(doe las' e tron mes' i late).
1H-Indole-3-carboxylic acid, octahydro-3-oxo-2,6-methano-2H-quinolizin-8-yl ester, (2,6,8,9a)-, monomethanesulfonate monohydrate;
Indole-3-carboxylic acid, ester with (8r)-hexahydro-8-hydroxy-2,6-methano-2H-quinolizin-3(4H)-one, monomethanesulfonate monohydrate [115956-13-3].
Dolasetron Mesylate contains NLT 98.0% and NMT 102.0% of C19H20N2O3·CH4O3S·H2O, calculated on the as-is basis.
• B. Procedure
Sample solution: 1 mg/mL
Analysis: Transfer 510 mg of 5,5'-methylenedisalicylic acid to a clean crucible, and heat in an oven at 150 for 5 min. Remove from the oven, and add 10 drops of the Sample solution. Return to the oven, and evaporate to dryness.
Acceptance criteria: A red or pink color (presence of methanesulfonic acid) develops in the white residue.
Mobile phase: Acetonitrile, water, and 1 M ammonium formate (450:440:110), adding 0.19 mL of triethylamine to the acetonitrile portion
Standard solution: 0.04 mg/mL and 0.004 mg/mL respectively of USP Dolasetron Mesylate RS and indole-3-carboxylic acid in Mobile phase
Sample solution: 0.04 mg/mL of Dolasetron Mesylate in Mobile phase
Detector: UV 285 nm
Column: 4.6-mm × 15-cm; packing L1
Flow rate: 1 mL/min
Injection size: 20 µL
Sample: Standard solution
Resolution: NLT 4 between indole-3-carboxylic acid and dolasetron mesylate
Tailing factor: NMT 1.8
Relative standard deviation: NMT 1.5% for replicate injections
Samples: Standard solution and Sample solution
Calculate the percentage of C19H20N2O3·CH4O3S·H2O in the Dolasetron Mesylate taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria: 98.0%102.0% on the as-is basis
0.01 M Dibasic ammonium phosphate solution: 1.32 g/L of dibasic ammonium phosphate. Adjust with 2.0 M phosphoric acid to a pH of 7.0.
Diluent: Acetonitrile and water (1:4)
Solution A: Acetonitrile and 0.01 M Dibasic ammonium phosphate solution (53:1000), filtered and degassed
Solution B: Acetonitrile and 0.01 M Dibasic ammonium phosphate solution (795:295), filtered and degassed
Mobile phase: See the gradient table below.
System suitability solution: 0.004 mg/mL and 0.03 mg/mL, respectively, of indole and USP Dolasetron Mesylate RS in Diluent
Standard solution A: 0.03 mg/mL of USP Dolasetron Mesylate RS in Diluent
Standard solution B: 6 mg/mL and 0.0072 mg/mL, respectively, of USP Dolasetron Mesylate RS and USP Dolasetron Mesylate Related Compound A RS in Diluent
Sample solution: 6 mg/mL of Dolasetron Mesylate in Diluent
Detector: UV 210 nm
Column: 4.6-mm × 25-cm; packing L7
Flow rate: 1.5 mL/min
Injection size: 100 µL
Resolution: NLT 1.5 between the first eluting peak, indole, and the second eluting peak, dolasetron mesylate from the System suitability solution. [NoteIf the dolasetron mesylate peak is found to elute before the indole peak, condition the column as follows: fill up the column with Solution A, plug the column, and place the column in a convection oven at 105 for about 16 h. Retest the column. ]
Relative standard deviation: NMT 5.0% for replicate injections of Standard solution A
Samples: Standard solution A, Standard solution B, and Sample solution
Calculate the percentage of dolasetron mesylate related compound A in the Dolasetron Mesylate taken:
Result = (rU/rS) × (CS/CU) × (Mr1/Mr2) × 100
Calculate the percentage of each impurity (other than dolasetron mesylate related compound A) in the portion of Dolasetron Mesylate taken:
Result = (rU/rS) × (CS/CU) × 100
Individual impurities: NMT 0.1%
Total impurities: NMT 0.3%
[NoteThe reporting level for impurities is 0.05%. ]
• Water Determination, Method Ia 921: Between 3.5% and 4.7%
• Packaging and Storage: Preserve in well-closed containers, protected from light.
• USP Reference Standards 11
USP Dolasetron Mesylate Related Compound A RS
Hexahydro-8-hydroxy-2,6-methano-2H-quinolizin-3 (4H)-one, hydrochloride.
Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 2963Pharmacopeial Forum: Volume No. 35(2) Page 272