Nabumetone 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

Nabumetone Tablets contain NLT 95.0% and NMT 105.0% of the labeled amount of nabumetone (C₁₅H₁₆O₂).

2 IDENTIFICATION

2.1 A.

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

Add the following:

2.2 B.

Diluent: Acetonitrile and water (50:50)

Standard solution: 0.25 mg/mL of USP Nabumetone RS in Diluent. Sonicate to dissolve, if necessary.

Sample solution: Nominally 0.25 mg/mL of nabumetone in Diluent from NLT 20 finely powdered Tablets. Sonicate to dissolve, if necessary.

Pass through a suitable filter of 0.45-µm pore size and discard the first few milliliters.

Acceptance criteria: The UV spectrum of the nabumetone peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

3 ASSAY

Change to read:

3.1 Procedure

Solution A: 0.1% (v/v) glacial acetic acid in water

Solution B: Acetonitrile and tetrahydrofuran (70:30)

Mobile phase: See Table 1.

Table 1

Diluent: Acetonitrile and water (50:50)

Standard solution: 0.5 mg/mL of USP Nabumetone RS in Diluent. Sonicate to dissolve, if necessary.

Sample solution: Nominally 0.5 mg/mL of nabumetone in Diluent from NLT 20 finely powdered Tablets. Sonicate to dissolve, if necessary.

Pass through a suitable filter of 0.45-µm pore size and discard the first few milliliters.

Chromatographic system

• (See Chromatography 〈621〉, System Suitability.)
• Mode: LC
• Detector: UV 254 nm. For Identification B, use a diode array detector in the range of 200–400 nm.
• Column: 4.6-mm × 15-cm; 5-µm packing L1
• Temperatures
• Autosampler: 10°
• Column: 30°
• Flow rate: 1.5 mL/min
• Injection volume: 10 µL

System suitability

• Sample: Standard solution
• Suitability requirements
• Tailing factor: NMT 2.0
• Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of nabumetone (C₁₅H₁₆O₂) in the portion of Tablets taken:

Result = (rᵤ/rₛ) × (Cₛ/Cᵤ) × 100

rᵤ = peak response of nabumetone from the Sample solution

rₛ = peak response of nabumetone from the Standard solution

Cₛ = concentration of USP Nabumetone RS in the Standard solution (mg/mL)

Cᵤ = nominal concentration of nabumetone in the Sample solution (mg/mL)

Acceptance criteria: 95.0%–105.0%

4 PERFORMANCE TESTS

4.1 Dissolution 〈711〉

Medium: Sodium lauryl sulfate solution (2 in 100); 900 mL

Apparatus 2: 50 rpm

Time: 45 min

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

Sample solution: Filter portions of the solution under test, and suitably dilute with Medium if necessary.

Analysis

Samples: Standard solution and Sample solution

Determine the labeled amount of nabumetone (C₁₅H₁₆O₂) dissolved from the differences between the UV absorbances at the wavelengths of maximum and minimum absorbances at about 270 and 296 nm, respectively.

Tolerances: NLT 75% (Q) of the labeled amount of nabumetone (C₁₅H₁₆O₂) is dissolved.

4.2 Uniformity of Dosage Units 〈905〉

Meet the requirements

5 IMPURITIES

Add the following:

5.1 Organic Impurities

Solution A and Solution B: Prepare as directed in the Assay.

Mobile phase: See Table 2.

Table 2

System suitability solution: 1 mg/mL of USP Nabumetone RS and 0.0015 mg/mL of USP Nabumetone Related Compound A RS prepared as follows. Transfer suitable amounts of USP Nabumetone RS and USP Nabumetone Related Compound A RS to a suitable volumetric flask. Add 10% of the flask volume of acetonitrile and dilute with acetonitrile to volume. Sonicate to dissolve, if necessary.

Sensitivity solution: 0.3 µg/mL of USP Nabumetone RS in acetonitrile

Standard solution: 0.01 mg/mL of USP Nabumetone RS in acetonitrile

Sample solution: Nominally 1 mg/mL of nabumetone from NLT 20 finely powdered Tablets in acetonitrile. Sonicate to dissolve, if necessary. Pass through a suitable filter of 0.45-µm pore size and discard the first few milliliters.

Chromatographic system: Proceed as directed in the Assay, except for the Column temperature and Flow rate.

Column temperature: 35°

Flow rate: 1.3 mL/min

System suitability

Samples: System suitability solution, Sensitivity solution, and Standard solution

Suitability requirements

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

Relative standard deviation: NMT 5.0%, Standard solution

Signal-to-noise ratio: NLT 10, Sensitivity solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of each degradation product in the portion of Tablets taken:

Result = (rᵤ/rₛ) × (Cₛ/Cᵤ) × 100

rᵤ = peak response of each degradation product from the Sample solution

rₛ = peak response of nabumetone from the Standard solution

Cₛ = concentration of USP Nabumetone RS in the Standard solution (mg/mL)

Cᵤ = nominal concentration of nabumetone in the Sample solution (mg/mL)

Acceptance criteria: See Table 3.

Table 3

ᵃ It is for peak identification only and is not included in the total degradation products.

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in well-closed containers, and store at controlled room temperature.

Change to read:

USP Reference Standards 〈11〉

USP Nabumetone RS

USP Nabumetone Related Compound A RS

(E)-4-(6-Methoxynaphthalen-2-yl)but-3-en-2-one.

C₁₅H₁₄O₂     226.27