Flurbiprofen Tablets

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

Flurbiprofen Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of urbiprofen (C₁₅H₁₃FO₂).

2 IDENTIFICATION

A. Infrared Absorption

Sample: Place 100 mg of urbiprofen from a number of Tablets in a ask. Add 10 mL of 0.1 N hydrochloric acid, and sonicate until the Tablets disintegrate. Extract with two 15-mL portions of ether, and combine the ether extracts in a ask containing 1 g of anhydrous sodium sulfate. Decant the ether, and evaporate to dryness.

Acceptance criteria: The IR absorption spectrum of a Mineral oil dispersion of the residue exhibits maxima only at the same wavelengths as those of a similar solution of USP Flurbiprofen RS.

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

3 ASSAY

Change to read: • Procedure

Solution A: Dissolve 1.26 g of ammonium formate in 1000 mL of water. Adjust with formic acid to a pH of 3.0.

Solution B: Acetonitrile and methanol (50:50)

Mobile phase: See Table 1.

Table 1 

Diluent: Acetonitrile and water (45:55)

Standard solution: 0.2 mg/mL of USP Flurbiprofen RS in Diluent

Sample stock solution: Nominally 1.0 mg/mL of urbiprofen in Diluent prepared as follows. Transfer a quantity of finely crushed Tablets (NLT 10), nominally equivalent to 25 mg of urbiprofen, to a 25-mL volumetric ask. Add 15 mL of Diluent and sonicate. [Note—A sonication time of 30 min may be suitable.]. Dilute with Diluent to volume. Centrifuge and use the clear supernatant.

Sample solution: Nominally 0.2 mg/mL of flurbiprofen from the Sample stock solution in Diluent. Pass a portion of the solution through a suitable filter of 0.45-μm pore size.

3.1 Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 254 nm

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

Flow rate: 1 mL/min

Injection volume: 10 µL

3.2 System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 1.5

Relative standard deviation: NMT 1.0%

3.3 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of urbiprofen (C₁₅H₁₃FO₂) in the portion of Tablets taken:

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

r_U = peak response of flurbiprofen from the Sample solution

r_S = peak response of urbiprofen from the Standard solution

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

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

(USP 1-Dec-2023)

Acceptance criteria: 90.0%–110.0%

4 PERFORMANCE TESTS

Change to read:

Dissolution 〈711〉

Medium stock solution: 122.5 g/L of monobasic potassium phosphate and 25 g/L of sodium hydroxide in water Medium: Dilute 166.5 mL of the Medium stock solution with water to 3000 mL. If necessary, adjust with 5 N sodium hydroxide or with phosphoric acid to a pH of 7.20 ± 0.05; 900 mL.

Apparatus 2: 50 rpm

Time: 45 min

Standard solution: A known concentration of USP Flurbiprofen RS in Medium

Sample solution: Pass a portion of the solution under test through a suitable filter. Suitably dilute with Medium to obtain a concentration similar to that of the Standard solution.

Instrumental conditions

Mode: UV

Analytical wavelength: Maximum absorbance at 247 nm

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of flurbiprofen (C₁₅H₁₃FO₂) dissolved:

Result = (A_U /A_S ) × C_S × V × D × (1/L) × 100

A_U = absorbance of the Sample solution

A_S = absorbance of the Standard solution

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

V = volume of Medium, 900 mL

D = dilution factor for the Sample solution

L = label claim (mg/Tablet)

(USP 1-Dec-2023)

Tolerances: NLT 75% (Q) of the labeled amount of urbiprofen (C₁₅H₁₃FO₂) is dissolved.

Change to read:

Uniformity of Dosage Units (USP 1-Dec-2023) 〈905〉: Meet the requirements (USP 1-Dec-2023)

5 IMPURITIES

Change to read:

Organic Impurities

Mobile: Acetonitrile, glacial acetic acid, and water (35:5:60)

Diluent: Acetonitrile and water (45:55)

Standard solution A: 0.004 mg/mL of USP Flurbiprofen RS in Diluent

Standard solution B: 0.01 mg/mL of USP Flurbiprofen Related Compound A RS in Diluent

Sensitivity solution: 0.002 mg/mL of USP Flurbiprofen RS in Diluent _{(USP 1-Dec-2023)}

Sample solution: Nominally 2 mg/mL of urbiprofen prepared as follows. Weigh, and finely powder Tablets (NLT 20). Dissolve 500 mg of urbiprofen from a portion of powdered Tablets in 50 mL of water, add 200 mL of acetonitrile, centrifuge, and use the supernatant. System suitability solution: 0.01 mg/mL each of USP Flurbiprofen RS and USP Flurbiprofen Related Compound A RSin Diluent. (USP 1-Dec 2023)

5.1 Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 254 nm

Column: 3.9-mm × 15-cm; 5-µm packing L1

Flow rate: 1 mL/min

Injection volume: 20 µL

5.2 System suitability

Samples: Standard solution A, Sensitivity solution, (USP 1-Dec-2023) and System suitability solution

[Note—The relative retention times for urbiprofen related compound A and urbiprofen are 0.87 and 1.0, respectively. These relative retention times are provided as information that could aid in peak assignment.] _{(USP 1-Dec-2023)}

Suitability requirements

Resolution: NLT 1.5 between urbiprofen and urbiprofen related compound A, System suitability solution

Relative standard deviation: NMT 5%  (USP 1-Dec-2023) , Standard solution A

Signal-to-noise ratio: NLT 10, Sensitivity solution (USP 1-Dec-2023)

5.3 Analysis

Samples: Standard solution A, Standard solution B, and Sample solution

Calculate the percentage of flurbiprofen related compound A in the portion of Tablets taken:

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

r_U = peak response of flurbiprofen related compound A from the Sample solution

r_S = peak response of urbiprofen related compound A from Standard solution B

C_S = concentration of USP Flurbiprofen Related Compound A RS in Standard solution B (mg/mL)

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

Calculate the percentage of any  (USP 1-Dec-2023) unspecified impurity in the portion of Tablets taken:

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

r_U = peak response for any unspecified impurity from the Sample solution

r_S = peak response of urbiprofen from Standard solution A

C_S = concentration of USP Flurbiprofen RS in Standard solution A (mg/mL)

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

Acceptance criteria: See Table 2. The reporting threshold is 0.1%. (USP 1-Dec-2023)

Table 2

6 ADDITIONAL REQUIREMENTS

Change to read:

Packaging and Storage: Preserve in well-closed containers. Protect from light. Store at controlled room temperature. _{(USP 1-Dec-2023)}

Change to read:

USP Reference Standards 〈11〉

USP Flurbiprofen RS

USP Flurbiprofen Related Compound A RS

2-(Biphenyl-4-yl)propanoic acid. _{(USP 1-Dec-2023)}

C₁₅H₁₄O₂           226.28