Methylprednisolone Sodium Succinate
C26H33NaO8
496.53
Pregna-1,4-diene-3,20-dione,21-(3-carboxy-1-oxopropoxy)-11,17-dihydroxy-6-methyl-,monosodium salt,(6a,11b)-.
11b,17,21-Trihydroxy-6a-methylpregna-1,4-diene-3,20-dione 21-(sodium succinate) [2375-03-3].
»Methylprednisolone Sodium Succinate contains not less than 97.0percent and not more than 103.0percent of C26H33NaO8,calculated on the dried basis.
Packaging and storage—
Preserve in tight,light-resistant containers.
Identification—
A:
Transfer about 100mg to a separator,dissolve in 10mLof water,add 1mLof 3Nhydrochloric acid,and extract immediately with 50mLof chloroform.Filter the chloroform extract through cotton,evaporate on a steam bath to dryness,and dry in vacuum at 60
for 3hours:the IRabsorption spectrum of a mineral oil dispersion of the residue so obtained exhibits maxima only at the same wavelengths as that of a similar preparation of USP Methylprednisolone Hemisuccinate RS.
for 3hours:the IRabsorption spectrum of a mineral oil dispersion of the residue so obtained exhibits maxima only at the same wavelengths as that of a similar preparation of USP Methylprednisolone Hemisuccinate RS.
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%.
C:
It responds to the flame test for Sodium á191ñ.
Specific rotation á781Sñ:
between +96and +104.
and +104.
Test solution:
10mg per mL,in alcohol.
Loss on drying á731ñ—
Dry it at 105for 3hours:it loses not more than 3.0%of its weight.
for 3hours:it loses not more than 3.0%of its weight.
Sodium content—
Dissolve,with gentle heating,about 1g of it,accurately weighed,in 75mLof glacial acetic acid.Add 20mLof dioxane,then add 1drop of crystal violet TS,and titrate with 0.1Nperchloric acid VSto a blue-green endpoint.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 2.299mg of Na.Not less than 4.49%and not more than 4.77%,calculated on the dried basis,is found.
Assay—
Standard preparation—
Proceed as directed under Assay for Steroids á351ñ,using USP Methylprednisolone Hemisuccinate RSto obtain a solution having a known concentration of about 12.5µg per mL.
Assay preparation—
Weigh accurately about 100mg of Methylprednisolone Sodium Succinate,dissolve it in alcohol to make 200.0mL,and mix.Pipet 5mLof this solution into a 200-mLvolumetric flask,add alcohol to volume,and mix.Pipet 20mLof the resulting solution into a glass-stoppered,50-mLconical flask.
Procedure—
To each of the flasks containing the Assay preparationand the Standard preparation,and to a similar flask containing 20.0mLof alcohol,to provide the blank,add 2.0mLof a solution prepared by dissolving 50mg of blue tetrazolium in 10mLof alcohol,and mix.Then to each flask add 4.0mLof a mixture of 1volume of tetramethylammonium hydroxide TSand 9volumes of alcohol.Mix,allow to stand in the dark for 90minutes,add 1.0mLof glacial acetic acid,mix,and proceed as directed for Procedureunder Assay for Steroids á351ñ,beginning with “Concomitantly determine the absorbances.”Calculate the quantity,in mg,of C26H33NaO8in the portion of Methylprednisolone Sodium Succinate taken by the formula:
8.37C(AU/AS).
Auxiliary Information—
Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA1)Pharmaceutical Analysis 1
USP28–NF23Page 1271
Phone Number:1-301-816-8139