Valrubicin Intravesical Solution
DEFINITION
Valrubicin Intravesical Solution is a sterile solution of Valrubicin in a suitable vehicle. It contains NLT 95.0% and NMT 105.0% of the labeled amount of valrubicin (C34H36F3NO13).
IDENTIFICATION
• A. Thin-Layer Chromatographic Identification Test 201
Standard solution:
Use the Standard solution, prepared as directed in the Assay, suitably diluted with methanol.
Sample solution:
Use the Sample solution, prepared as directed in the Assay, suitably diluted with methanol.
Solution A:
0.1 M ammonium formate. Adjust with formic acid to a pH of 4.0.
Developing solvent system:
Acetonitrile and Solution A (45:55)
• 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
• Procedure
Buffer:
0.1 M ammonium formate. Adjust with formic acid to a pH of 4.0.
Mobile phase:
Acetonitrile and Buffer (45:55)
Standard solution:
0.2 mg/mL of USP Valrubicin RS in methanol
Sample solution:
Equivalent to 0.2 mg/mL of valrubicin, from Intravesical Solution in methanol
Chromatographic system
Mode:
LC
Detector:
UV 254 mm
Column:
5-mm × 10-cm; 4-µm packing L1, and a guard column
Flow rate:
2.5 mL/min
Injection size:
10 µL
System suitability
Sample:
Standard solution
Suitability requirements
Relative standard deviation:
NMT 2%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of C34H36F3NO13 in the Intravesical Solution taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
95.0%105.0%
IMPURITIES
Organic Impurities
• Procedure
Buffer, Mobile phase, and Chromatographic system:
Proceed as directed in the Assay.
Sample solution:
0.2 mg/mL of valrubicin in methanol
Analysis
Sample:
Sample solution
Measure the areas for the major peaks. Calculate the percentage of each impurity in the portion of Intravesical Solution taken:
Result = (rU/rT) × 100
[NoteDo not consider any peaks due to solvent or excipients. ]
Acceptance criteria
Individual impurities:
See Impurity Table 1.
Total impurities:
NMT 3.5%
Impurity Table 1
SPECIFIC TESTS
• Bacterial Endotoxins Test 85:
NMT 0.14 USP Endotoxin Unit/mg of valrubicin
• pH 791:
4.07.0 in a solution equivalent to 66.7 mg/mL of valrubicin in 0.9% sodium chloride solution
• Other Requirements:
Meets the requirements under Injections 1
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in single-dose or multiple-dose containers, preferably of Type I glass. Store in a refrigerator.
• Labeling:
Label it to indicate that it is not intended for intravenous or intramuscular injection but is to be used for intravesical instillation.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 4996
Pharmacopeial Forum: Volume No. 34(6) Page 1486
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