Codeine Sulfate
(C18H21NO3)2·H2SO4·3H2O
750.85
Morphinan-6-ol,7,8-didehydro-4,5-epoxy-3-methoxy-17-methyl-,(5a,6a)-,sulfate (2:1)(salt),trihydrate.
7,8-Didehydro-4,5a-epoxy-3-methoxy-17-methylmorphinan-6a-ol sulfate (2:1)(salt)trihydrate [6854-40-6].
Anhydrous 696.82 [1420-53-7].
»Codeine Sulfate,dried at 105
for 3hours,contains not less than 98.5percent and not more than 100.5percent of (C18H21NO3)2·H2SO4.
for 3hours,contains not less than 98.5percent and not more than 100.5percent of (C18H21NO3)2·H2SO4.
Packaging and storage—
Preserve in tight,light-resistant containers.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Ultraviolet Absorption á197Uñ—
Solution:
100µg per mL.
Medium:
water.
Absorptivities at 284nm,calculated on the dried basis,do not differ by more than 3.0%.
C:
It responds to the tests for Sulfate á191ñ.
Specific rotation á781Sñ:
between -112.5and -115.0.
and -115.0.
Test solution:
20mg per mL,in water.
Acidity—
Dissolve 500mg in 15mLof water,add 1drop of methyl red TS,and titrate with 0.020Nsodium hydroxide:not more than 0.30mLis required for neutralization.
Water,Method IIIá921ñ—
Dry about 500mg,accurately weighed,at 105for 3hours:it loses between 6.0%and 7.5%of its weight.
for 3hours:it loses between 6.0%and 7.5%of its weight.
Readily carbonizable substances á271ñ—
Dissolve 10mg in 5mLof sulfuric acid TS:the solution has no more color than Matching Fluid S.
Residue on ignition á281ñ:
not more than 0.1%.
Limit of morphine—
Dissolve about 50mg of potassium ferricyanide in 10mLof water,and add 1drop of ferric chloride TSand 1mLof a solution of Codeine Sulfate (1in 100):no blue color is produced immediately.
Chromatographic purity—
Using Codeine Sulfate,proceed as directed in the test for Chromatographic purityunder Codeine,except to use a mixture of 0.01Nhydrochloric acid and dehydrated alcohol (4:1),instead of dehydrated alcohol,to prepare Solution A,Solution B,and Solution C.
Assay—
Dissolve about 1.4g of Codeine Sulfate,previously dried and accurately weighed,in 50mLof glacial acetic acid,warming,if necessary,to effect solution.Titrate with 0.1Nperchloric acid VS,determining the endpoint potentiometrically.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 69.68mg of (C18H21NO3)2·H2SO4.
Auxiliary Information—
Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA2)Pharmaceutical Analysis 2
USP28–NF23Page 536
Phone Number:1-301-816-8139