. 6 shows cuvettes in which gum arabic of various origins and modified starch were tested with the Folin-Ciolteau reagent for reducing properties (see Example 3). Cuvettes 1 and 2 contain gum arabic (Seyal lot 32), cuvettes 3 and 4 contain gum arabic (Seyal lot 59), cuvettes 5 and 6 contain gum arabic (Senegal lot 55) and cuvettes 7 and 8 contain modified starch (lot 70).

EXAMPLE 1: SHELF LIFE OF SPRAY PRODUCTS WITH DIFFERENT BINDERS

[0078] Standard formulations were selected which have comparatively low shelf lives due to the sensitivity of the aroma, or which have new applications made possible by extending their shelf lives. Since the oxidation sensitivity of citrus aromas is very high, such were used here. The formulation comprises as solids about 20% aroma, 20% emulsifier and 60% carrier. Modified starch or gum arabic was used as emulsifier, and maltodextrins were used as carrier.

[0079] The spray products were subjected to agglomeration with different binder liquids at different concentrations. The binder liquids are listed below:

TABLE-US-00001 Original Lemon Experiment 1 Maltodextrin DE 17-20 10% Experiment 2 Maltodextrin DE 17-20 30% Experiment 3 Maltodextrin DE 8-10 10% Experiment 4 Maltodextrin DE 8-10 30% Experiment 5 Gum arabic Senegal 10% Experiment 6 modified starch 10% Experiment 7 Mannitol 10% Experiment 8 Glucose 10% Experiment 9 Glucose 30% Experiment 10 Ascorbic acid 10% Experiment 11 Pectin amidated 2% Experiment 12 Protein potato 10% Experiment 13 Protein whey 10% Experiment 14 Water Experiment 15 Protein whey 10% acidic, pH 4.5

[0080] DE 17-20 and DE 8-10 are the dextrose equivalents of the maltodextrin used.

[0081] The products were physically characterized and stored for the accelerated storage tests in such a way that the temperature and oxygen partial pressure were increased so that a storage period of one year could be simulated within 12 to 24 hours. Stability was tested after 6 or 12 months of accelerated storage, depending on the shelf life of the liquid flavor. The results are shown in Table 1. Oxipress 12 months and Oxipress 6 months mean that accelerated storage was performed under conditions simulating 12 and 6 months, respectively.

[0082] It can be seen from the results that both the material itself and the concentration in which it was sprayed have an influence on the storage stability. The results can be explained by different spreading behavior and the drying properties of the binder liquids. It is surprising, however, that substances which are actually only applied to bond the particles increase the storage stability more than pure surface reduction (simulated by bonding by means of water or steam) does. This is because the substances do not cover the entire surface of the particles, so they cannot seal them. The physical parameters support the results of the stability test.

TABLE-US-00002 TABLE 1 Physical properties and results of the storage test Particle Particle size size FFC Bulk Residual 0.5 bar 3 bar (flowability) density Dust Oxipress 12 Oxipress 6 moisture D50 D90 D50 D90 FFC g/L value months months Original Lemon FDI 10038 AA 5.00% 69.3 115 46.9 115 10.4 424.3 15.1 Failed Failed Experiment 1 Maltodextrin 17-20 4.40% 103.2 202.9 63.7 147.1 11.7 410.2 11.5 Passed 104966 10% Experiment 2 Maltodextrin 17-20 5.07% 135 407.8 76.9 245 11.5 419.4 9.7 Passed 104966 30% Experiment 3 Maltodextrin 8-10 5.56% 128.8 316.6 77.7 207 11.6 413 10 Passed 10% Experiment 4 Maltodextrin 8-10 5.75% 113.5 235.1 69.2 164.6 11.2 439.4 11.8 Failed Passed 30% Experiment 5 Rubber Senegal 10% 5.31% 138.6 350.3 83.2 228.8 11.3 421.1 8.3 Passed Experiment 6 modified starch 10% 4.61% 127.4 279.2 76.3 172.9 11.2 428.6 8.1 Failed Passed Experiment 7 Mannitol 10% 4.19% 97.9 201.1 58.5 137.5 10.4 449.6 13 Passed Experiment 8 Glucose 107544 10% 4.78% 130.8 287.8 78.4 177.1 11.4 402.6 6.7 Passed Experiment 9 Glucose 107544 30% 4.78% 126.1 495.4 73.4 194.9 12.9 408.2 7.4 Passed Experiment 10 Ascorbic acid 115414 4.01% 114.4 234.2 67.2 153.6 11.5 423.5 13 Failed Passed 10% Experiment 11 Pectin amide 2% 5.04% 159 403.3 97 282.3 11.3 410.7 7.7 Failed Passed Experiment 12 Protein potato 10% 6.20% 129 268.3 75.7 168.5 11.3 390.9 6.6 Passed Experiment 13 Protein whey 10% 3.58% 111.6 208.1 67.8 150 12.8 396.9 6.4 Failed Passed Experiment 14 Water 4.94% 119.1 258.6 71.4 166.5 11.4 391.7 9.7 Passed Experiment 15 Protein whey 10% 4.21% 124.6 268.3 71.9 163.8 13.2 377.9 5.1 Passed acidic

EXAMPLE 2: TEST FOR DIFFERENCE OF SAMPLES

[0083] Because the panelists' descriptions in Example 1 showed strong differences that were not reflected in the “pass, fail” classification, another testing method was used to further tease out the differences.

