Prednisolone Hemisuccinate
;)
Pregna-1,4-diene-3,20-dione,21-(3-carboxy-1-oxopropoxy)-11,17-dihydroxy-,(11b)-.
11b,17,21-Trihydroxypregna-1,4-diene-3,20-dione 21-(hydrogen succinate) [2920-86-7].
»Prednisolone Hemisuccinate contains not less than 98.0percent and not more than 102.0percent of C25H32O8,calculated on the dried basis.
Packaging and storage—
Preserve in tight containers.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Ultraviolet Absorption á197Uñ—
Solution:
20µg per mL.
Medium:
methanol.
Absorptivities at 243nm,calculated on the dried basis,do not differ by more than 3.0%.
Specific rotation á781Sñ:
between +99
and +104.
and +104.
Test solution:
6.7mg per mL,in dioxane.
Loss on drying á731ñ—
Dry it in vacuum at 65for 3hours:it loses not more than 0.5%of its weight.
for 3hours:it loses not more than 0.5%of its weight.
Residue on ignition á281ñ:
negligible,from 100mg.
Assay—
Standard preparation—
Dissolve an accurately weighed quantity of USP Prednisolone Hemisuccinate RSin a mixture of equal volumes of alcohol and chloroform to obtain a solution having a known concentration of about 8mg per mL.
Assay preparation—
Weigh accurately about 80mg of Prednisolone Hemisuccinate,previously dried,dissolve in a mixture of equal volumes of alcohol and chloroform to make 10.0mL,and mix.
Procedure—
Use a 20-×20-cm chromatographic plate coated with a 0.25-mm layer of chromatographic silica gel mixture,which has been activated by heating at 105for 1hour.Using a solvent system consisting of a mixture of 5parts of butyl alcohol,4parts of acetic acid,and 1part of water,proceed as directed for Procedureunder Single-steroid Assay á511ñ,ending with “Centrifuge the tubes for 5minutes,”except to apply 50µLin place of 200µLof the solutions to the plate.Concomitantly determine the absorbances of the solutions in 1-cm cells at the wavelength of maximum absorbance at about 243nm,with a suitable spectrophotometer,against the blank.Calculate the quantity,in mg,of C25H32O8in the portion of Prednisolone Hemisuccinate taken by the formula:
for 1hour.Using a solvent system consisting of a mixture of 5parts of butyl alcohol,4parts of acetic acid,and 1part of water,proceed as directed for Procedureunder Single-steroid Assay á511ñ,ending with “Centrifuge the tubes for 5minutes,”except to apply 50µLin place of 200µLof the solutions to the plate.Concomitantly determine the absorbances of the solutions in 1-cm cells at the wavelength of maximum absorbance at about 243nm,with a suitable spectrophotometer,against the blank.Calculate the quantity,in mg,of C25H32O8in the portion of Prednisolone Hemisuccinate taken by the formula:
10C(AU/AS),
in which Cis the concentration,in mg per mL,of USP Prednisolone Hemisuccinate RSin the Standard preparation,and AUand ASare the absorbances of the solutions from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information—
Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 1612
Phone Number:1-301-816-8139