Tripelennamine Hydrochloride

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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C₁₆H₂₁N₃ · HCI           291.82

1,2-Ethanediamine, N,N-dimethyl-N'-(phenylmethyl)-N-2-pyridinyl-, monohydrochloride;

2-[Benzyl[2-(dimethylamino) ethyl)amino]pyridine monohydrochloride    CAS RN^®: 154-69-8; UNII: FWV8GJ56ZN.

1 DEFINITION

Tripelennamine Hydrochloride contains NLT 98.0% and NMT 102.0% of tripelennamine hydrochloride (C₁₆H₂₁N₃ · HCI), calculated on the dried basis.

2 IDENTIFICATION

Change to read:

A. ^▲SPECTROSCOPIC IDENTIFICATION TESTS (197), Infrared Spectroscopy: 197A or 197K_{▲(CN 1-May-2020)}

B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay

C. IDENTIFICATION TESTS GENERAL (191), Chemical Identification Tests, Chloride: Meets the requirements

3 ASSAY

PROCEDURE

Solution A: 29 mM sodium 1-octanesulfonate solution

Mobile phase: Methanol, N.N-dimethyloctylamine, and Solution A (530:1:430), prepared as follows. Transfer 530 ml of methanol to a suitable container, add 1.0 ml. of N.N-dimethyloctylamine, and mix thoroughly. Add 430 mL of Solution A, mix, and adjust with phosphoric acid to a pH of 3.0.

Benzaldehyde stock solution: Transfer 1.0 mL of benzaldehyde to a 100-ml volumetric flask, and dilute with Mobile phase to volume.

Benzaldehyde solution: Transfer 5.0 mL of the Benzaldehyde stock solution to a 100-mL volumetric flask, and dilute with Mobile phase to volume.

System suitability stock solution: 0.5 mg/ml of 2-benzylaminopyridine in Mobile phase prepared as follows. Transfer 50 mg of 2-benzylaminopyridine to a 100-ml volumetric flask. Add 10 mL of methanol, sonicate to dissolve, and dilute with Mobile phase to volume.

System suitability solution: Transfer 5.0 mL of the System suitability stock solution to a 100-mL. volumetric flask. Add 5.0 mL of Benzaldehyde solution, and dilute with Mobile phase to volume.

Standard solution: 0.5 mg/mL of USP Tripelennamine Hydrochloride RS in Mobile phase

Sample solution: 0.5 mg/mL of Tripelennamine Hydrochloride in Mobile phase

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 242 nm

Column: 4.6-mm x 25-cm; 5-um packing L7

Column temperature: 35°

[NOTE-New columns are conditioned with Mobile phase overnight before the initial use, and may be reconditioned, as necessary, thereafter.]

Flow rate: 1 mL/min

Injection volume: 10 µL

System suitability

Samples: System suitability solution and Standard solution

[NOTE-The relative retention times for benzaldehyde and 2-benzylaminopyridine are 0.75 and 1.0, respectively.]

Suitability requirements

Resolution: NLT 3.5 between benzaldehyde and 2-benzylaminopyridine, System suitability solution

Tailing factor: NMT 1.5, Standard solution

Relative standard deviation: NMT 1.0%, Standard solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of tripelennamine hydrochloride (C₁₆H₂₁N₃ · HCI) in the portion of Tripelennamine Hydrochloride taken:

                         Result = (r_U/r_S) × (C_S/C_U)

r_U = peak response from the Sample solution 

r_S = peak response from the Standard solution 

C_S = concentration of USP Tripelennamine Hydrochloride RS in the Standard solution (mg/mL)

C_U = concentration of Tripelennamine Hydrochloride in the Sample solution (mg/mL)

Acceptance criteria: 98.0%-102.0% on the dried basis

4 IMPURITIES

4.1 RESIDUE ON IGNITION (281)

NMT 0.1%

4.2 ORGANIC IMPURITIES

Solution A, Mobile phase, System suitability solution, Standard solution, Sample solution, Chromatographic system, and System suitability: Proceed as directed in the Assay.

Analysis

Sample: Sample solution

Calculate the percentage of each impurity in the portion of Tripelennamine Hydrochloride taken:

                         Result = (r_U/r_T) x 100

r_U = peak response of each impurity from the Sample solution 

r_T = surn of all the peak responses from the Sample solution

Acceptance criteria

Each individual impurity: NMT 0.1%

Total impurities: NMT 1.0%

5 SPECIFIC TESTS

LOSS ON DRYING (731)

Analysis: Dry at 105° for 3 h.

Acceptance criteria: NMT 1.0%

6 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Preserve in well-closed, light-resistant containers.

USP REFERENCE STANDARDS (11)

USP Tripelennamine Hydrochloride RS