Deferoxamine Mesylate

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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C₂₅H₄₈N₆O₈·CH₄O₃S    656.79

Butanediamide, N′-[5-[[4-[[5-(acetylhydroxyamino)pentyl]amino]-1,4-dioxobutyl]hydroxyamino]pentyl]-N-(5-aminopentyl)-N-hydroxy-, monomethanesulfonate;

N-[5-[3-[(5-Aminopentyl)hydroxycarbamoyl]propionamido]pentyl]-3-[[5-(N-hydroxyacetamido)pentyl]carbamoyl]propionohydroxamic acid monomethanesulfonate (salt)

CAS RN®: 138-14-7; UNII: V9TKO7EO6K.

1 DEFINITION

Deferoxamine Mesylate contains NLT 93.0% and NMT 102.0% of deferoxamine mesylate (C₂₅H₄₈N₆O₈·CH₄O₃S), calculated on the anhydrous basis.

2 IDENTIFICATION

Change to read:

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

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

3.1 Procedure

Solution A: 1.32 g/L of dibasic ammonium phosphate in water. Adjust with phosphoric acid to a pH of 3.0.

Solution B: Acetonitrile and Solution A (1:1)

Mobile phase: See Table 1.

Diluent: Acetonitrile and water (6:94)

Standard solution: 1.0 mg/mL of USP Deferoxamine Mesylate RS in Diluent

Sample solution: 1.0 mg/mL of Deferoxamine Mesylate in Diluent

Chromatographic system

• (See Chromatography 〈621〉, System Suitability.)
• Mode: LC
• Detector: UV 220 nm
• Column: 4.6-mm × 7.5-cm; 3.5-µm packing L1
• Temperatures
• Column: 32°
• Autosampler: 5°
• Flow rate: 1.5 mL/min
• Injection volume: 20 µL
• System suitability
• Sample: Standard solution
• Suitability requirements
• Relative standard deviation: NMT 0.73%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of deferoxamine mesylate (C₂₅H₄₈N₆O₈·CH₄O₃S) in the portion taken:

Result = (r_u/r_s) × (C_s/C_u) × 100

r_u = peak response of deferoxamine from the Sample solution

r_s = peak response of deferoxamine from the Standard solution

C_s = concentration of the Standard solution (mg/mL)

C_u = concentration of the Sample solution (mg/mL)

Acceptance criteria: 93.0%–102.0% on the anhydrous basis

4 IMPURITIES

4.1 Residue on Ignition 〈281〉

NMT 0.1%, 2.0 g being used

4.2 Chloride and Sulfate, Chloride 〈221〉

NMT 0.012%; a 1.2-g portion shows no more chloride than corresponds to 0.20 mL of 0.020 N hydrochloric acid.

4.3 Chloride and Sulfate, Sulfate 〈221〉

NMT 0.04%; a 0.5-g portion shows no more sulfate than corresponds to 0.20 mL of 0.020 N sulfuric acid.

4.4 Organic Impurities

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

Standard stock solution: Use the Standard solution, prepared as directed in the Assay. [Note-USP Deferoxamine Mesylate RS contains impurity A as a minor component.]

Standard solution: 0.01 mg/mL of USP Deferoxamine Mesylate RS in Diluent from the Standard stock solution

System suitability

• Samples: Standard stock solution and Standard solution
• Suitability requirements
• Resolution: NLT 2.0 between the impurity A and deferoxamine peaks, Standard stock solution
• Relative standard deviation: NMT 5.0% for the deferoxamine peak, Standard solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of each impurity in the portion of Deferoxamine Mesylate taken:

Result = (r_u/r_s) × (C_s/ C_u) × 100

r_u = peak response of each impurity from the Sample solution

r_s = peak response of deferoxamine from the Standard solution

C_s = concentration of the Standard solution (mg/mL)

C_u = concentration of the Sample solution (mg/mL)

Acceptance criteria: see Table 2

[Note-The reporting level for impurities is 0.04%.]

a Des-methylene impurity (Desferrioxamine A₁ and/or other desferrioxamines).

b All des-methylene impurities that elute in the 0.85–0.87 range should be treated as a single impurity. Where the cluster of unresolved peaks in this range is present, it should be integrated together as one peak to determine compliance.

c The acceptance criterion of NMT 3.0% applies to the sum of the peaks in the specied range.

5 SPECIFIC TESTS

pH 〈791〉: 4.0–6.0, in a solution (1 in 100)

Water Determination, Method I 〈921〉: NMT 2.0%

Sterility Tests 〈71〉: Meets requirements if labeled sterile

Bacterial Endotoxins Test 〈85〉: NMT 0.33 USP EU/mg if sterile or for injectable preparation

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight containers. Store at room temperature.

Labeling: If intended for injectable dosage form preparation, label indicates sterile or requires further processing.

USP Reference Standards 〈11〉

USP Deferoxamine Mesylate RS