Packaging and storage
Preserve in tight containers. Store at 25
, excursions permitted between 15
and 30
.
Related compounds
0.01 M Sodium 1-octanesulfonate solution
Dissolve 1.0814 g of 1-sodium octanesulfonate in 500 mL of water.
Mobile phase
Prepare a mixture of
0.01 M Sodium 1-octanesulfonate solution, acetonitrile, glacial acetic acid, and triethylamine (81:19:2:0.5). Make adjustments if necessary (see
System Suitability under
Chromatography 621).
Standard solution
Dissolve an accurately weighed quantity of
USP Bretylium Tosylate RS in
Mobile phase, and dilute quantitatively, and stepwise if necessary, to obtain a solution having a known concentration of about 20 µg per mL.
Test solution
Transfer about 200 mg of Bretylium Tosylate, 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 265-nm detector and a 4.6-mm × 25-cm column that contains packing L11. The flow rate is about 1.9 mL per minute. Chromatograph the
Standard solution, record the chromatograms, and record the peak responses as directed for
Procedure: the relative standard deviation for replicate injections is not more than 3.0%.
Procedure
Separately inject equal volumes (about 30 µL) of the Test solution and the Standard solution into the chromatograph, record the chromatograms, and measure the peak responses. The relative retention times are about 0.25, 0.74, 1.0, 1.27, 1.40 for tosylate ion, o-bromobenzyldimethylamine, bretylium, m-bromobenzyldimethylamine, and p-bromobenzyldimethylamine, respectively. The sum of the responses for all the peaks, excluding those of the bretylium and tosylate peaks, from the Test solution is not more than two times the bretylium response from the Standard solution (2%); and no individual peak response is greater than that of the bretylium peak from the Standard solution (1%).
Assay
Dissolve about 300 mg of Bretylium Tosylate, accurately weighed, in 50 mL of dioxane in a conical flask. Add 2 drops of
crystal violet TS, and titrate with 0.025 N perchloric acid in dioxane VS to a blue-green endpoint. Perform a blank determination (see
Titrimetry 541), and make any necessary correction. Each mL of 0.025 N perchloric acid is equivalent to 10.36 mg of C
18H
24BrNO
3S.