A: It meets the requirements under Identification—Organic Nitrogenous Bases 181.

B: It meets the requirements of the tests for Chloride 191.

Ion-pair solution, Mobile phase, and Benzaldehyde solution— Proceed as directed in the Assay.

Chromatographic system —Proceed as directed in the Assay. To evaluate system suitability requirements, use the System suitability preparation and the Standard preparation, as prepared in the Assay.

Test solution— Use the Assay preparation.

Procedure— Inject a volume (about 10 µL) of the Test solution into the chromatograph, record the chromatogram, and measure all of the peak responses. Calculate the percentage of each impurity in the portion of Tripelennamine Hydrochloride taken by the formula: in which ri is the peak response for each impurity, and rS is the sum of the responses for all the peaks: not more than 0.1% of any individual impurity is found; and not more than 1.0% of total impurities is found.

(Official January 1, 2007)

Ion-pair solution— Prepare a 29-mM sodium 1-octanesulfonate solution.

Mobile phase— Transfer 530 mL of methanol to a suitable container, add 1.0 mL of N,N-dimethyloctylamine, and mix thoroughly. Add 430 mL of the Ion-pair solution, mix, and adjust with phosphoric acid to a pH of 3.0. Make adjustments if necessary (see System Suitability under Chromatography 621).

Benzaldehyde solution— Transfer 1.0 mL of benzaldehyde to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix. Transfer 5.0 mL of the solution so obtained to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix.

System suitability preparation— Transfer about 50 mg of 2-benzylaminopyridine, accurately weighed, to a 100-mL volumetric flask, add 10 mL of methanol, sonicate to dissolve, dilute with Mobile phase to volume, and mix. Transfer 5.0 mL of the solution so obtained to a 100-mL volumetric flask, add 5.0 mL of Benzaldehyde solution, dilute with Mobile phase to volume, and mix.

Standard preparation— Dissolve an accurately weighed quantity of USP Tripelennamine Hydrochloride RS in Mobile phase, and dilute quantitatively, and stepwise if necessary, with Mobile phase to obtain a solution having a known concentration of about 0.5 mg per mL.

Assay preparation— Transfer about 50 mg of Tripelennamine Hydrochloride, accurately weighed, to a 100-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.

Chromatographic system (see Chromatography 621)— The liquid chromatograph is equipped with a 242-nm detector and a 4.6-mm × 25-cm column that contains packing L7. The flow rate is about 1 mL per minute. The column temperature is maintained at 35. [NOTE—New columns are conditioned with Mobile phase overnight before the initial use and may be reconditioned, as necessary, thereafter.] Chromatograph the System suitability preparation, and record the peak responses as directed for Procedure: the relative retention times are about 0.75 for benzaldehyde and 1.0 for 2-benzylaminopyridine; and the resolution, R, between benzaldehyde and 2-benzylaminopyridine is not less than 3.5. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency is not less than 10,000 theoretical plates; and the relative standard deviation for replicate injections is not more than 1.0%.

Procedure— Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in percentage, of C16H21N3·HCl in the portion of Tripelennamine Hydrochloride taken by the formula: in which CU and CS are the concentrations, in mg per mL, of the Assay preparation and of USP Tripelennamine Hydrochloride RS in the Standard preparation, respectively; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.