Dissolution 711
Medium:
water; 500 mL.
Apparatus 1:
50 rpm.
Time:
20 minutes.
Determine the amount of C13H17N·HCl dissolved using the following method.
Monobasic ammonium phosphate solution
Dissolve 11.5 g of monobasic ammonium phosphate in 1000 mL of water. Adjust with 85% phosphoric acid to a pH of 3.1.
Mobile phase
Prepare a filtered and degassed mixture of
Monobasic ammonium phosphate solution and acetonitrile (4:1). Make adjustments if necessary (see
System Suitability under
Chromatography 621).
Standard solution
Transfer 25.0 mg, accurately weighed, of
USP Selegiline Hydrochloride RS to a 50-mL volumetric flask. Dissolve in and dilute with water to volume, and mix. Pipet 2.0 mL of this solution into a 100-mL volumetric flask, dilute with water to volume, and mix.
Test solution
At 20 minutes withdraw a 10-mL portion of the solution under test and centrifuge for 10 minutes at 3500 rpm.
Chromatographic system
The liquid chromatograph is equipped with a 205-nm detector and a 3.9-mm × 30-cm column that contains packing L1. Chromatograph the Standard solution, and record the peak responses. The relative standard deviation for replicate injections is not more than 2.0%.
Procedure
Separately inject equal volumes (about 15 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the amount of C13H17N·HCl dissolved.
Tolerances
Not less than 80% (Q) of the labeled amount of C13H17N·HCl is dissolved in 20 minutes.
Chromatographic purity
Standard solution
Transfer 10.0 mL of the
System suitability solution to a 100-mL volumetric flask, dilute with
Mobile phase to volume, and mix. Transfer 10.0 mL of this solution to a 20-mL volumetric flask, dilute with
Mobile phase to volume, and mix.
Test solution
Use a portion of the supernatant obtained from the Assay preparation.
Procedure
Proceed as directed in the test for
Chromatographic purity under
Selegiline Hydrochloride. Calculate the percentage of each impurity, excluding methamphetamine hydrochloride, in the portion of Tablets taken by the formula:
5000(C / W)(ri / rs),
in which
W is the weight, in mg, of the labeled content of selegiline hydrochloride in the portion of Tablets taken to prepare the
Test solution, and the other terms are as defined therein. Not more than 0.5% of any individual impurity is found, and the sum of all impurities, excluding methamphetamine hydrochloride, is not more than 2.0%.
Limit of methamphetamine hydrochloride
Standard solution
Transfer 10.0 mL of the
System suitability solution to a 50-mL volumetric flask, dilute with
Mobile phase to volume, and mix.
Procedure
Proceed as directed in the test for
Chromatographic purity under
Selegiline Hydrochloride. Calculate the percentage of methamphetamine hydrochloride in the portion of Tablets taken by the formula:
5000(C / W)(rU / rS),
in which
C is the concentration, in mg per mL, of
USP Methamphetamine Hydrochloride RS in the
Standard solution,
W is the weight, in mg, of the labeled content of selegiline hydrochloride in the portion of Tablets taken to prepare the
Test solution, and
rU and
rS are the methamphetamine peak responses obtained from the
Test solution and the
Standard solution, respectively. Not more than 2.0% of methamphetamine hydrochloride is found.
Assay
Assay preparation
Weigh and powder not less than 20 Tablets. Transfer an accurately weighed portion of the powder equivalent to about 50 mg of selegiline hydrochloride to a 50-mL volumetric flask. Add 40 mL of
Mobile phase, sonicate for 10 minutes, dilute with
Mobile phase to volume, and mix. Centrifuge a 25-mL aliquot of this solution at 3500 rpm for 10 minutes.
[NOTERetain a portion of the supernatant for the
Chromatographic purity and
Limit of methamphetamine hydrochloride tests.
] Transfer 10.0 mL of the supernatant to a 100-mL volumetric flask, dilute with
Mobile phase to volume, and mix.
Procedure
Proceed as directed for
Procedure in the
Assay under
Selegiline Hydrochloride. Calculate the quantity, in mg, of C
13H
17N·HCl in the portion of Tablets taken by the formula:
500C(rU / rS),
in which the terms are as defined therein.