Dexbrompheniramine Maleate

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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1 DEFINITION 

Dexbrompheniramine Maleate contains NLT 98.0% and NMT 102.0% of dexbrompheniramine maleate (C₁₆H₁₉BrN₆ . C₄H₄O₄), calculated on the dried basis. 

2 IDENTIFICATION

Change to read: 

A. Spectroscopic Identification Tests 〈197〉, Infrared Spectroscopy: 197M (CN 1-May-2020) 

B. The retention times of the maleic acid and dexbrompheniramine peaks of the Sample solution correspond to those of the Standard solution, as obtained in the Assay. 

3 ASSAY 

3.1 Procedure 

Solution A: 5.44 g/L of monobasic potassium phosphate. Adjust with phosphoric acid to a pH of 3.0 ± 0.1. 

Solution B: Acetonitrile 

Diluent: Acetonitrile and Solution A (5:95) 

System suitability stock solution: 0.02 mg/mL each of USP Pheniramine Maleate RS, USP Chlorpheniramine Maleate RS, and USP Chlorpheniramine Related Compound B RS in Diluent. Sonicate for 1 min. 

System suitability solution: 0.5 mg/mL of USP Dexbrompheniramine Maleate RS and 2 µg/mL each of USP Pheniramine Maleate RS, USP Chlorpheniramine Maleate RS, and USP Chlorpheniramine Related Compound B RS in Diluent, prepared as follows. Transfer 5.0 mg of USP Dexbrompheniramine Maleate RS to a 10-mL volumetric ask, add 5.0 mL of Diluent and 1.0 mL of the System suitability stock solution, and dilute with Diluent to volume. 

Standard solution: 0.5 mg/mL of USP Dexbrompheniramine Maleate RS in Diluent. Sonicate for 1 min. 

Sample solution: 0.5 mg/mL of Dexbrompheniramine Maleate in Diluent. Sonicate for 1 min. 

Mobile phase: See Table 1. 

Table 1 

Chromatographic system 

(See Chromatography 〈621〉, System Suitability.) 

Mode: LC 

Detector: UV 225 nm 

Column: 4.6-mm × 25-cm; 5-µm packing L1 

Column temperature: 30° 

Flow rate: 1 mL/min 

Injection volume: 10 µL 

System suitability 

Samples: System suitability solution and Standard solution 

Suitability requirements 

[Note—The relative retention times for maleic acid and dexbrompheniramine are 0.18 and 1.0, respectively.] 

Resolution: NLT 1.5 between chlorpheniramine and dexbrompheniramine; NLT 2.0 between chlorpheniramine related compound B and pheniramine, System suitability solution 

Tailing factor: NMT 2.0, Standard solution 

Relative standard deviation: NMT 0.73%, Standard solution 

Analysis 

Samples: Standard solution and Sample solution 

Calculate the percentage of dexbrompheniramine maleate (C₁₆H₁₉BrN₆ . C₄H₄O₄) in the portion of Dexbrompheniramine Maleate taken: 

Result = (r_u/r_s) x (C_s/C_u) × 100 

r_u = peak response from the Sample solution 

r_s = peak response from the Standard solution 

C_s = concentration of USP Dexbrompheniramine Maleate RS in the Standard solution (mg/mL) 

C_u = concentration of Dexbrompheniramine Maleate in the Sample solution (mg/mL) 

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

4 IMPURITIES 

Residue on Ignition 〈281〉: NMT 0.2% 

Organic Impurities 

Solution A, Diluent, System suitability solution, Mobile phase, and Chromatographic system: Proceed as directed in the Assay. Standard solution: 2.7 µg/mL of USP Dexbrompheniramine Maleate RS in Diluent, equivalent to 2.0 µg/mL of dexbrompheniramine. Sonicate for 1 min. 

Sensitivity solution: 0.74 µg/mL of USP Pheniramine Maleate RS in Diluent 

Sample solution: 0.5 mg/mL of Dexbrompheniramine Maleate in Diluent. Sonicate for 1 min. 

System suitability 

Samples: System suitability solution, Standard solution, and Sensitivity solution 

Suitability requirements 

Resolution: NLT 1.5 between chlorpheniramine and dexbrompheniramine; NLT 2.0 between chlorpheniramine related compound B and pheniramine, System suitability solution 

Signal-to-noise ratio: NLT 10, Sensitivity solution 

Relative standard deviation: NMT 5.0%, Standard solution 

Analysis 

Sample: Sample solution 

[Note—Exclude the maleic acid peak at the relative retention time 0.18.] 

Calculate the percentage of each impurity in the portion of Dexbrompheniramine Maleate taken: 

Result = (r_U/r_T) × 100 

r_U = peak response of each impurity 

r_T = sum of the responses of all the peaks 

Acceptance criteria 

Total impurities: NMT 2.0% 

5 SPECIFIC TESTS 

5.1 Loss on Drying 〈731〉 

Analysis: Dry at 65° for 4 h. 

Acceptance criteria: NMT 0.5% 

5.2 Optical Rotation, Specific Rotation〈781S〉 

Sample solution: 50 mg/mL, in dimethylformamide 

Acceptance criteria: +35.0° to +38.5° 

6 ADDITIONAL REQUIREMENTS 

6.1 Packaging and Storage: Preserve in tight, light-resistant containers. 

6.2 USP Reference Standards 〈11〉 

USP Chlorpheniramine Maleate RS 

USP Chlorpheniramine Related Compound B RS 

Di(pyridin-2-yl)amine. 

C₁₀H₉N₃      171.20 

USP Dexbrompheniramine Maleate RS 

USP Pheniramine Maleate RS