Drug – bio-affecting and body treating compositions – Preparations characterized by special physical form – Particulate form
Reexamination Certificate
1999-09-24
2001-12-11
Page, Thurman K. (Department: 1615)
Drug, bio-affecting and body treating compositions
Preparations characterized by special physical form
Particulate form
C424S499000, C514S725000, C514S458000, C514S474000
Reexamination Certificate
active
06328995
ABSTRACT:
Stable vitamin and/or carotenoid products in powder form and process for their production.
The invention relates to stable vitamin and/or carotenoid products in powder form and to a process for their preparation.
Vitamin and carotenoid products in powder form are generally known and are used on a large scale in the pharmaceutical industry and in animal feed and human food industries. Thus, many processes for producing suitable products are described in the literature.
As a rule, the lipid-soluble vitamins and/or carotenoids are dispersed in an aqueous solution of an organic film-forming colloid and the resulting dispersion is finally converted into dry products in powder form.
Gelatin is normally used as film-forming colloid in the prior art.
The stability of products of this type must meet particularly high demands when they are intended to be used as additives to human foods or animal feeds because in this use they are exposed to a high variety of effects such as elevated temperatures, humidity, mechanical friction or pressure which are extremely harmful for the sensitive vitamins and carotenoids. There has thus been no lack of attempts to develop processes providing particularly thermally and mechanically stable products.
Thus, for example, GB 993 138 discloses the stabilization of gelatin-containing vitamin products, the particles being treated with a gelatin-denaturing agent such as formaldehyde, glyoxal, acetaldehyde or dihydroxyacetone, and then being heated or else only subjected to a heat treatment.
EP-B-0 285 682 discloses a process for producing spherical products which contain lipid-soluble vitamins, by forming an emulsion using water, gelatin and a sugar, converting the emulsion into droplets, collecting the droplets in a starch powder composition in such a way that the droplets remain separated from one another until better shape has been permanently formed, separating the resulting particles from excess starch powder and then treating with heat at temperatures of from 90 to 180° C.
In addition, EP-A-0 494 417 describes a process for crosslinking gelatin in the presence of a reducing sugar and of a water-soluble salt of a carboxylic acid or of an inorganic acid at temperatures in the range from 55 to 180° C.
However, the abovementioned processes have the disadvantage that the required crosslinking times are often too long or the crosslinking temperatures are too high so that there may be damage to the thermally unstable lipid-soluble vitamins or carotenoids in the product.
It is an object of the present invention to provide a process for producing stable vitamin and/or carotenoid products in powder form which do not have the abovementioned disadvantages.
We have found that this object is achieved by a process for producing stable dry powders which are insoluble in hot water and which contain one or more lipid-soluble vitamins and/or one or more carotenoids, which comprises the following process steps:
A. preparation of an aqueous dispersion containing:
a1) 2 to 50% by weight of at least one protein,
a2) 1 to 30% by weight of at least one sugar,
a3) 0.2 to 20% by weight of at least one inorganic salt,
a4) 0.1 to 20% by weight of at least one lipid-soluble vitamin and/or at least one carotenoid,
a5) 5 to 95% by weight of water,
where all the % by weight data are based on the total weight of the aqueous dispersion, and the total of the percentage data for the individual components a1) to a5) is 100%,
B. converting this dispersion into a dry powder and
C. heating the dry powder to a temperature in the range from 55° C. to 180° C.,
wherein alkali metal phosphates are used as inorganic salt a3), so that the protein is crosslinked to an extent such that the dry powder is insoluble in water for at least 3 minutes after introduction into water at 100° C.
The proteins a1) employed as protective colloid in the preparation of the aqueous dispersion in process step (A) may be both of vegetable and of animal origin. Examples which may be mentioned are, in particular, gelatin, inter alia bone gelatin, bovine gelatin, fish gelatin, in each case of the A and B type in a wide bloom range, and pectin, casein or caseinate, soyabean proteins and corn proteins. The gelatins preferably used have a bloom value of from 50 to 300, particularly preferably from 80 to 150. The protective colloid is generally used in amounts of about 2 to 50% by weight, preferably 3 to 25% by weight, particularly preferably 5 to 15% by weight, based on the total weight of the aqueous dispersion.
It is possible to use as component a2) all reducing sugars or sugar syrups containing reducing sugars. Reducing sugars include fructose, glucose, lactose, maltose, xylose, arabinose, ribose and sucrose, and honey and fructose and glucose syrups.
Sugars preferably used for the purpose of the invention are fructose, glucose and sucrose and mixtures thereof. Glucose and/or fructose are particularly preferred sugars. The sugars are generally used in amounts of about 1 to 30% by weight, preferably 2 to 20% by weight, particularly preferably 3 to 15% by weight, based on the total weight of the aqueous dispersion.
The lipid-soluble vitamins of component a4) include vitamins A, E, D and K, including derivatives thereof, for example vitamin A esters such as vitamin A acetate, vitamin A propionate or vitamin A palmitate, and vitamin E esters such as tocopheryl acetate. For the purpose of the invention they can be employed in the form of vitamin solutions in oils, as provitamins and as pure vitamins of natural or synthetic origin. Vitamin A and its derivatives are of particular interest, particularly preferably vitamin A acetate, vitamin A propionate and vitamin A palmitate and mixtures thereof, very particularly preferably vitamin A acetate.
Carotenoids are understood as meaning compounds such as &bgr;-carotene, lycopine, bixine, zeaxanthine, citranaxanthine, canthaxanthine, astaxanthine, lutein, capsanthin, cryptoxanthine, &bgr;-apo-8′-carotenoic acid and its esters, &bgr;-apo-8′-carotenal, &bgr;-apo-12′-carotenal and mixtures thereof. Preferred carotenoids are &bgr;-carotene, lycopine, lutein, zeaxanthine, canthaxanthine and astaxanthine.
The contents of vitamins and/or carotenoids are generally from 0.1 to 20% by weight, preferably 1 to 15% by weight, particularly preferably 2 to 12% by weight, based on the total weight of the aqueous dispersion obtainable by process step (A).
According to the invention at least one alkali metal phosphate is employed as inorganic salt a3) for preparing the abovementioned aqueous dispersion. Possible examples thereof are sodium, potassium or lithium salts both of mono-, di- and triphosphoric acids and of polyphosphoric acid.
Preferred alkali metal phosphates are tertiary sodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, disodium dihydrogen diphosphate, pentasodium triphosphate, sodium trimethaphosphate [sic], tertiary potassium phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, dipotassium hydrogen diphosphate, pentapotassium triphosphate, potassium trimethaphosphate [sic]. Tertiary sodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, tertiary potassium phosphate, potassium dihydrogen phosphate and dipotassium hydrogen phosphate are particularly preferred. Disodium hydrogen phosphate is very particularly preferred.
The contents of alkali metal phosphate are generally from 0.2 to 20% by weight, preferably 0.3 to 15% by weight, particularly preferably 0.4 to 10% by weight, very particularly preferably 0.5 to 5% by weight, based on the total weight of the aqueous dispersion obtainable by process step (A).
In addition to the abovementioned constituents, it is possible and advantageous to add to the dispersion other auxiliaries and additives customary for producing dry powders of active substances.
Particularly important for use of the dry powders as animal feed additive when the active substances are sensitive to oxidation is addition of antioxidants such as ethoxyquin, butylated hydrox
Betz Roland
Bewert Wolfgang
Bower David Kenneth
Chaundy Frederick Kenneth
Schmitt Peter
BASF - Aktiengesellschaft
Keil & Weinkauf
Page Thurman K.
Pulliam Amy E
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