VIBRATION DROPLET FORMATION

Abstract

The present invention relates to a method for producing particles containing carotenoid and/or vitamin and/or omega-3 fatty acids and/or phytosterols and/or conjugated linoleic acids, having a narrow particle size distribution and uniform spherical shape and density, and also to particles obtainable by this method and use thereof as food supplements, foodstuffs, feedstuffs, body care products and medicaments. The particles according to the invention exhibit improved storage stability compared to the prior art.

Claims

1.-18. (canceled)

19. A method for producing spherical particles containing carotenoid and/or vitamin and/or omega-3 fatty acids and/or phytosterols and/or conjugated linoleic acids, wherein carotenoid and/or vitamin and/or omega-3 fatty acids and/or phytosterols and/or conjugated linoleic acids are dispersed in a solution comprising at least one hydrocolloid and droplets are produced from the dispersion formed by means of a nozzle, wherein the dispersion droplets are generated by vibrational excitation and the droplets are solidified and dried by evaporation of the solvent.

20. The method according to claim 19, wherein the nozzle and/or the dispersion and/or a reservoir vessel containing the dispersion and/or a feed line supplying the dispersion to the nozzle are excited by vibrations.

21. The method according to claim 19, wherein the vibrational excitation is a superimposed frequency of vibration in the range from 50 to 10 000 Hz.

22. The method according to claim 19, wherein the dispersion to be dropletized has a viscosity of 80 mPas at 40 C.

23. The method according to claim 19, wherein carotenoids and/or vitamins and/or omega-3 fatty acids and/or phytosterols and/or conjugated linoleic acids are homogeneously distributed in the hydrocolloid matrix of the particle.

24. The method according to claim 19, wherein the cavity volume enclosed in the particles is 40% of the total volume of the particles.

25. The method according to claim 19, wherein the particles have a particle size distribution greater than 75% in the range from 150 to 600 m.

26. The method according to claim 19, wherein the polydispersity, measured as X90X10 divided by X50, is less than 1.0.

27. The method according to claim 19, wherein the hydrocolloid is selected from the group consisting of plant gums, modified plant gums, gelatine, modified gelatine, modified starch, lignosulfonate, chitosan, carrageenan, casein, caseinate, whey protein, zein, modified cellulose, pectin, modified pectin, plant proteins and modified plant proteins and mixtures thereof.

28. The method according to claim 19, wherein the carotenoid and/or vitamin and/or omega-3 fatty acids and/or phytosterols and/or conjugated linoleic acids is selected from the group consisting of vitamins A, D, E, K, derivatives thereof, and mixtures thereof.

29. The method according to claim 19, wherein the dispersion to be dropletized comprises at least one antioxidant selected from the group consisting of dl--tocopherol, d--tocopherol, -tocopherol, -tocopherol, -tocopherol, butylhydroxytoluene (BHT), butylhydroxyanisole, propyl gallate, octyl gallate, dodecyl gallate, extracts of rosemary, extracts of green tea and other gallic acid derivatives, tert-butylhydroxyquinoline, ethoxyquin, carnosol, carnosic acid, ascorbyl palmitate and ascorbyl stearate and mixtures thereof.

30. The method according to claim 19, wherein the dispersion to be dropletized comprises an oil selected from the group consisting of sesame oil, corn germ oil, cottonseed oil, soybean oil, peanut oil, sunflower oil, rapeseed oil, coconut oil, palm oil, olive oil and animal fats, lard and tallow, modified oils and mixtures thereof.

31. The method according to claim 19, wherein the dispersion to be dropletized comprises at least one softener selected from sugars or sugar alcohols.

32. The method according to claim 19, wherein the droplets generated by vibrational excitation are coated with a powdering agent and are subsequently solidified and dried.

33. The method according to claim 19, wherein the droplets generated are coated with a powdering agent at temperatures between 10 and 80 C. and are subsequently solidified and dried at feed air temperatures between 40 and 20 C.

34. The method according to claim 32, wherein the powdering agent is selected from the group consisting of hydrophobic silica, hydrophilic silica, starch, modified starch, corn starch, celluloses, modified celluloses, calcium silicate, calcium-magnesium silicate, calcium carbonate, tricalcium phosphate, calcium adipate, magnesium adipate, titanium dioxide, lignins, highly dispersed pectin, modified pectin, plant proteins, modified plant proteins and combinations of these.

35. A preparation form obtained by the method according to claim 19.

36. A food supplement, foodstuff, feedstuff, body care product, or medicament comprising the preparation form according to claim 35.

