Patent US2657884A successfully refreshed from Google Patents.
US4254100A
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US
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Vitamin A compositions
Assignee: Hoffmann La Roche Inc
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Filing: 1980-03-07
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Granted: 1981-03-03
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Expires: 2000-03-07
Abstract
Abstract Microcrystalline vitamin A acetate dry free-flowing powders containing microcrystalline vitamin A acetate and a process for their preparation are disclosed.
Inventors
- 👤 Hans E. Keller
- 👤 Heinrich Klaeui
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 02:43
CPC Classifications
A; A61; A61K; A61K9/00; A61K9/48; A61K9/50; A61K31/00; A61K31/045; A61K31/07
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
305 words
A process for the preparation of dry, free flowing beadlets containing microcrystalline vitamin A acetate which exhibits excellent vitamin A stability without containing any antioxidants and which comprises (a) homogenizing with sufficient high shear force to obtain particle sizes of from about 0.5μ to about 50μ of molten or wet-milled vitamin A acetate in an aqueous solution containing from about 0.1% to about 5% by weight, based on the weight of the solution, of an edible, water-soluble carrier composition selected from the group consisting of gelatin, gum arabic, pectin, sugar, tragacanth, alginates, guar sperm meal, methylcellulose, sodium carboxymethyl cellulose, modified starch, sodium ascorbyl palmitate, a polyoxyalkylene derivative of sorbitan monostearate, mixtures of glycerol mono- annd di-ricinoleates with polyoxyethylene glycol ether groups and monoricinoleic esters of polyethylene glycol; (b) cooling the resulting emulsion to about 15° C. while continuing the homogenization technique until such particle size ranges are obtained, of completely crystalline vitamin A acetate microcrystals; (c) separating the completely crystallized microcrystalline vitamin A acetate from the liquid medium by centrifugation; (d) adding the microcrystalline vitamin A acetate to a gelatin/sugar solution wherein the ratio of gelatin to sugar is about 3 to 1; (e) heating the resulting mixture to from about 40° to about 50° C. with vigorous stirring to suspend the microcrystals; (f) adding the resulting microcrystal suspension of step (e) to an oil which has been heated to 45° C. using sufficient stirring to form fine droplets; (g) cooling the resultant mixture with stirring to from about 5° to about 15° C. to solidify the droplets; (h) washing the beadlets with a solvent for the oil; (i) separating the beadlets from the suspension medium, and (j) drying the beadlets to thus form dry, free-flowing beadlets containing vitamin A acetate in microcrystalline form and which exhibit excellent vitamin A stability without containing any antioxidants.
Claim 2
Dependent Claim
305 words
A process for the preparation of dry, free flowing beadlets containing microcrystalline vitamin A acetate which exhibits excellent vitamin A stability without containing any antioxidants and which comprises (a) homogenizing with sufficient high shear force to obtain particle sizes of from about 0.5μ to about 50μ of molten or wet-milled vitamin A acetate in an aqueous solution containing from about 0.1% to about 5% by weight, based on the weight of the solution, of an edible, water-soluble carrier composition selected from the group consisting of gelatin, gum arabic, pectin, sugar, tragacanth, alginates, guar sperm meal, methylcellulose, sodium carboxymethyl cellulose, modified starch, sodium ascorbyl palmitate, a polyoxyalkylene derivative of sorbitan monostearate, mixtures of glycerol mono- annd di-ricinoleates with polyoxyethylene glycol ether groups and monoricinoleic esters of polyethylene glycol; (b) cooling the resulting emulsion to about 15° C. while continuing the homogenization technique until such particle size ranges are obtained, of completely crystalline vitamin A acetate microcrystals; (c) separating the completely crystallized microcrystalline vitamin A acetate from the liquid medium by centrifugation; (d) adding the microcrystalline vitamin A acetate to a gelatin/sugar solution wherein the ratio of gelatin to sugar is about 3 to 1; (e) heating the resulting mixture to from about 40° to about 50° C. with vigorous stirring to suspend the microcrystals; (f) adding the resulting microcrystal suspension of step (e) to an oil which has been heated to 45° C. using sufficient stirring to form fine droplets; (g) cooling the resultant mixture with stirring to from about 5° to about 15° C. to solidify the droplets; (h) washing the beadlets with a solvent for the oil; (i) separating the beadlets from the suspension medium, and (j) drying the beadlets to thus form dry, free-flowing beadlets containing vitamin A acetate in microcrystalline form and which exhibit excellent vitamin A stability without containing any antioxidants.
