Meloxicam Oral Suspension

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

Meloxicam Oral Suspension contains NLT 90.0% and NMT 110.0% of the labeled amount of meloxicam (C₁₄H₁₃N₃O₄S₂).

2 IDENTIFICATION

A. The UV absorption spectrum of the meloxicam peak of the Sample solution exhibits maxima and minima at the same wavelengths as those of the Standard solution, as obtained in the Assay.

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

3 ASSAY

Procedure

Buffer: Dissolve 2 g of monohydrate citric acid and 2 g of boric acid in 1000 mL of water, and adjust with dihydrate trisodium citrate to a pH of 2.9.

Solution A: Acetonitrile, methanol, and Buffer (200:260:565)

Mobile phase: Dissolve 200 mg of sodium dodecyl sulfate in 1000 mL of Solution A.

Diluent: Dissolve 3 g of boric acid and 1.5 g of dihydrate trisodium citrate in 1000 mL of water, and adjust with 2 M sodium hydroxide to a pH of 8.3. Mix 420 mL of the resulting buffer with 420 mL of methanol and 160 mL of acetonitrile.

Related compound standard stock solution: 8.4 μg/mL of USP Meloxicam Related Compound B RS prepared as follows. Transfer 21 mg of USP Meloxicam Related Compound B RS into a 100-mL volumetric flask. Add 3.0 mL of dimethylformamide, 15 mL of methanol, and about 60 mL of Diluent. Sonicate, and mix until dissolved. Cool to room temperature. Dilute with Diluent to volume. Dilute further with Diluent to a concentration of 8.4 μg/mL.

System suitability solution: Transfer a volume of Oral Suspension, nominally equivalent to 15 mg of meloxicam, to a 50-mL volumetric flask.

Add 3.0 mL of Related compound standard stock solution. Add 3.0 mL of dimethylformamide. Swirl the flask, and allow to stand for 5 min.

Add 15 mL of methanol. Dilute with Diluent to just below volume. Sonicate for 30 min, mixing the flask vigorously about every 5 min. Cool to room temperature. Dilute with Diluent to volume. Mix, and allow particulates to settle. Pass through a 0.45-μm membrane filter with a berglass pre filter.

Standard stock solution: Transfer about 67 mg of USP Meloxicam RS into a 100-mL volumetric flask. Add 3.0 mL of dimethylformamide.

Swirl the flask, and allow to stand for 5 min. Add 15 mL of methanol. Dilute with Diluent to just below volume. Sonicate for 30 min, and mix until dissolved. Cool to room temperature. Dilute with Diluent to volume.

Standard solution: 0.3 mg/mL of USP Meloxicam RS in Diluent from Standard stock solution

Sample solution: Nominally 0.3 mg/mL of meloxicam prepared as follows. Transfer a volume of Oral Suspension, nominally equivalent to 15mg of meloxicam, to a 50-mL volumetric flask. Add 3.0 mL of dimethylformamide. Swirl the flask, and allow to stand for about 5 min. Add 15 mL of methanol. Dilute with Diluent to just below volume. Sonicate for 30 min, mixing the flask vigorously about every 5 min. Cool to room temperature. Dilute with Diluent to volume. Mix, and allow particulates to settle. Pass through a 0.45-μm membrane filter with a berglass pre filter.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 360 nm. For Identi

cation A, use a diode array detector in the range of 200–400 nm.

Column: 4-mm × 12.5-cm; 5-μm packing L1

Column temperature: 40°

Flow rate: 1.0 mL/min

Run time: NLT 2 times the retention time of meloxicam

Injection volume: 10 μL

System suitability

Samples: System suitability solution and Standard solution

Suitability requirements

Resolution: NLT 1.5 between meloxicam and any other adjacent peak, System suitability solution

Tailing factor: NMT 2.0 for the meloxicam peak, System suitability solution

Relative standard deviation: NMT 1.5%, Standard solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of meloxicam (C₁₄H₁₃N₃O₄S₂) in the portion of Oral Suspension taken:

Result = (r_U/r_S) × (C_S/C_U) × 100

r_U = peak area of meloxicam from the Sample solution

r_S = peak area of meloxicam from the Standard solution

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

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

Acceptance criteria: 90.0%–110.0%

4 PERFORMANCE TESTS

Change to read:

Dissolution 〈711〉

Medium: pH 7.5 phosphate buffer; 900 mL

Apparatus 2: 25 rpm

Time: 15 min

Standard solution: Transfer about 20.83 mg of USP Meloxicam RS into a 100-mL volumetric flask. Dissolve in 5 mL of methanol and 1 mL of 0.1 M sodium hydroxide, and dilute with Medium to volume. Dilute with Medium to a final concentration of 8.3 μg/mL of meloxicam.

