Secobarbital Sodium
C12H17N2NaO3
260.27
2,4,6(1H,3H,5H)-Pyrimidinetrione,5-(1-methylbutyl)-5-(2-propenyl)-,monosodium salt.
Sodium 5-allyl-5-(1-methylbutyl)barbiturate [309-43-3].
»Secobarbital Sodium contains not less than 98.5percent and not more than 100.5percent of C12H17N2NaO3,calculated on the dried basis.
Packaging and storage—
Preserve in tight containers.
Labeling—
Where it is intended for use in preparing injectable dosage forms,the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms.
Completeness of solution—
Mix 1.0g with 10mLof carbon dioxide-free water:after 1minute,the solution is clear and free from undissolved solid.
Identification—
A:
The IRabsorption spectrum of a chloroform solution of the residue of secobarbital obtained as directed in the Assayexhibits maxima only at the same wavelengths as that of a similar preparation of USP Secobarbital RS.
B:
Ignite about 500mg:the residue effervesces with acids,and responds to the tests for Sodium á191ñ.
pHá791ñ:
between 9.7and 10.5,in the solution prepared in the test for Completeness of solution.
Loss on drying á731ñ—
Dry it at 80
for 5hours:it loses not more than 3.0%of its weight.
for 5hours:it loses not more than 3.0%of its weight.
Heavy metals,Method IIá231ñ:
0.003%.
Organic volatile impurities,Method Iá467ñ:
meets the requirements.
Isomer content—
Dissolve about 300±5mg in 5mLof sodium hydroxide solution (1in 100),add a solution of 300±5mg of p-nitrobenzyl bromide in 10mLof alcohol,reflux for 30minutes,cool,collect the precipitate on a small filter,and wash with water:the precipitate,recrystallized from 25mLof alcohol and dried at 105for 30minutes,melts between 156and 161.
for 30minutes,melts between 156and 161.
Other requirements—
Where the label states that Secobarbital Sodium is sterile,it meets the requirements for Sterility Tests á71ñand for Bacterial endotoxinsunder Secobarbital Sodium for Injection.Where the label states that Secobarbital Sodium must be subjected to further processing during the preparation of injectable dosage forms,it meets the requirements for Bacterial endotoxinsunder Secobarbital Sodium for Injection.
Assay—
Dissolve about 500mg of Secobarbital Sodium,accurately weighed,in 15mLof water in a separator.To the solution add 2mLof hydrochloric acid,shake,and extract the liberated secobarbital with eight 25-mLportions of chloroform.Test for completeness of extraction by extracting with an additional 10-mLportion of chloroform and evaporating the solvent:not more than 0.5mg of residue remains.Filter the extracts into a tared beaker,and finally rinse the separator and the filter with several small portions of chloroform.Evaporate the combined filtrate and washings on a steam bath with the aid of a current of air just to dryness.Dissolve the residue in 2mLof dehydrated alcohol,and evaporate to dryness.Repeat the dissolution and evaporation with 2mLof dehydrated alcohol,and dry the residue at 100for 2hours.The weight of the residue,multiplied by 1.092,represents the weight of C12H17N2NaO3.
for 2hours.The weight of the residue,multiplied by 1.092,represents the weight of C12H17N2NaO3.
Auxiliary Information—
Staff Liaison:Ravi Ravichandran,Ph.D.,Senior Scientist
Expert Committee:(PA3)Pharmaceutical Analysis 3
USP28–NF23Page 1759
Pharmacopeial Forum:Volume No.29(6)Page 1978
Phone Number:1-301-816-8330