Deferoxamine Mesylate
(de fer ox' a meen mes' i late).
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) [138-14-7]. DEFINITION
Change to read:
Deferoxamine Mesylate contains NLT 93.0%(RB 1-May-2011) and NMT 102.0% of C25H48N6O8·CH4O3S, calculated on the anhydrous basis.
IDENTIFICATION
• B.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
Change to read:
• 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.
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
Mode:
LC
Detector:
UV 220 nm
Column:
4.6-mm × 7.5-cm; 3.5-µm packing L1
Column temperature:
32
Autosampler temperature:
5
Flow rate:
1.5 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of deferoxamine mesylate (C25H48N6O8·CH4O3S) in the portion of Deferoxamine Mesylate taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
93.0%(RB 1-May-2011)102.0% on the anhydrous basis
IMPURITIES
• Residue on Ignition 281:
NMT 0.1%, 2.0 g being used
• Chloride and Sulfate, Chloride 221:
A 1.2-g portion shows no more chloride than corresponds to 0.20 mL of 0.020 N hydrochloric acid (NMT 0.012%).
• Chloride and Sulfate, Sulfate 221:
A 0.5-g portion shows no more sulfate than corresponds to 0.20 mL of 0.020 N sulfuric acid (NMT 0.04%).
• Heavy Metals, Method II 231:
NMT 10 ppm
Change to read:
• 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. [NoteUSP 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 = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
See Table 2.
[NoteThe reporting level for impurities is 0.04%. ]
Table 2
SPECIFIC TESTS
• pH 791:
4.06.0, in a solution (1 in 100)
• Water Determination, Method I 921:
NMT 2.0%
• Sterility Tests 71:
Where the label states that Deferoxamine Mesylate is sterile, it meets the requirements.
• Bacterial Endotoxins Test 85:
Where the label states that Deferoxamine Mesylate is sterile or must be subjected to further processing during the preparation of injectable dosage forms, it contains NMT 0.33 USP Endotoxin Unit/mg of deferoxamine mesylate.
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight containers. Store in a cold place.
• Labeling:
Where it is intended for use in preparing injectable dosage forms, the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 2813
Pharmacopeial Forum: Volume No. 35(4) Page 847
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