Methylprednisolone 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

Methylprednisolone Tablets contain NLT 92.5% and NMT 107.5% of the labeled amount of methylprednisolone (C₂₂H₃₀O₅).

2 IDENTIFICATION

A. Spectroscopic Identification Tests 〈197〉, Infrared Spectroscopy: 197K

Sample: Digest an amount nominally equivalent to about 40 mg of methylprednisolone from powdered Tablets with 25 mL of solvent hexane

for 15 min. Filter, and discard the [Ký tự không đọc được]ltrate. Digest the residue with 25 mL of chloroform for 15 min. Filter, evaporate the

[Ký tự không đọc được]ltrate to dryness, and dry at 105° for 2 h.

Acceptance criteria: Meets the requirements

B.

Sample: Use the Sample from Identification A.

Analysis: Dissolve about 5 mg of Sample in 2 mL of sulfuric acid.

Acceptance criteria: A red color is produced

3 ASSAY

Procedure

Mobile phase: Butyl chloride, water-saturated butyl chloride, tetrahydrofuran, methanol, and glacial acetic acid (95:95:14:7:6)

Solution A: 3% Glacial acetic acid in chloroform

Internal standard solution: 0.2 mg/mL of Prednisone in Solution A

Standard solution: 0.2 mg/mL of USP Methylprednisolone RS in the Internal standard solution

Sample solution: Nominally 0.19 mg/mL of methylprednisolone prepared as follows. Transfer an amount nominally equivalent to about

10 mg of methylprednisolone, from 20 [Ký tự không đọc được]nely powdered Tablets in a mortar and pestle, to a suitable container. Add

2.5 mL of water and swirl to form a [Ký tự không đọc được]ne slurry. Add 50.0 mL of Internal standard solution and shake for 15 min. If

necessary, pass a portion of the solution through a suitable [Ký tự không đọc được]lter or centrifuge a portion of the solution and analyze

the clear supernatant.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 254 nm

Column: 4.0-mm × 25.0-cm; packing L3

Flow rate: 1 mL/min

Injection volume: 10 µL

System suitability

Sample: Standard solution

[Note—The relative retention times for prednisone and methylprednisolone are about 0.7 and 1.0, respectively.]

Suitability requirements

Resolution: NLT 4.0 between prednisone and methylprednisolone

Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of methylprednisolone (C₂₂H₃₀O₅) in the portion of Tablets taken:

Result = (Rᵤ / Rₛ) × (Cₛ / Cᵤ) × 100

Rᵤ = peak response ratio of methylprednisolone to prednisone from the Sample solution

Rₛ = peak response ratio of methylprednisolone to prednisone from the Standard solution

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

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

Acceptance criteria: 92.5%–107.5%

4 PERFORMANCE TESTS

Change to read:

Dissolution 〈711〉

▲Test 1▲ (RB 1-Jun-2022)

Medium: Water; 900 mL

Apparatus 2: 50 rpm

Time: 30 min

Standard solutions: 20 µg/mL of USP Methylprednisolone RS prepared as follows. Dissolve a suitable quantity of USP Methylprednisolone

RS in 0.1% of the flask volume of alcohol and dilute with water to volume. Prepare quantitative dilutions of this solution for the development

of a standard curve.

Sample solution: Pass a portion of the solution under test through a suitable [Ký tự không đọc được]lter. Dilute with Medium, if necessary

Instrumental conditions

Mode: UV

Analytical wavelength: 246 nm

Cell: 1 cm

Blank: Water

Analysis

Samples: Standard solutions, Sample solution, and Blank

Using a standard curve, representing the absorbance versus concentration of the Standard solutions, determine the labeled amount of

methylprednisolone (C₂₂H₃₀O₅) dissolved.

Tolerances: NLT 70% (Q) of the labeled amount of methylprednisolone (C₂₂H₃₀O₅) is dissolved.

▲Test 2: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 2.

Medium: Water; 500 mL

Apparatus 2: 50 rpm

Time: 20 min

Standard stock solution: 0.2 mg/mL of USP Methylprednisolone RS prepared as follows. Transfer a suitable amount of USP

Methylprednisolone RS to an appropriate volumetric flask. Add 2% of the flask volume of ethyl alcohol and sonicate to dissolve. Dilute

with water to volume.

Standard solution A: 0.002 mg/mL of USP Methylprednisolone RS from Standard stock solution in water

Standard solution B: 0.004 mg/mL of USP Methylprednisolone RS from Standard stock solution in water

Standard solution C: 0.008 mg/mL of USP Methylprednisolone RS from Standard stock solution in water

Standard solution D: 0.010 mg/mL of USP Methylprednisolone RS from Standard stock solution in water

Standard solution E: 0.012 mg/mL of USP Methylprednisolone RS from Standard stock solution in water

Sample solution: Pass a portion of the solution under test through a suitable [Ký tự không đọc được]lter of 0.45-µm pore size.

Instrumental conditions

Mode: UV

Analytical wavelength: 246 nm

Cell: 1 cm

Blank: Water

System suitability

Samples: Standard solution A, Standard solution B, Standard solution C, Standard solution D, and Standard solution E

Suitability requirements

Correlation coefficient: NLT 0.99, as determined from the linear calibration constructed in the Analysis

Analysis

Samples: Standard solution A, Standard solution B, Standard solution C, Standard solution D, Standard solution E, Sample solution, and Blank

Determine the responses for Standard solution A, Standard solution B, Standard solution C, Standard solution D, and Standard solution E.

Construct a linear calibration curve by plotting response values of Standard solution A, Standard solution B, Standard solution C,

Standard solution D, and Standard solution E versus their corresponding concentrations in mg/mL. Determine the concentration (C) in

mg/mL of methylprednisolone (C₂₂H₃₀O₅) in the portion of Tablets taken from the calibration curve.

Calculate the percentage of the labeled amount of methylprednisolone (C₂₂H₃₀O₅) dissolved:

Result = C × V × (1 / L) × 100

C = concentration of methylprednisolone in the Sample solution (mg/mL), as determined from the calibration curve

V = volume of Medium, 500 mL

L = label claim (mg/Tablet)

Tolerances: NLT 80% (Q) of the labeled amount of methylprednisolone (C₂₂H₃₀O₅) is dissolved. ▲ (RB 1-Jun-2022)

Uniformity of Dosage Units 〈905〉: Meet the requirements

Procedure for content uniformity

Mobile phase, Solution A, Internal Standard solution, Standard solution, Chromatographic system, and System suitability: Proceed as

directed in the Assay.

Sample solution: Place 1 Tablet in a suitable container. For tablet-labeled strengths of 10 mg or less, add 0.5 mL of water. For tablet-labeled

strengths greater than 10 mg, add 1.0 mL of water. Allow the Tablet to stand for about 2 min, then swirl the container to disperse the

Tablet. Add 5.0 mL of Internal standard solution for each milligram of labeled Tablet strength, shake for 15 min, and pass a portion of

solution through a suitable [Ký tự không đọc được]lter or centrifuge a portion of the solution and analyze the clear supernatant.

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of methylprednisolone (C₂₂H₃₀O₅) in the Tablet taken:

Result = (Rᵤ / Rₛ) × (Cₛ / Cᵤ) × 100

Rᵤ = peak response ratio of methylprednisolone to prednisone from the Sample solution

Rₛ = peak response ratio of methylprednisolone to prednisone from the Standard solution

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

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

5 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight containers.

Add the following:

▲Labeling: When more than one Dissolution Test is given, the labeling states the test used only if Test 1 is not used.▲ (RB 1-Jun-2022)

USP Reference Standards 〈11〉

USP Methylprednisolone RS