37. The method according to claim 19, wherein the vibrational excitation is a superimposed frequency of vibration in the range from 100 to 5000 Hz.

38. The method according to claim 19, wherein the vibrational excitation is a superimposed frequency of vibration in the range from 400 to 4000 Hz.

Description

FIGURES

[0032] FIG. 1: Scanning electron micrograph of the particles produced according to 1A

[0033] FIG. 2: Scanning electron micrograph of the particles produced according to 1B

[0034] FIG. 3: Particle size distribution of experiments 1A and 1B

[0035] In the examples below, the preparation of the particles according to the invention is explained in more detail.

NON-INVENTIVE EXAMPLE 1A

[0036] 30 g of canthaxanthin are suspended in 240 g of isopropanol together with 0.6 g of ascorbyl palmitate and 8 g of ethoxyquin and, on setting the pressure limiting valve to 30 bar, mixed continuously with 390 g of isopropanol in a mixing chamber A. At a metering rate of 6 l/h on the suspension side and of 9 l/h on the solvent side, a mixing temperature of 170 C. is set in the mixing chamber A. After a residence time of 0.3 seconds, the molecularly disperse solution is mixed in mixing chamber B with a solution of 32 g of gelatine and 120 g of glucose syrup in 4000 g of water at a flow rate of 100 I/h of isopropanol. After removal of the solvent under reduced pressure in a distillation apparatus, an active ingredient dispersion is obtained which can be converted by spray drying to a stable, water-soluble dry powder. After dissolution in water, a particle size of 150 nm is measured. The emulsion thus prepared was sprayed into a spray tower via a nozzle at 25 bar in which hydrophobic silica was fluidized at 60 C. The still moist particles were further dried at 60 C. air inlet temperature in the underlying fluidized bed for 5h. A broad particle size distribution (FIG. 3) was determined for the particles with a maximum at ca. 500 m, associated with a high proportion of cavities, based on the total volume of the particles.

Determination of the Proportion of Hollow Spheres in Example 1A

[0037] 4 ml of the particles produced were charged in a 15 ml centrifuge tube. n-Pentane was then added to the tube until a volume of 12 ml had been reached. The tube was sealed and shaken until the particles had been completely stirred up from the bottom. The tube was then placed in an upright position and the measurement was assessed after 5 minutes.

[0038] The amount of hollow spheres was read off a mm scale and specified in millimeters.

[0039] For example 1A, a mean value of 6.2 mm was measured in a triplicate determination.

INVENTIVE EXAMPLE 1B

[0040] Example 1B was carried out analogously to Example 1A with the difference that a vibration nozzle was used at a pressure of 0.5 bar. The device used was a Buchi Encapsulator B-390 with a 200 m nozzle opening at a frequency of 1400 Hz. The flow rate achieved through a nozzle was 30 g per hour. A narrow particle size distribution (FIG. 3) was determined for the particles with a maximum at ca. 400 m, associated with a very low proportion of cavities, based on the total volume of the particles.

Determination of the Proportion of Hollow Spheres in Example 1B

[0041] The amount of hollow spheres of example 1B was determined according to the experimental method of example 1A.

[0042] For example 1B, a mean value of 0 mm was measured in a triplicate determination.

Stability Test for Canthaxanthin The stability of the particles thus produced was tested in a premix stress test. For this purpose, test specimens of 25 mg of the particles produced in each case and 4 g of premixed mixture was weighed into 50 ml glass bottles. The premixed mixture consisted of 20% wheat semolina bran, 20% of 50% choline chloride supported on silica and 10% trace element mixture. The trace element mixture consisted of 46.78% FeSO.sub.4x7H.sub.2O, 37.43% CuSO4x5H.sub.2O, 11.79% ZnO, 3.61% MnO and 0.39% CoCO.sub.3. After addition of all ingredients, the test specimens were carefully mixed by hand. These test specimens were stored in a climate chamber at 40 C. and 70% for 4 weeks. Prior to commencement of the storage and after completion of the storage, the canthaxanthin content of the test specimens was determined. From the ratio of the canthaxanthin contents after and prior to storage, the retention was calculated.

[0043] The retention values of the examples are compiled in the table which follows.

TABLE-US-00001 Name Retention (%) 1A 25 1B 86

[0044] The higher the retention, the better the stability of the particles or preparation thereof. If the stability of the particles of the inventive example is compared to the corresponding non-inventive example, the improvement in the stability is clearly apparent.