Sample solution: Shake each sample for 15 min. Weigh six portions, equivalent to 7.5 mg of the Oral Suspension, into separate tared 10-mL beakers, and record each weight. Introduce each of the samples to the middle of the dissolution vessels, and rinse each beaker with 20 mL of the Medium withdrawn from the vessel. Carefully lower the paddle to the appropriate height and start the rotation. After completion of the dissolution, pass a 20-mL aliquot through a nylon filter having 0.45-μm porosity, discarding the first 3 mL of the filtrate.

Instrumental conditions

Mode: UV-Vis

Analytical wavelength: At about 362 nm (wavelength of maximum absorbance)

Blank: Medium

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of meloxicam (C₁₄H₁₃N₃O₄S₂) dissolved:

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

A_U = absorbance of the Sample solution

A_S = absorbance of the Standard solution

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

W_U = weight of the Oral Suspension taken (g) (ERR 1-Aug-2022)

L = label claim (mg/mL)

d = density of the Oral Suspension (g/mL)

V = volume of Medium, 900 mL

Tolerances: NLT 75% (Q) of the labeled amount of meloxicam (C₁₄H₁₃N₃O₄S₂) is dissolved.

5 IMPURITIES

Organic Impurities

Buffer, Solution A, Mobile phase, Diluent, Related compound standard stock solution, and Sample solution: Proceed as directed in the Assay.

Sensitivity solution: 0.08 μg/mL of USP Meloxicam Related Compound B RS in Diluent from Related compound standard stock solution

Standard solution: 0.5 μg/mL of USP Meloxicam Related Compound B RS in Diluent from Related compound standard stock solution

Chromatographic system: Proceed as directed in the Assay, except for the Detector.

Detector: UV 260 and 360 nm

System suitability

Samples: Sensitivity solution and Standard solution

Suitability requirements

Tailing factor: NMT 2.0 for the meloxicam related compound B peak at 260 nm, Standard solution

Relative standard deviation: NMT 10% for meloxicam related compound B at 260 nm, Sensitivity solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of meloxicam related compound B in the portion of Oral Suspension taken:

Result = (r_U/r_S) × (C_S/C_U) × 100

r_U = peak area of meloxicam related compound B in the Sample solution at 260 nm

r_S = peak area of meloxicam related compound B in the Standard solution at 260 nm

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

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

Calculate the percentage of each unknown degradation product in the portion of Oral Suspension taken:

Result = (r_U/r_T ) × 100

r_U = peak area of any unknown degradation product in the Sample solution at 360 nm

r_T = sum of peak areas of meloxicam and all impurities in the Sample solution at 360 nm

Acceptance criteria

Meloxicam related compound B: NMT 0.15%

Any individual unknown degradation product: NMT 0.2%

Total degradation products: NMT 0.5%

6 SPECIFIC TESTS

Microbial Enumeration Tests 〈61〉 and Tests for Specified Microorganisms 〈62〉: The total aerobic microbial count does not exceed 102 cfu/g or 102 cfu/mL. The total yeasts and molds count does not exceed 5 × 101 cfu/g or 5 × 101 cfu/mL. It meets the requirements of the test for the absence of Escherichia coli.

pH 〈791〉: 3.5–4.5

Viscosity—Rotational Methods 〈912〉

Analysis: Determine at 20° by using a shear rate programmable rotational viscometer.

Acceptance criteria: 40–100 centipoises

7 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in well-closed containers. Store at 25°, excursions permitted between 15° and 30°.

USP Reference Standards 〈11〉

USP Meloxicam RS

USP Meloxicam Related Compound B RS