Fentanyl Citrate Injection
»Fentanyl Citrate Injection is a sterile solution of Fentanyl Citrate in Water for Injection.It contains the equivalent of not less than 90.0percent and not more than 110.0percent of the labeled amount of fentanyl (C22H28N2O),present as the citrate.
Packaging and storage Preserve in single-dose containers,preferably of Type Iglass,protected from light.
Identification 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.
Bacterial endotoxins á85ñ It contains not more than 50.0USP Endotoxin Units per mg.
pHá791ñ: between 4.0and 7.5.
Other requirements It meets the requirements under Injections á1ñ.
Mobile phase Prepare a filtered and degassed mixture containing 4volumes of ammonium acetate solution (1in 100)and 6volumes of a mixture of methanol,acetonitrile,and glacial acetic acid (400:200:0.6).Adjust this solution to a pHof 6.6±0.1by the dropwise addition of glacial acetic acid,and make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ),to obtain a retention time of about 5minutes for the fentanyl peak.
Standard preparation Dissolve an accurately weighed quantity of USP Fentanyl Citrate RSin water,and quantitatively dilute with water to obtain a solution having a known concentration of about 80µg per mL.
Assay preparation If necessary,dilute the Injection with water so that each mLcontains the equivalent of about 50µg of fentanyl.
Chromatographic system (see Chromatography á621ñ)The liquid chromatograph is equipped with a 230-nm detector and a 4.6-mm ×25-cm column that contains packing L1.The flow rate is about 2mLper minute.Chromatograph the Standard preparation,and record the peak response as directed for Procedure:the tailing factor for the fentanyl peak is not more than 2.0,and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure Separately inject equal volumes (about 25µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the quantity,in µg,of fentanyl (C22H28N3O)in each mLof the Injection taken by the formula:
(336.48/528.59)CD(rU/rS),in which 336.48and 528.59are the molecular weights of fentanyl and fentanyl citrate,respectively;Cis the concentration,in µg per mL,of USP Fentanyl Citrate RSin the Standard preparation;Dis the dilution factor used to obtain the Assay preparation;and rUand rSare the peak responses for the fentanyl peak obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information Staff Liaison:Clydewyn M.Anthony,Ph.D.,Scientist
Expert Committee:(PA2)Pharmaceutical Analysis 2