Packaging and storage—
Preserve in tight, light-resistant containers, and store at a temperature between 15
and 30
.
Clarity of solution—
Dissolve 1.0 g in 30 mL of hot water, and observe without delay: the solution initially is clear.
Identification—
B:
Dissolve 0.5 g of propafenone hydrochloride in 50 mL of water with heating. Adjust with 0.1 N sodium hydroxide to a pH of 9.5 to 10.0: a precipitate is formed. Cool the mixture, and filter. Add 1 mL of 6 N nitric acid and 2 to 3 drops of 0.1 N silver nitrate to the filtrate: a precipitate is formed, which dissolves upon the addition of a few drops of ammonium hydroxide.
pH 
791
:
between 5.0 and 6.2 in a solution (1 in 200).
Loss on drying 731—
Dry it at 105
to constant weight; it loses not more than 0.5% of its weight.
Heavy metals, Method II 231:
20 ppm.
Limit of methanol and acetone—
Proceed as directed for
Test Preparation and
Chromatographic System in
Method V under
Organic Volatile Impurities 467.
Standard preparation—
Prepare a solution, in dimethyl sulfoxide, containing 2.0 µg of methanol and 20.0 µg of acetone.
Procedure—
Separately inject equal volumes (about 1 µL) of the Standard preparation and the Test preparation into the chromatograph, record the chromatograms, and measure the peak responses. Identify, based on retention time, any peaks present in the chromatogram of the Test preparation, and calculate the amounts of methanol and acetone present. Not more than 100 ppm of methanol and 1000 ppm of acetone are found.
Chromatographic purity—
Mobile phase—
Prepare a filtered and degassed mixture of 2.5 mM tetrabutylammonium hydrogen sulfate and acetonitrile (16:9). Make adjustments if necessary (see
System Suitability under
Chromatography 621).
Diluent—
Prepare a mixture of acetonitrile and water (9:1).
Standard solution—
Dissolve an accurately weighed quantity of USP Propafenone RS in Diluent, and dilute quantitatively, and stepwise if necessary, with Diluent to obtain a solution having a known concentration of about 5 µg per mL.
Test solution—
Transfer about 50 mg of Propafenone Hydrochloride, accurately weighed, to a 50-mL volumetric flask, dissolve in 5 mL of Diluent, dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)—
The liquid chromatograph is equipped with a 222-nm detector and a 3.9-mm × 15-cm column that contains packing L10. The flow rate is about 1.0 mL per minute. Chromatograph the
Standard solution, and record the peak responses as directed for
Procedure: the column efficiency is not less than 2000 theoretical plates; and the relative standard deviation for replicate injections is not more than 15%.
Procedure—
Separately inject a volume (about 10 µL) of the Standard solution and the Test solution into the chromatograph, and allow the Test solution to elute for not less than eight times the retention time of propafenone. Record the chromatogram, and measure the peak responses for all the peaks: the sum of the peak responses, other than that of propafenone, in the chromatogram of the Test solution is not more than two times the propafenone response obtained from the Standard solution (1.0%); and no other peak response, other than that of propafenone, in the chromatogram of the Test solution is greater than the propafenone response obtained from the Standard solution (0.5%).
Assay—
Transfer about 250 mg of Propafenone Hydrochloride, accurately weighed, to a 125-mL flask. Dissolve in 30 mL of methanol, add 15 mL of
mercuric acetate TS, and titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 37.79 mg of C
21H
27NO
3·HCl.
;)
