(lee'' voe ka bas' teen hye'' droe klor' ide).
4-Piperidinecarboxylic acid, 1-[4-cyano-4-(4-fluorophenyl)cyclohexyl]-3-methyl-4-phenyl-, monohydrochloride, ()-[1(cis),3,4]-;
()-trans-1-[cis-4-Cyano-4-(p-fluorophenyl)cyclohexyl]-3-methyl-4-phenylisonipecotic acid monohydrochloride [79547-78-7].
Levocabastine Hydrochloride contains NLT 98.5% and NMT 101.5% of C26H29FN2O2·HCl, calculated on the dried basis.
• B. Identification TestsGeneral, Chloride 191: Meets the requirements
• C. Optical Rotation, Specific Rotation 781S: Meets the requirements
Sample solution: Dissolve 175 mg of Levocabastine Hydrochloride in 50 mL of alcohol, and add 5.0 mL of 0.01 N hydrochloric acid.
(See Titrimetry 541.)
Mode: Direct titration
Titrant: 0.1 N sodium hydroxide VS
Endpoint detection: Potentiometric
Sample: Sample solution
The volume of titrant required to titrate Levocabastine Hydrochloride is the difference between the first and third endpoints. Perform a blank determination and make any necessary correction. Each mL of 0.1 N sodium hydroxide VS is equivalent to 22.85 mg of C26H29FN2O2·HCl.
Acceptance criteria: 98.5%101.5% on the dried basis
• Residue on Ignition 281: NMT 0.1%, based on a sample weight of about 1.000 g
[NotePrepare solutions immediately before use. ]
Diluent: 2 mg/mL of sodium hydroxide in water
Solution A: Dissolve 1.39 g of boric acid in water, and adjust with 1 N sodium hydroxide to a pH of 9.0. Dilute with water to 100 mL.
Run buffer: Dissolve 1.08 g of sodium dodecyl sulfate and 650 mg of hydroxypropyl--cyclodextrin in 5 mL of isopropyl alcohol, then dilute with Solution A to 50 mL.
System suitability solution: 12.5 µg/mL of USP Levocabastine Hydrochloride RS and 12.5 µg/mL of USP Levocabastine Related Compound A RS in Diluent
Standard solution: Dilute 5.0 mL of the Sample solution with Diluent to 100 mL. Dilute 1.0 mL of this solution with Diluent to 10 mL to obtain a solution containing 12.5 µg/mL of Levocabastine Hydrochloride.
Sample solution: 2.5 mg/mL of Levocabastine Hydrochloride in Diluent
Capillary electrophoresis system
Detector: UV 214 nm
Column: 75-µm × 50-cm uncoated fused-silica capillary column
Column temperature: 50
Current: See the gradient table below.
[NoteBefore performing the System suitability, equilibrate the capillary column with Diluent for 2 min, then equilibrate with Run buffer for at least 5 min. ]
Sample: System suitability solution
[NoteThe relative migration times for levocabastine and levocabastine related compound A are approximately 1.0 and 1.07, respectively. ]
Resolution: NLT 4 between levocabastine and levocabastine related compound A
[NoteIf necessary, adjust the current gradient to achieve the required resolution. ]
Samples: Diluent (blank), Standard solution, and Sample solution
Separately inject equal volumes (pressure of 3450 Pa for 5 s) of the Samples, and record the peak responses.
[NoteDisregard any peak originating from the Diluent. Disregard any peak with an area of less than 0.1 times the major peak area of the Standard solution (0.05%). ]
Acceptance criteria: The area for any peak in the Sample solution, other than the major peak, is not greater than the major peak area of the Standard solution (0.5%); and the sum of all peak areas in the Sample solution, except for the major peak, is not greater than twice the major peak area of the Standard solution (1.0%).
• Optical Rotation, Specific Rotation 781S: 102 to 106 at 20
Sample solution: 10 mg/mL in methanol
• Loss on Drying 731: Dry about 1.000 g of the sample at 105 to constant weight: it loses NMT 0.5% of its weight.
• Packaging and Storage: Preserve in well-closed containers. Protect from light.
• USP Reference Standards 11
USP Levocabastine Related Compound A RS
Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 3664Pharmacopeial Forum: Volume No. 36(1) Page 116