Fluphenazine Hydrochloride Tablets
»Fluphenazine Hydrochloride Tablets contain not less than 90.0percent and not more than 110.0percent of the labeled amount of fluphenazine hydrochloride (C22H26F3N3OS·2HCl).
Packaging and storage— Preserve in tight,light-resistant containers.
USP Reference standards á11ñ— 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— Transfer a portion of finely powdered Tablets,equivalent to about 10mg of fluphenazine hydrochloride,to a separator,and to a second separator transfer 10mg of USP Fluphenazine Hydrochloride RS.Add 5mLof water and 20mLof dilute hydrochloric acid (1in 120)to each separator,shake for 10minutes,and to each mixture add 20mLof chloroform-saturated sodium carbonate solution (1in 10).Extract each mixture with five 20-mLportions of chloroform,shaking gently to avoid emulsion formation,and pass the extracts through separate chloroform-washed cotton filters into separate 150-mLbeakers.Evaporate the extracts on a steam bath to dryness,and dissolve the residues in 0.5-mLportions of a mixture of 4volumes of methanol and 1volume of water.Apply 10µLof each solution to a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture.Allow the spots to dry,and develop the chromatogram in a solvent system consisting of a mixture of acetone,cyclohexane,and diethylamine (40:15:1)until the solvent front has moved about three-fourths of the length of the plate.Remove the plate from the developing chamber,mark the solvent front,and allow the solvent to evaporate.Locate the spots on the plate by lightly spraying with a solution of sulfuric acid in methanol (2in 5):the RFvalue and color of the principal spot obtained from the test solution correspond to those obtained from the Standard solution.
Dissolution á711ñ—
Medium: 0.01Nhydrochloric acid;900mL.
Apparatus 1: 100rpm.
Time: 45minutes.
Procedure— Determine the amount of C22H26F3N3OS·2HCl dissolved by employing the procedure set forth in the Assay,with the following differences:in the Mobile phase,use 0.3%triethylamine;in the Assay preparation,dilute the amount of sample to be withdrawn with an equal volume of Mobile phase;in the Standard preparation,use a concentration and composition similar to that of the Assay preparation;in the Chromatographic system,use a flow rate of about 2.0mLper minute;in the Procedure,inject a volume of about 100µL.
Tolerances— Not less than 75%(Q)of the labeled amount of C22H26F3N3OS·2HCl is dissolved in 45minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Assay—
Diluent solution ,Mobile phase,Standard preparation,and Chromatographic system—Proceed as directed in the Assayunder Fluphenazine Hydrochloride.
Assay preparation— Transfer 6Tablets to a suitable volumetric flask,add Diluent solution,shake for 1hour,and sonicate for 10minutes or until a fine suspension is obtained.Dilute quantitatively,and stepwise if necessary,with Diluent solutionto obtain a final concentration of 0.06mg of fluphenazine hydrochloride per mL.Filter,discarding the first 5mLof the filtrate.
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 mg,of fluphenazine hydrochloride (C22H26F3N3OS·2HCl)in the portion of Tablets taken by the formula:
100CT(rU/rS),
in which Cis the concentration,in mg per mL,of USP Fluphenazine Hydrochloride RSin the Standard preparation;Tis the labeled quantity,in mg,of fluphenazine hydrochloride in the Tablet;and rUand rSare the peak responses 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 861
Phone Number:1-301-816-8330