Fluticasone Propionate Lotion

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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1 DEFINITION

Fluticasone Propionate Lotion is fluticasone propionate in a suitable lotion base. It contains NLT 90.0% and NMT 110.0% of the labeled amount of fluticasone propionate (C₂₅H₃₁F₃O₅S).

2 IDENTIFICATION

A. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

B. The UV spectrum of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

3 ASSAY

3.1 PROCEDURE

Buffer: 1.15 g/L of monobasic ammonium phosphate in water. Adjust with phosphoric acid to a pH of 3.5. Pass the solution through a suitable filter of 0.45-µm pore size.

Mobile phase: Acetonitrile, methanol, and Buffer (13:50:37)

Standard stock solution: 0.8 mg/mL of USP Fluticasone Propionate RS, prepared as follows. Transfer 40 mg of USP Fluticasone Propionate RS to a 50-mL volumetric flask. Add 10 mL of tetrahydrofuran and sonicate to dissolve. Dilute with methanol to volume.

Standard solution: 0.04 mg/mL of USP Fluticasone Propionate RS in methanol from Standard stock solution

Sample solution: Nominally 0.04 mg/mL of fluticasone propionate from Lotion, prepared as follows. Transfer a portion of Lotion to a suitable volumetric flask. Add tetrahydrofuran equivalent to about 20% of the flask volume and vortex until the Lotion is dispersed. Add methanol equivalent to 60% of the flask volume and sonicate for 10 min to dissolve. Dilute with methanol to volume. Pass a portion of the solution through a suitable filter of 0.45-µm pore size.

3.2 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: 239 nm. For Identification B, use a diode array detector in the range of 200-400 nm.

Column: 4.6-mm × 25-cm; 5-µm packing L1

Column temperature: 45°

Flow rate: 1 mL/min

Injection volume: 20 µL

Run time: NLT 1.25 times the retention time of fluticasone propionate

3.3 System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 2.0

Column efficiency: NLT 5000 theoretical plates

Relative standard deviation: NMT 2.0%

3.4 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of fluticasone propionate (C₂₅H₃₁F₃O₅S) in the portion of Lotion taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of fluticasone propionate from the Sample solution

r_S = peak response of fluticasone propionate from the Standard solution

C_S = concentration of USP Fluticasone Propionate RS in the Standard solution (mg/mL)

C_U = nominal concentration of fluticasone propionate in the Sample solution (mg/mL)

Acceptance criteria: 90.0%-110.0%

4 PERFORMANCE TESTS

MINIMUM FILL (755): Meets the requirements

5 IMPURITIES

5.1 ORGANIC IMPURITIES

Solution A: Methanol, phosphoric acid, and water (30:0.5:970)

Solution B: Acetonitrile, methanol, and phosphoric acid (950:50:0.5)

Mobile phase: See Table 1.

Table 1

System suitability solution: 0.13 mg/mL of USP Fluticasone Propionate RS and 0.38 µg/mL of USP Fluticasone Propionate Related Compound D RS in methanol

Standard stock solution: 0.25 mg/mL of USP Fluticasone Propionate RS, prepared as follows. Transfer 25 mg of USP Fluticasone Propionate RS to a 100-mL volumetric flask. Add 25 mL of tetrahydrofuran and sonicate to dissolve. Dilute with methanol to volume.

Standard solution: 0.63 µg/mL of USP Fluticasone Propionate RS in methanol from Standard stock solution

Sample solution: Nominally 0.13 mg/mL of fluticasone propionate from Lotion, prepared as follows. Transfer a portion of Lotion, equivalent to 1.25 mg of fluticasone propionate, to a suitable volumetric flask. Add tetrahydrofuran equivalent to 20% of the flask volume and vortex until the Lotion is dispersed. Add methanol equivalent to 40% of the flask volume and sonicate for 10 min to dissolve. Dilute with methanol to volume. Pass a portion of the solution through a suitable filter of 0.45-µm pore size.

5.2 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: 239 nm

Column: 4.6-mm × 25-cm; 5-µm packing L1

Column temperature: 40°

Flow rate: 1.5 mL/min

Injection volume: 40 µL

5.3 System suitability

Samples: System suitability solution and Standard solution

[NOTE-See Table 2 for the relative retention times.]

Suitability requirements

Resolution: NLT 1.5 between fluticasone propionate related compound D and fluticasone propionate, System suitability solution

Relative standard deviation: NMT 5.0% from six replicate injections, Standard solution

5.4 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of fluticasone propionate related compound C, fluticasone propionate related compound D, or any individual unspecified degradation product in the portion of Lotion taken:

Result = (r_U/r_S) x (C_S/C_U) x (1/F) x 100

r_U = peak response of fluticasone propionate related compound C, fluticasone propionate related compound D, or each unspecified degradation product from the Sample solution

r_S = peak response of fluticasone propionate from the Standard solution

C_S = concentration of USP Fluticasone Propionate RS in the Standard solution (µg/mL)

C_U = nominal concentration of fluticasone propionate in the Sample solution (µg/mL)

F = relative response factor (see Table 2)

Acceptance criteria: See Table 2.

Table 2

^a S-Fluoromethyl 17α-acetyloxy-6α, 9α-difluoro-11β-hydroxy-16α-methyl-3-oxoandrosta-1,4-diene-17β-carbothioate.

6 SPECIFIC TESTS

6.1 PH (791)

Sample: 50 mg/mL of Lotion in water

Acceptance criteria: 4.0-6.0

6.2 MICROBIAL ENUMERATION TESTS (61) and TESTS FOR SPECIFIED MICROORGANISMS (62)

Meets the requirements of the tests for absence of Salmonella species, Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa. The total aerobic microbial count is NMT 10² cfu/g, and the total combined molds and yeasts count is NMT 10 cfu/g.

7 ADDITIONAL REQUIREMENTS

7.1 PACKAGING AND STORAGE

Preserve in tight containers. Store at controlled room temperature. Do not refrigerate.

7.2 USP REFERENCE STANDARDS (11)

USP Fluticasone Propionate RS

USP Fluticasone Propionate Related Compound D RS

S-Methyl 6α,9α-difluoro-11β-hydroxy-16α-methyl-3-oxo-17α-propionyloxyandrosta-1,4-diene-17β-carbothioate.

C₂₅H₃₂F₂O₅S 482.58