US3855712A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of preparation of pharmaceutical products
Assignee: Cephalon France SAS
•
Filing: 1974-04-02
•
Granted: 1974-12-24
•
Expires: 1994-04-02
Abstract
Abstract The use of organic solvents having an evaporation rate, as compared with ether, of not more than 50 times has been formed to afford considerable handling and production advantages in the preparation of pharmaceutical products made from lyophilised pharmaceutical compositions and water-soluble or waterdispersible polymeric binders; the products are made by forming a paste from the pharmaceutical compositions, the polymeric binder and the organic solvent, solidifying the paste at a temperature of -15* to -50*C. and then lyophilising the frozen material under vacuum. This technique is especially desirable as it enables lyophilised products to be made which contain a water-activated effervescent couple.
Inventors
- 👤 P Blonde
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 15:12
CPC Classifications
A; A61; A61K; A61K9/00; A61K9/0002; A61K9/0007; A61K9/14; A61K9/19
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
104 words
A PROCESS OF PREPARING OF A DEHYDRATED OR DESOLVATED PHARMACEUTICAL PRODUCT BY LYOPHILISATION, WHICH COMPRISES THE STEPS OF: I. COMBINING WITH A PHARMACEUTICAL COMPOSITION TO BE LYOPHILISED A. A POLYMER BINDER SELECTED FROM THE GROUP CONSISTING OF POLYMERIC COMPOUNDS WHICH ARE SOLUBLE IN WATER AND POLYMERIC COMPOUNDS CAPABLE OF GIVING COLLODIAL SOLUTIONS IN WATER; AND B. AN ORGANIC SOLVENT FOR THE BINDER HAVING A SPEED OF EVAPORATION LESS THAN 500 TIMES THAT OF ETHER; II. SOLIDIFYING THE PASTE TO OBTAINED AT A TEMPERATURE IN THE RANGE OF -150* TO -50*C; AND III. SUBJECTING THE RESULTANT FROZEN MATERIAL TO A PROCESS OF LYOPHILISATION UNDER VACUUM.
Claim 2
Dependent Claim
104 words
A PROCESS OF PREPARING OF A DEHYDRATED OR DESOLVATED PHARMACEUTICAL PRODUCT BY LYOPHILISATION, WHICH COMPRISES THE STEPS OF: I. COMBINING WITH A PHARMACEUTICAL COMPOSITION TO BE LYOPHILISED A. A POLYMER BINDER SELECTED FROM THE GROUP CONSISTING OF POLYMERIC COMPOUNDS WHICH ARE SOLUBLE IN WATER AND POLYMERIC COMPOUNDS CAPABLE OF GIVING COLLODIAL SOLUTIONS IN WATER; AND B. AN ORGANIC SOLVENT FOR THE BINDER HAVING A SPEED OF EVAPORATION LESS THAN 500 TIMES THAT OF ETHER; II. SOLIDIFYING THE PASTE TO OBTAINED AT A TEMPERATURE IN THE RANGE OF -150* TO -50*C; AND III. SUBJECTING THE RESULTANT FROZEN MATERIAL TO A PROCESS OF LYOPHILISATION UNDER VACUUM.
Claim 3
Dependent Claim
25 words
The process of claim 1, in which the organic solvent has a speed of evaporation less than or equal to 10 times that of ether.
Claim 4
Dependent Claim
29 words
The process of claim 1, in which the organic solvent is selected from the group consisting of dioxane, carbon tetrachloride, chloroform, benzene, cyclohexane, dimethylamine, dimethylsulphoxide, tertiary butanol and diethylaminoethanol.
Claim 5
Dependent Claim
50 words
The process of claim 1, in which the polymeric binder is selected from the group consisting of polyvinylpyrrolidone, copolymers of polyvinylpyrrolidone and polyvinyl alcohols, polyvinyl alcohols, carboxypolymethylenes, polyethylene glycols, copolymers of maleic anhydride and polyvinylmethylether, copolymers of polyethylene and maleic anhydride and block copolymers of ethylene oxide and propylene oxide.
