Valrubicin Intravesical Solution
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).
•  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.
•  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%
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
rU== peak response from the Sample solution
rS== peak response from the Standard solution
CS== concentration of USP Valrubicin RS in the Standard solution (mg/mL)
CU== nominal concentration of valrubicin in the Sample solution (mg/mL)
Acceptance criteria:  95.0%–105.0%
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
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
rU== peak area for each impurity
rT== sum of the peak areas of all the peaks
[Note—Do 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
Name Relative
NMT (%)
Valrubicin impurity 1 0.11 0.5
Valrubicin impurity 2 0.16 0.8
Valrubicin impurity 3 0.51 0.8
Valrubicin impurity 4 0.71 0.8
Any unspecified
•  Bacterial Endotoxins Test 85: NMT 0.14 USP Endotoxin Unit/mg of valrubicin
•  pH 791: 4.0–7.0 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
•  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.
•  USP Reference Standards 11
USP Endotoxin RS
USP Valrubicin RS Click to View Structure
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Ahalya Wise, M.S.
Senior Scientific Liaison
(SM12010) Monographs - Small Molecules 1
85 Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison
(GCM2010) General Chapters - Microbiology
Reference Standards RS Technical Services
USP35–NF30 Page 4996
Pharmacopeial Forum: Volume No. 34(6) Page 1486