Sulbactam Sodium
;)
4-Thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid,3,3-dimethyl-7-oxo-,4,4-dioxide,sodium salt,(2S-cis)-.
Sodium (2S,5R)-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylate 4,4-dioxide [69388-84-7].
»Sulbactam Sodium contains not less than 886µg and not more than 941µg of sulbactam (C8H11NO5S)per mg,calculated on the anhydrous 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.
Identification—
A:
The retention time of the major peak in the chromatogram of the Assay preparationcorresponds to that in the chromatogram of the Standard preparation,as obtained in the Assay.
B:
It meets the requirements of the tests for Sodium á191ñ.
Crystallinity á695ñ:
meets the requirements.
Bacterial endotoxins á85ñ—
Where the label states that Sulbactam Sodium is sterile or must be subjected to further processing during the preparation of injectable dosage forms,it contains not more than 0.17USP Endotoxin Unit per mg of sulbactam.
Sterility á71ñ—
Where the label states that Sulbactam Sodium is sterile,it meets the requirements when tested as directed for Membrane Filtrationunder Test for Sterility of the Product to be Examined.
Water,Method Iá921ñ:
not more than 1.0%.
Assay—
0.005M Tetrabutylammonium hydroxide—
Dilute 6.6mLof a 40%solution of tetrabutylammonium hydroxide with water to obtain 1800mLof solution.Adjust with 1Mphosphoric acid to a pHof 5.0±0.1,dilute with water to 2000mL,and mix.
Mobile phase—
Prepare a filtered and degassed mixture of 0.005M Tetrabutylammonium hydroxideand acetonitrile (1650:350).Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Standard preparation—
Quantitatively dissolve an accurately weighed quantity of USP Sulbactam RSin Mobile phaseto obtain a solution having a known concentration of about 1mg per mL.[NOTE—Inject this solution promptly.]
Assay preparation—
Transfer about 110mg of Sulbactam Sodium,accurately weighed,to a 100-mLvolumetric flask,dissolve in and dilute with Mobile phaseto volume,and mix.[NOTE—Inject this solution promptly.]
Chromatographic system
(see Chromatography á621ñ)—The liquid chromatograph is equipped with a 230-nm detector and a 4-mm ×30-cm column that contains packing L1.The flow rate is about 2mLper minute.Chromatograph the Standard preparation,and record the responses as directed for Procedure:the column efficiency is not less than 3500theoretical plates;the tailing factor is not more than 1.5;and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure—
Separately inject equal volumes (about 10µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the areas for the major peaks.Calculate the quantity,in µg,of sulbactam (C8H11NO5S)in each mg of Sulbactam Sodium taken by the formula:
100(CP/W)(rU/rS),
in which Cis the concentration,in mg per mL,of USP Sulbactam RSin the Standard preparation;Pis the assigned sulbactam content,in µg per mg,of USP Sulbactam RS;Wis the quantity,in mg,of Sulbactam Sodium taken to prepare the Assay preparation;and rUand rSare the peak areas for sulbactam obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information—
Staff Liaison:William W.Wright,Ph.D.,Scientific Fellow
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 1813
Pharmacopeial Forum:Volume No.27(1)Page 1818
Phone Number:1-301-816-8335