Ofloxacin Ophthalmic Solution
»Ofloxacin Ophthalmic Solution is a sterile aqueous solution of Ofloxacin.It contains not less than 90.0percent and not more than 110.0percent of the labeled amount of ofloxacin (C18H20FN3O4).
Packaging and storage— Preserve in tight containers at controlled room temperature.
Identification—
A: Thin-Layer Chromatographic Identification Test á201ñ—
Test solution— Dilute a portion of Ophthalmic Solution with a mixture of chloroform and methanol (1:1)to obtain a solution having a concentration of about 0.3mg of ofloxacin per mL.
Standard solution— Dissolve an accurately weighed quantity of USP Ofloxacin RSin a mixture of chloroform and methanol (1:1)to obtain a solution having a concentration of 3.0mg per mL.Transfer 5.0mLof this solution to a 50-mLvolumetric flask,add 5mLof water,dilute with a mixture of chloroform and methanol (1:1)to volume,and mix.
Application volume: 2µL.
Developing solvent system: a mixture of chloroform,methanol,and a solution (1in 30)of ammonium hydroxide (150:75:15).Saturate a paper-lined chromatographic chamber with this mixture.
B: The retention time of the ofloxacin peak in the chromatogram of the Assay preparationcorresponds to that in the chromatogram of the Standard preparation,as obtained in the Assay.
Sterility á71ñ— It meets the requirements when tested as directed for Membrane Filtrationunder Test for Sterility of the Product to be Examined.
pHá791ñ: between 6.0and 6.8.
Assay—
Mobile phase— Prepare a filtered and degassed mixture of sodium dodecyl sulfate (0.24%aqueous solution),acetonitrile,and glacial acetic acid (580:400:20).Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
0.05N Hydrochloric acid— Add 4.0mLof hydrochloric acid to 500mLof water,dilute with water to 1000mL,and mix.
Resolution solution— Prepare a solution of about 0.1mg of USP Ofloxacin RSand about 2.4mg of propylparaben in each mLof acetonitrile.
Standard preparation— Quantitatively dissolve an accurately weighed quantity of USP Ofloxacin RSin 0.05N Hydrochloric acidto obtain a solution having a known concentration of about 0.06mg per mL.
Assay preparation— Transfer an accurately measured volume of Ophthalmic Solution,equivalent to about 3mg of ofloxacin,to a 50-mLvolumetric flask,dilute with0.05N Hydrochloric acidto volume,and mix.
Chromatographic system (see Chromatography á621ñ)— The liquid chromatograph is equipped with a 294-nm detector and a 4.6-mm ×25-cm column that contains 5-µm packing L1.The flow rate is about 1.5mLper minute.The column temperature is maintained at a constant temperature of about 35.Chromatograph the Resolution solution,and record the peak responses as directed for Procedure:the resolution,R,between propylparaben and ofloxacin is not less than 2.Chromatograph the Standard preparation,and record the peak responses as directed for Procedure:the tailing factor is not more than 3;and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure— Separately inject equal volumes (about 20µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the areas for the major peaks.Calculate the quantity,in mg,of ofloxacin (C18H20FN3O4)in each mLof the Ophthalmic Solution taken by the formula:
50(C/V)(rU/rS),
in which Cis the concentration,in mg per mL,of USP Ofloxacin RSin the Standard preparation;Vis the volume,in mL,of Ophthalmic Solution taken to prepare the Assay preparation;and rUand rSare the ofloxacin peak areas obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Behnam Davani,Ph.D.,MBA,Senior Scientist
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 1414
Pharmacopeial Forum:Volume No.28(4)Page 1170
Phone Number:1-301-816-8394