Meclofenamate Sodium Capsules

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

Meclofenamate Sodium Capsules contain an amount of meclofenamate sodium (C₁₄H₁₀Cl₂NNaO₂) equivalent to NLT 90.0% and NMT 110.0% of the labeled amount of meclofenamic acid (C₁₄H₁₁Cl₂NO₂).

2 IDENTIFICATION

Delete the following:

Thin-Layer Chromatographic Identification Test 〈201〉

Sample solution: 20 mg/mL of meclofenamate sodium, from Capsule contents in methanol; filter

Developing solvent system: Methylene chloride, methyl ethyl ketone, and glacial acetic acid (50:48:2)

Acceptance criteria: The filtrate meets the requirements. (USP 1-May-2022)

Add the following:

A. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay. (USP 1-May-2022)

Add the following:

B. The UV spectrum of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay. (USP 1-May-2022)

3 ASSAY

Change to read:

Procedure

Solution A: 0.63 g/L of ammonium formate in water. Adjust with formic acid to a pH of 3.0.

Solution B: Acetonitrile

Mobile phase: See Table 1.

Table 1

Diluent: Methanol and water (50:50)

Standard solution: 0.3 mg/mL of USP Meclofenamate Sodium RS in Diluent

Sample solution: Nominally 0.28 mg/mL of meclofenamic acid, equivalent to 0.3 mg/mL of meclofenamate sodium (anhydrous) in Diluent, prepared as follows. Mix the contents of Capsules (NLT 10) and transfer a suitable portion to a suitable volumetric flask. Add Diluent to about 80% of the volume, vortex, and sonicate for NLT 5 min. Dilute with Diluent to volume. Pass through a suitable filter of 0.45-μm pore size and use the filtrate.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 270 nm. For Identification B, use a diode array detector in the range of 190–400 nm.

Column: 4.6-mm × 15-cm; 3.5-μm packing L1

Column temperature: 35°

Flow rate: 0.8 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 meclofenamic acid (C₁₄H₁₁Cl₂NO₂) in the portion of Capsules taken:

Result = (r_U/r_S) × (C_S/C_U) × (M_r1/M_r2) × 100

r_U = peak response of meclofenamate from the Sample solution

r_S = peak response of meclofenamate from the Standard solution

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

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

M_r1 = molecular weight of meclofenamic acid, 296.15

M_r2 = molecular weight of meclofenamate sodium (anhydrous), 318.13 (USP 1-May-2022)

Acceptance criteria: 90.0%–110.0%

4 PERFORMANCE TESTS

Change to read:

Dissolution 〈711〉

Medium: 0.05 M pH 7.5 phosphate buffer (See Reagents, Indicators, and Solutions, Solutions, Buffer Solutions); 900 mL

Apparatus 2: 50 rpm

Time: 45 min

Standard solution: A known concentration of USP Meclofenamate Sodium RS in Medium

Sample solution: Pass a portion of the solution under test through a suitable filter. Dilute with Medium, if necessary.

Instrumental conditions

Analytical wavelength: 279 nm (maximum absorbance)

Mode: UV

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of meclofenamic acid (C₁₄H₁₁Cl₂NO₂) dissolved:

Result = (A_U/A_S) × C_S × V × D × (1/L) × (M_r1/M_r2) × 100

A_U = absorbance of the Sample solution

A_S = absorbance of the Standard solution

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

V = volume of Medium, 900 mL

D = dilution factor of the Sample solution if needed

L = label claim (mg/Capsule)

M_r1 = molecular weight of meclofenamic acid, 296.15

M_r2 = molecular weight of meclofenamate sodium (anhydrous), 318.13 (USP 1-May-2022)

Tolerances: NLT 75% (Q) of the labeled amount of meclofenamic acid (C₁₄H₁₁Cl₂NO₂) is dissolved.

Uniformity of Dosage Units 〈905〉: Meet the requirements

5 IMPURITIES

Add the following:

Organic Impurities

Solution A, Mobile phase, Diluent, Sample solution, and Chromatographic system: Proceed as directed in the Assay.

Standard solution: 0.6 μg/mL of USP Meclofenamate Sodium RS in Diluent

Sensitivity solution: 0.3 μg/mL of USP Meclofenamate Sodium RS in Diluent from Standard solution

System suitability

Samples: Standard solution and Sensitivity solution

Suitability requirements

Tailing factor: NMT 2.0, Standard solution

Relative standard deviation: NMT 5.0%, Standard solution

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

Analysis

Samples: Sample solution and Standard solution

Calculate the percentage of any degradation product in the portion of Capsules taken:

Result = (r_U/r_S) × (C_S/C_U) × (M_r1/M_r2) × 100

r_U = peak response of any degradation product from the Sample solution

r_S = peak response of meclofenamate from the Standard solution

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

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

M_r1 = molecular weight of meclofenamic acid, 296.15

M_r2 = molecular weight of meclofenamate sodium (anhydrous), 318.13

Acceptance criteria: See Table 2. The reporting threshold is 0.1%.

Table 2

(USP 1-May-2022)

6 ADDITIONAL REQUIREMENTS

Change to read:

Packaging and Storage: Preserve in tight, light-resistant containers at controlled room temperature. (USP 1-May-2022)

USP Reference Standards 〈11〉

USP Meclofenamate Sodium RS