Fluphenazine Decanoate

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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C₃₂H₄₄F₃N₃O₂S 591.78 (CN 1-May-2024)

Decanoic acid, 2-[4-[3-[2-(trifluoromethyl)-10H-decanoate phenothiazin-10-yl]propyl]-1-piperazinyl]ethyl ester;

2-[4-[3-[2-(Trifluoromethyl)phenothiazin-10-yl]propyl]-1-piperazinyl]ethyl decanoate CAS RN®: 5002-47-1; UNII: FMU62K1L3C.

1 DEFINITION

Fluphenazine Decanoate contains NLT 98.0% and NMT 102.0% of fluphenazine decanoate (C₃₂H₄₄F₃N₃O₂S), calculated on the dried basis.

[Note - Throughout the following procedures, protect samples, the Reference Standard, and solutions containing them by conducting the procedures without delay under subdued light, or using low-actinic glassware.]

2 IDENTIFICATION

A. Infrared Absorption

Solution A: Sodium hydroxide solution (1 in 250)

Standard solution: Transfer 50 mg of USP Fluphenazine Decanoate Dihydrochloride RS to a glass-stoppered, small centrifuge tube, and add 1.5 mL of Solution A. Add 2 mL of carbon disulfide, shake vigorously for 2 min, and centrifuge. Dry the lower, clear layer by filtering through 2 g of anhydrous sodium sulfate. Use the filtrate.

Sample solution: Transfer 50 mg of Fluphenazine Decanoate to a glass-stoppered, small centrifuge tube, and add 1.5 mL of Solution A. Add 2 mL of carbon disulfide, shake vigorously for 2 min, and centrifuge. Dry the lower, clear layer by filtering through 2 g of anhydrous sodium sulfate. Use the filtrate.

Instrumental conditions

Mode: IR

Cell: 0.1 mm

Acceptance criteria: The absorption spectrum of the Sample solution exhibits maxima only at the same wavelengths as that of the Standard solution.

B. Thin-Layer Chromatography

Standard solution: 22.5 mg/mL of USP Fluphenazine Decanoate Dihydrochloride RS (equivalent to 20 mg/mL of fluphenazine decanoate) in alcohol

Sample solution: 20 mg/mL of Fluphenazine Decanoate in alcohol

Chromatographic system

(See Chromatography 〈621〉, Thin-Layer Chromatography.)

Adsorbent: 0.25-mm layer of chromatographic silica gel mixture. Impregnate the plate with a 1-in-20 solution of tetradecane in hexane, and allow to air-dry.

Application volume: 1 μL

Developing solvent system: Methanol and water (90:10)

Analysis

Samples: Standard solution and Sample solution

Apply the Standard solution and the Sample solution to the plate. Allow the spots to dry. Apply 1.0 μL of 0.1 N sodium hydroxide to the spot from the Standard solution, and allow it to dry. Develop the plate in an equilibrated chamber using the Developing solvent system.

Examine the plate under short-wavelength UV light at 254 nm.

Acceptance criteria: The R value of the principal spot of the Sample solution corresponds to that of the Standard solution.

3 ASSAY

Procedure

Sample: 500 mg of Fluphenazine Decanoate

Blank: 50 mL of glacial acetic acid

Titrimetric system

Mode: Direct titration

Titrant: 0.1 N perchloric acid VS

Endpoint detection: Visual

Analysis: Dissolve the Sample in 50 mL of glacial acetic acid, add one drop of crystal violet TS, and titrate with Titrant to a blue-green endpoint. Perform the Blank determination, and make any necessary correction.

Calculate the percentage of fluphenazine decanoate (C₃₂H₄₄F₃N₃O₂S) in the portion of Fluphenazine Decanoate taken. Each mL of 0.1 N perchloric acid is equivalent to 29.59 mg of fluphenazine decanoate (C₃₂H₄₄F₃N₃O₂S).

Acceptance criteria: 98.0%–102.0% on the dried basis

4 IMPURITIES

Residue on Ignition 〈281〉: NMT 0.2%

Ordinary Impurities 〈466〉

Test solution and Standard solution: Methanol

Eluant: Acetone, cyclohexane, and ammonium hydroxide (16:6:1)

Visualization: 1; then spray the plate with 50% sulfuric acid.

Acceptance criteria

Individual impurity: NMT 1.0%

Total impurities: NMT 2.0%

5 SPECIFIC TESTS

Loss on Drying 〈731〉

Analysis: Dry under vacuum at 60° for 3 h.

Acceptance criteria: NMT 1.0%

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight, light-resistant containers.

USP Reference Standards 〈11〉

USP Fluphenazine Decanoate Dihydrochloride RS