Fluphenazine Decanoate Injection
» Fluphenazine Decanoate Injection is a sterile solution of Fluphenazine Decanoate in a suitable vegetable oil. It contains not less than 90.0 percent and not more than 115.0 percent of the labeled amount of fluphenazine decanoate (C32H44F3N3O2S).
Packaging and storage—
Preserve in single-dose or multiple-dose containers, of Type I glass, protected from light.
USP Reference standards 
11
—
USP Fluphenazine Decanoate Dihydrochloride RS.
USP Fluphenazine Hydrochloride RS.
11—
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 50 mg of fluphenazine decanoate, add 2 mL of methanol and 3 mL of palladium chloride solution (1 in 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 preparation corresponds 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 Injection taken by the formula:
3.43(W / V)(rU / rS)
in which W is the weight, in mg, of USP Fluphenazine Hydrochloride RS used to prepare the Standard preparation; V is the amount, in mg, of fluphenazine decanoate in the portion of Injection taken to prepare the Assay preparation, based on the labeled concentration; and rU and rS are the fluphenazine peak responses obtained from the Assay preparation and 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 ri is the peak response for each peak eluting after fluphenazine decanoate; and rs is 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 1.
1.
Assay—
Mobile phase—
Prepare a filtered and degassed mixture of methanol, acetonitrile, and 0.05 M ammonium acetate (2:2:1). Make adjustments if necessary (see System Suitability under Chromatography 621).
621).
Standard preparation—
Accurately weigh about 25 mg of USP Fluphenazine Hydrochloride RS, and transfer it to a 250-mL volumetric flask. Dissolve in isopropyl alcohol, dilute with isopropyl alcohol to volume, and mix (Solution A). Accurately weigh about 25 mg of Fluphenazine Decanoate Dihydrochloride RS. Transfer it to a 50-mL volumetric flask, and add 10 mL of Solution A, quantitatively measured. Add 20 mL of 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 0.1 mg of fluphenazine decanoate per mL.
Assay preparation—
Transfer an accurately measured quantity of the Injection, equivalent to about 25 mg of fluphenazine decanoate, to a glass-stoppered, 50-mL volumetric flask. Add about 20 mL of isopropyl alcohol, insert the stopper, and shake vigorously for at least 1 minute. Add 20 mL more 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 0.1 mg per mL.
System suitability preparation—
Weigh suitable quantities of USP Fluphenazine Decanoate Dihydrochloride RS and 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 RS of about 0.1 mg per mL.
Chromatographic system
(see Chromatography 621)—The chromatograph is equipped with a 254-nm detector and a 4.6-mm × 25-cm column containing 10-µm packing L1 preceded by a 4.6-mm × 5-cm pre-column containing similar packing of larger particle size (30–40 µm). The flow rate is about 2 mL per minute. Chromatograph the Standard preparation and 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 preparation is not less than 3.0; and the relative standard deviation of the fluphenazine decanoate peak for replicate injections of the Standard preparation does not exceed 2.0. The relative retention times for fluphenazine and fluphenazine decanoate are 0.6 and 1, respectively.
621)—The chromatograph is equipped with a 254-nm detector and a 4.6-mm × 25-cm column containing 10-µm packing L1 preceded by a 4.6-mm × 5-cm pre-column containing similar packing of larger particle size (30–40 µm). The flow rate is about 2 mL per minute. Chromatograph the Standard preparation and 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 preparation is not less than 3.0; and the relative standard deviation of the fluphenazine decanoate peak for replicate injections of the Standard preparation does not exceed 2.0. The relative retention times for fluphenazine and fluphenazine decanoate are 0.6 and 1, respectively.
Procedure—
Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, continuing the chromatography, in each case, for a time equal to 2.5 times 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 mL of the Injection taken by the formula:
0.890(WS / WU)(rU / rS)
in which WS is the weight, in mg, of USP Fluphenazine Decanoate Dihydrochloride RS corrected for its moisture content, used to prepare the Standard preparation; WU is the volume, in mL, of Injection taken, and rU and rS are the peak responses of fluphenazine decanoate obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information—
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Chromatographic Column—
| Topic/Question | Contact | Expert Committee |
| Monograph | Ravi Ravichandran, Ph.D.
Senior Scientist 1-301-816-8330 |
(MDPP05) Monograph Development-Psychiatrics and Psychoactives |
| Reference Standards | Lili Wang, Technical Services Scientist 1-301-816-8129 RSTech@usp.org |
USP32–NF27 Page 2421
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.