[0084] The stored samples that passed the test in example 1 were tasted against each other according to the DoD (Degree of difference) test procedure. In order not to overload the panelists, the tests had to be divided up, as no more than 5 samples should be compared at the same time, otherwise the risk of panelist fatigue increases.

[0085] The task of the panelists was to describe the differences of the samples from the standard (STD) using the given terms. To validate the results, the standard was also tasted as a sample. The fresh sample produced by spray drying without agglomeration was used as the standard. Accordingly, a slight difference means that the stored sample is very close to the fresh product, which indicates a good protective effect of the agglomeration carried out by means of the binder substance. The % values given refer to the proportion of panelists who arrived at the respective assessment.

[0086] Tasting was performed with 0.2% of sample on a test solution with sugar and citric acid.

[0087] The result shows that the stored samples [0088] Lemon with binder glucose [0089] Lemon with binder maltodextrin EN 17-20 [0090] Lemon with binder gum/modified starch

[0091] showed a better protective effect than the other binders used for agglomeration.

[0092] The protective effect of the glucose and maltodextrin is possibly due to the reducing effect of the sugar. However, it is surprising that a reducing sugar applied to the outside of the particles has such an effect. In the case of the agglomerate, where a mixture of gum arabic and modified starch was used as a binder, it can be assumed that due to the high interfacial activity of these substances, the binder liquid spreads particularly well and thus leads to an even coating of the particles, accompanied by a sealing. In addition, gum arabic has reducing groups, as can be seen from Example 3, and can thus contribute to oxidation stability.

TABLE-US-00003 TABLE 2 Tasting without binder and with mannitol and glucose as binders very No very Slightly Sharply sharply difference small Small Medium increasing increasing increasing (STD) difference difference difference difference difference difference 237 10% 10% 40% 20% 20% 134 20% 10% 20% 30% 10% 10% 456 10% 30% 60% 890 100% Description of the difference: 237: carvony, more bitter than STD, oxidized but still distinctly citric, bitter note, smells barely citric, smells like toilet stone, slightly bitter, weaker, off, broken. 134: bitter, similar to STD, off, least bad, broken, slightly bitter, slightly citric, slight off notes, less fresh 456: non-tasting, p-methylacetophenone, bitter, artificial, off, completely oxidized, no citron, toilet stone, heavily shabby, very bitter 890: STD STD Lemon SD fresh 237 Lemon Mannitol 134 Lemon Glucose 456 Lemon SD 890 Lemon SD fresh SD = spray dried (spray dried)

TABLE-US-00004 TABLE 3 Tasting without binder and with maltodextrin, glucose and gum/modified starch as binders very No very Slightly Sharply sharply difference small Small Medium increasing increasing increasing (STD) difference difference difference difference difference difference 569 20% 10% 10% 60% 134 10% 20% 30% 10% 30% 862 30% 70% 709 90% 10% 302 20% 20% 30% 30% Description of the difference: 569: clearly oxidized (2x), slightly bitter (2x), slightly rancid, toilet stone 134: oxidized, very bitter 862: worst sample, totally off (2x), shabby, toilet stone 709: standard 302: best sample, slightly oxidized and bitter, slightly bitter notes STD Lemon SD fresh 569 Lemon Maltodextrin De 17-20 134 Lemon Glucose 862 Lemon SD 709 Lemon SD fresh 302 Lemon gum/modified starch

TABLE-US-00005 TABLE 4 Tasting without binder and with maltodextrin, whey and gum/modified starch as binder very No very Slightly Sharply sharply difference small Small Medium increasing increasing increasing (STD) difference difference difference difference difference difference 234 10% 10% 10% 40% 10% 20% 890 50% 20% 20% 10% 410 10% 20% 40% 30% — 622 10% 90% 398 20% 10% 20% 30% 20% Description of the difference: 234: bitter (3x), slightly rancid 890: slightly bitter, standard, odor fresh (STD) 410: bitter (2x), artificial, slightly off, toilet stone 622: slightly menthol, strongly bitter, totally um 398: slightly bitter, slightly rancid STD Lemon SD fresh 234 Lemon Maltodextrin De 17-20 890 Lemon SD fresh 410 Lemon whey 622 Lemon SD 398 Lemon gum/modified starch

EXAMPLE 3: TEST FOR REDUCING PROPERTIES OF GUM ARABIC AND MODIFIED STARCH

[0093] The Folin-Cioltaeu reagent shows a color change from yellow to blue in the presence of reducing groups due to the reaction: Mo(VI)+e->Mo(V).

[0094] For each assay, 500 μl of 10% solution of gum arabic was shaken with +750 μl of Folin-Cioltaeu reagent, 750 μm of 8% Na2CO3 solution was added, shaken again, and then stored for 2 h in cuvettes.

TABLE-US-00006 Absorbance measurement after 2 h at 765 nm 1. 2. Mean Measurement Measurement value Gum arabic (A Seyal lot 32) 0.7684 0.8863 0.83 Gum arabic (Seyal lot 59) 0.8782 0.7754 0.83 Gum arabidum (Senegal lot 55) 0.5964 0.555 0.58 Modified starch (lot 70) 0.28 0.28

[0095] FIG. 6 shows the cuvettes. The darker the coloration of the solution, the stronger the reducing properties of the tested substance. Cuvettes 1 and 2 contain gum arabic (Seyal lot 32), cuvettes 3 and 4 gum arabic (Seyal lot 59), cuvettes 5 and 6 gum arabic (Senegal lot 55) and cuvettes 7 and 8 modified starch (lot 70). Modified starch shows little coloration and therefore contains few reducing groups.