Fluphenazine Decanoate Injection
»Fluphenazine Decanoate Injection is a sterile solution of Fluphenazine Decanoate in a suitable vegetable oil.It contains not less than 90.0percent and not more than 115.0percent of the labeled amount of fluphenazine decanoate (C32H44F3N3O2S).
Packaging and storage— Preserve in single-dose or multiple-dose containers,of Type Iglass,protected from light.
USP Reference standards á11ñ— USP Fluphenazine Decanoate Dihydrochloride RS.USP Fluphenazine Hydrochloride RS.
NOTE—Throughout the following procedures,protect test or assay specimens,the USP Reference Standard,and solutions containing them,by conducting the procedures without delay,under subdued light,or using low-actinic glassware.
Identification—
A: To a volume of Injection,equivalent to about 50mg of fluphenazine decanoate,add 2mLof methanol and 3mLof palladium chloride solution (1in 1000):a rust-red color is produced.Add an excess of the palladium chloride solution:the color is intensified to a brownish red.
B: 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.
Chromatographic purity— From the chromatograms obtained in the Assay,calculate the percentage of fluphenazine in the portion of Injectiontaken by the formula:
3.43(W/V)(rU/rS),
in which Wis the weight,in mg,of USP Fluphenazine Hydrochloride RSused to prepare the Standard preparation;Vis the amount,in mg,of fluphenazine decanoate in the portion of Injection taken to prepare the Assay preparation,based on the labeled concentration;and rUand rSare the fluphenazine peak responses obtained from the Assay preparationand the Standard preparation,respectively.The fluphenazine content is not more than 4%of the labeled amount of fluphenazine decanoate.[NOTE—Use peak heights where peak responses are indicated.]Calculate the percentage of each impurity eluting after fluphenazine decanoate in the portion of Injection taken by the formula:
100(ri/rs),
in which riis the peak response for each peak eluting after fluphenazine decanoate;and rsis the sum of the responses for fluphenazine decanoate and all of the peaks eluting after fluphenazine decanoate:the sum of the responses for all of the peaks eluting after fluphenazine decanoate is not more than 2%.
Other requirements— It meets the requirements under Injections á1ñ.
Assay—
Mobile phase— Prepare a filtered and degassed mixture of methanol,acetonitrile,and 0.05Mammonium acetate (2:2:1).Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Standard preparation— Accurately weigh about 25mg of USP Fluphenazine Hydrochloride RS,and transfer it to a 250-mLvolumetric flask.Dissolve in isopropyl alcohol,dilute with isopropyl alcohol to volume,and mix (Solution A).Accurately weigh about 25mg of Fluphenazine Decanoate Dihydrochloride RS.Transfer it to a 50-mLvolumetric flask,and add 10mLof Solution A,quantitatively measured.Add 20mLof isopropyl alcohol and dissolve sonicating,if necessary.Dilute with isopropyl alcohol to volume,and mix.Quantitatively dilute the resulting solution with acetonitrile (1:5)to obtain a solution having a known concentration of about 0.1mg of fluphenazine decanoate per mL.
Assay preparation— Transfer an accurately measured quantity of the Injection,equivalent to about 25mg of fluphenazine decanoate,to a glass-stoppered,50-mLvolumetric flask.Add about 20mLof isopropyl alcohol,insert the stopper,and shake vigorously for at least 1minute.Add 20mLmore of isopropyl alcohol,and repeat the vigorous shaking.Dilute with isopropyl alcohol to volume,and mix.Quantitatively dilute the resulting solution with acetonitrile (1:5)to obtain a solution having a concentration of fluphenazine decanoate of about 0.1mg per mL.
System suitability preparation— Weigh suitable quantities of USP Fluphenazine Decanoate Dihydrochloride RSand USP Fluphenazine Hydrochloride RS(5:4),and dissolve in a mixture of methanol and acetonitrile (1:1).Dilute the solution quantitatively and stepwise with the same solvent mixture to obtain a solution having a concentration of anhydrous USP Fluphenazine Decanoate Dihydrochloride RSof about 0.1mg per mL.
Chromatographic system (see Chromatography á621ñ)—The chromatograph is equipped with a 254-nm detector and a 4.6-mm ×25-cm column containing 10-µm packing L1preceded by a 4.6-mm ×5-cm pre-column containing similar packing of larger particle size (30–40µm).The flow rate is about 2mLper minute.Chromatograph the Standard preparationand the System suitability preparation,and record the peak responses as directed for Procedure:the resolution,R,between fluphenazine and fluphenazine decanoate in the System suitability preparationis not less than 3.0;and the relative standard deviation of the fluphenazine decanoate peak for replicate injections of the Standard preparationdoes not exceed 2.0.The relative retention times for fluphenazine and fluphenazine decanoate are 0.6and 1,respectively.
Procedure— Separately inject equal volumes (about 20µL)of the Standard preparationand the Assay preparationinto the chromatograph,continuing the chromatography,in each case,for a time equal to 2.5times the elution time of fluphenazine decanoate.Record the chromatograms,and measure responses for the major peaks and for the peaks from all substances eluting after fluphenazine decanoate.Calculate the quantity,in mg,of fluphenazine decanoate (C32H44F3N3O2S)in each mLof the Injection taken by the formula:
0.890(WS/WU)(rU/rS),
in which WSis the weight,in mg,of USP Fluphenazine Decanoate Dihydrochloride RScorrected for its moisture content,used to prepare the Standard preparation;WUis the volume,in mL,of Injectiontaken,and rUand rSare the peak responses of fluphenazine decanoate obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Ravi Ravichandran,Ph.D.,Senior Scientist
Expert Committee:(PA3)Pharmaceutical Analysis 3
USP28–NF23Page 858
Phone Number:1-301-816-8330