Disintegration 
701
—
Place 1 tablet in each of the 6 tubes of the basket and, if the tablets have a soluble external coating, immerse the basket in water at room temperature for 5 minutes. Then add a disk to each tube, and operate the apparatus, using
simulated gastric fluid TS maintained at 37 ± 2
as the immersion fluid. After 30 minutes of operation in
simulated gastric fluid TS, lift the basket from the fluid, and observe the tablets. If the tablets have not disintegrated completely, substitute simulated intestinal fluid TS maintained at 37 ± 2
as the immersion fluid. Continue the test for a total period of time, including previous exposure to water and simulated gastric fluid TS, of 1 hour and 30 minutes. Lift the basket from the fluid, and observe the tablets: all of the tablets have disintegrated completely. If 1 or 2 tablets fail to disintegrate completely, repeat the test on 12 additional tablets: not less than 16 of the total 18 tablets tested disintegrate completely.
Assay—
Ion-pair solution—
Dissolve about 6.8 g of monobasic potassium phosphate and about 2.16 g of sodium 1-octanesulfonate in 1000 mL of water, and mix. Adjust with phosphoric acid to a pH of 3.0, and filter.
Mobile phase—
Prepare a filtered and degassed mixture of
Ion-pair solution and methanol (60:40). Make adjustments if necessary (see
System Suitability under
Chromatography 621).
Standard preparation—
Dissolve an accurately weighed quantity of
USP Phenelzine Sulfate RS in
Mobile phase, and dilute quantitatively, and stepwise if necessary, with
Mobile phase to obtain a solution having a known concentration of about 258 µg per mL.
Assay preparation—
Transfer not less than 20 Tablets to a suitable container, add about 300 mL of Mobile phase, and homogenize until dissolved. Transfer this solution to a 500-mL volumetric flask, dilute with Mobile phase to volume, mix, centrifuge, and filter, discarding the first 5 mL of the filtrate. Transfer a portion of the filtrate, equivalent to about 12.9 mg of phenelzine sulfate, to a 50-mL volumetric flask, dilute with Mobile phase to volume, and mix.
Chromatographic system
(see
Chromatography 621)—The liquid chromatograph is equipped with a 210-nm detector and a 3.9-mm × 15-cm column that contains packing L1. The flow rate is about 1.0 mL per minute. Chromatograph the
Standard preparation, and record the peak responses as directed for
Procedure: the column efficiency is not less than 3000 theoretical plates, the tailing factor is not more than 2.0, and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure—
Separately inject equal volumes (about 20 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 µg, of phenelzine (C
8H
12N
2) in the
Assay preparation by the formula:
(136.20 / 234.27)(50C)(rU / rS),
in which 136.20 and 234.27 are the molecular weights of phenelzine and phenelzine sulfate, respectively,
C is the concentration, in µg per mL, of
USP Phenelzine Sulfate RS in the
Standard preparation, and
rU and
rS are the peak responses obtained from the
Assay preparation and the
Standard preparation, respectively.