Claim 3
Dependent Claim
38 words
A dry free-flowing vitamin A powder composition which exhibits excellent vitamin A stability without containing any antioxidants and which comprises microcrystalline vitamin A acetate coated with an edible, water-soluble carrier composition produced by the process of claim 1.
Claim 4
Dependent Claim
136 words
A process for the preparation of microcrystalline vitamin A acetate which comprises (a) homogenizing with sufficient high shear force to obtain particle sizes of from about 0.5μ to about 0.5μ of molten or wet-milled vitamin A acetate in water or an aqueous solution containing from about 0.1% to about 5% by weight, based on the weight of the solution, of an edible, water-soluble carrier composition selected from the group consisting of gelatin, gum arabic, pectin, agar, tragacanth, alginates, guar sperm meal, methylcellulose, sodium carboxymethyl cellulose, modified starch, sodium ascorbyl palmitate, a polyoxyalkylene derivative of sorbitan monosterate, mixtures of glycerol mono- and di-ricinoleates with polyoxyethylene glycol ether groups and monoricinoleic esters of polyethylene glycol, and (b) cooling the resulting emulsion to about 15° C. while continuing the homonegization technique to thus obtain microcrystals of vitamin A acetate.
Claim 5
Dependent Claim
136 words
A process for the preparation of microcrystalline vitamin A acetate which comprises (a) homogenizing with sufficient high shear force to obtain particle sizes of from about 0.5μ to about 0.5μ of molten or wet-milled vitamin A acetate in water or an aqueous solution containing from about 0.1% to about 5% by weight, based on the weight of the solution, of an edible, water-soluble carrier composition selected from the group consisting of gelatin, gum arabic, pectin, agar, tragacanth, alginates, guar sperm meal, methylcellulose, sodium carboxymethyl cellulose, modified starch, sodium ascorbyl palmitate, a polyoxyalkylene derivative of sorbitan monosterate, mixtures of glycerol mono- and di-ricinoleates with polyoxyethylene glycol ether groups and monoricinoleic esters of polyethylene glycol, and (b) cooling the resulting emulsion to about 15° C. while continuing the homonegization technique to thus obtain microcrystals of vitamin A acetate.
Claim 6
Dependent Claim
13 words
The process of claim 3 wherein the edible water-soluble carrier material is gelatin.
Claim 7
Dependent Claim
24 words
The process of claim 3 wherein the vitamin A acetate, after homogenization, has a particle size range of from about 0.5μ to about 50μ.
Claim 8
Dependent Claim
24 words
The process of claim 3 wherein the vitamin A acetate, after homogenization, has a particle size range of from about 1μ to about 25μ.
Claim 9
Dependent Claim
18 words
The dry, free-flowing vitamin A powder composition of claim 2 wherein the edible water-soluble carrier composition is gelatin.
Claim 10
Dependent Claim
13 words
The process of claim 1 wherein the edible, water-soluble carrier composition is gelatin.
Claim 11
Dependent Claim
24 words
The process of claim 1 wherein the vitamin A acetate, after homogenization, has a particle size range of from about 0.5μ to about 50μ.
Claim 12
Dependent Claim
24 words
The process of claim 9 wherein the vitamin A acetate, after homogenization, has a particle size range of from about 1μ to about 25μ.
Claim 13
Dependent Claim
19 words
Dry, free-flowing vitamin A beadlets which comprise the vitamin A powder composition of claim 2 within a gelatin/sugar coating.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-03-02 | 1984-09-01 | 1985-03-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-03-02 | 1988-09-01 | 1989-03-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-03-02 | 1992-09-01 | 1993-03-03 | $7700.00 | Window Closed / Lapsed |