Claim 6
Dependent Claim
38 words
The process of claim 1, in which at least one lyophilisation additive selected from the group consisting of lactose, saccharose, glucose, xylose, levulose, glycocol, sorbitol, mannitol, starch and sodium saccharinate is included in the composition of step (i).
Claim 7
Dependent Claim
29 words
The process of claim 1, in which the organic solvent is employed in a proportion of 5 percent to 75 percent by weight with respect to the dry mixture.
Claim 8
Dependent Claim
26 words
The process of claim 1, in which the binder is employed in an amount up to 10 percent by weight with respect to the dry mixture.
Claim 9
Dependent Claim
55 words
The process of claim 1, in which a dry mixture is prepared by combining the pharmaceutical composition with the polymeric binder (a) and optionally at least one lyophilisation additive, the dry mixture is rendered into a paste with the organic solvent (b), the paste so obtained is frozen and the frozen material is then lyophilised.
Claim 10
Dependent Claim
17 words
The process of claim 8, in which at least one lyophilisation additive in included in the mixture.
Claim 11
Dependent Claim
116 words
The process of claim 1, in which a dry mixture is prepared from the pharmaceutical composition and, optionally, either or both of at least one lyophilisation additive and a part of the binder (a), a solution of 0.1 to 10 percent by weight of the binder or the rest of the binder in the organic solvent is separately prepared, the solution is added to the dry mixture to form a paste in the proportion of 5 percent to 75 percent of the solvent with respect to the total weight of the dry mixture, the paste is admixed in a homogenous manner, the paste so obtained is then frozen and the frozen material is lyophilised under vacuum.
Claim 12
Dependent Claim
17 words
The process of claim 10, in which at least one lyophilisation additive is included in the mixture.
Claim 13
Dependent Claim
14 words
The process of claim 8, in which the pharmaceutical composition contains an effervescent mixture.
Claim 14
Dependent Claim
19 words
The process of claim 12, in which the effervescent mixture comprises an organic acid and a weak mineral base.
Claim 15
Dependent Claim
46 words
The process of claim 13, in which the organic acid is selected from the group consisting of citric acid, tartaric acid and ascorbic acid and the weak mineral base is selected from the group consisting of the alkali metal and alkaline earth metal carbonates and bicarbonates.
Claim 16
Dependent Claim
37 words
The process of claim 1, in which the pharmaceutical composition is combined with polyvinyl pyrrolidone, the resultant dry mixture is made into a paste with tertiary butanol, the paste is frozen and the frozen material is lyophilised.
Claim 17
Dependent Claim
66 words
The process of claim 1, in which the pharmaceutical composition is combined with a polymeric binder selected from the group consisting of polyethylene glycols and block polymers of ethylene oxide and propylene oxide, the resultant dry mixture is made into a paste with an organic solvent selected from the group consisting of tertiary butanol and dioxane, the paste is frozen and the frozen material is lyophilised.
Claim 18
Dependent Claim
71 words
A process of preparation of a desolvated pharmaceutical product, which comprises the steps of: i. combining a pharmaceutical composition with: a. polyvinylpyrrolidone; b. tertiary butanol; c. citric acid; d. mono potassium citrate; e. mono sodium citrate; and f. optionally sodium bicarbonate; ii. solidifying the resultant paste at a temperature in the range of -15* to -50*C; and iii. subjecting the frozen material so obtained to a process of lyophilisation under vacuum.
Claim 19
Dependent Claim
71 words
A process of preparation of a desolvated pharmaceutical product, which comprises the steps of: i. combining a pharmaceutical composition with: a. polyvinylpyrrolidone; b. tertiary butanol; c. citric acid; d. mono potassium citrate; e. mono sodium citrate; and f. optionally sodium bicarbonate; ii. solidifying the resultant paste at a temperature in the range of -15* to -50*C; and iii. subjecting the frozen material so obtained to a process of lyophilisation under vacuum.
References Cited (Backward Citations)
US27583A
Cited
US3397462A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1977-12-23 | 1978-06-24 | 1978-12-24 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-12-23 | 1982-06-24 | 1982-12-24 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-12-23 | 1986-06-24 | 1986-12-24 | $7700.00 | Window Closed / Lapsed |