Phenelzine Sulfate

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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C₈H₁₂N₂·H₂SO₄ 234.27

Hydrazine, (2-phenylethyl)-, sulfate (1:1);

Phenethylhydrazine sulfate (1:1) CAS RN^®: 156-51-4; UNII: 2681D7P965.

1 DEFINITION

Phenelzine Sulfate contains NLT 98.0% and NMT 102.0% of phenelzine sulfate (C₈H₁₂N₂·H₂SO₄), calculated on the dried basis.

2 IDENTIFICATION

A. SPECTROSCOPIC IDENTIFICATION TESTS (197), Infrared Spectroscopy: 197K

B.

Sample: Dissolve 100 mg of Phenelzine Sulfate in 5 mL of water, render the solution alkaline with 1 N sodium hydroxide, and add 1 mL of alkaline cupric tartrate TS.

Acceptance criteria: A red to yellow-red precipitate is formed

C. IDENTIFICATION TESTS-GENERAL (191), Chemical Identification Tests, Sulfate

Sample solution: 1 in 10 solution of Phenelzine Sulfate in water

Acceptance criteria: Meets the requirements

3 ASSAY

Change to read:

3.1 PROCEDURE

Solution A: About 6.8 g/L of monobasic potassium phosphate and about 2.16 g/L of sodium 1-octanesulfonate in water. Adjust with

phosphoric acid to a pH of 3.0.

Mobile phase: Methanol and Solution A (40:60)

Standard solution: 0.26 (IRA 1-May-2023) mg/mL of USP Phenelzine Sulfate RS in Mobile phase

Sample solution: 0.26 mg/mL of Phenelzine Sulfate in Mobile phase (IRA 1-May-2023)

3.2 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 210 nm

Column: 3.9-mm x 15-cm; 5-µm (IRA 1-May-2023) Packing L1

Flow rate: 1 mL/min

Injection volume: 20 µL

Run time: NLT 2 times the retention time of phenelzine (IRA 1-May-2023)

3.3 System suitability

Sample: Standard solution

Suitability requirements

(IRA 1-May-2023)

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0%

3.4 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of phenelzine sulfate (C₈H₁₂N₂·H₂SO₄) in the portion of Phenelzine Sulfate taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of phenelzine from the Sample solution

r_S = peak response of phenelzine from the Standard solution

C_S = concentration of USP Phenelzine Sulfate RS in the Standard solution (mg/mL)

C_U = concentration of Phenelzine Sulfate in the Sample solution (mg/mL)

Acceptance criteria: 98.0%-102.0% on the dried basis

4 IMPURITIES

4.1 ORDINARY IMPURITIES (466)

Standard solution: Methanol and water (50:50)

Sample solution: Methanol and water (50:50)

Eluent: Acetone

[NOTE-Prewash the plate with Eluent, and dry.]

Visualization: 1

Acceptance criteria: Meets the requirements

Change to read:

4.2 LIMIT OF HYDRAZINE

Solution A: 1% monobasic ammonium phosphate in water

Mobile phase: Methanol and Solution A (75:25)

Standard stock solution A: 0.1 mg/mL hydrazine prepared as follows. Dissolve about 42.0 mg of hydrazine sulfate, equivalent to about 10 mg of hydrazine, in water in a 100-mL volumetric flask, and sonicate for about 5 min. Dilute with methanol to volume.

Standard stock solution B: 5.0 µg/mL of hydrazine from Standard stock solution A in methanol

System suitability solution: 0.125 µg/mL of hydrazine and 0.129 mg/mL of USP Phenelzine Sulfate RS prepared as follows. Transfer about 25.8 mg of USP Phenelzine Sulfate RS to a 200-mL volumetric flask, add 50 mL of methanol, and sonicate to dissolve. Add 5 mL of Standard stock solution B and 0.7 mL of ammonium hydroxide and shake. Add 0.5 mL of salicylaldehyde and shake by mechanical means for about 5 min. Dilute with methanol to volume, sonicate for about 2 min, and mix.

Standard solution: 0.125 µg/mL of hydrazine prepared as follows. Transfer 5.0 mL of Standard stock solution B to a 200-mL volumetric flask, add 50 mL of methanol and 0.7 mL of ammonium hydroxide, and shake. Add 0.5 mL of salicylaldehyde and shake by mechanical means for about 5 min. Dilute with methanol to volume, sonicate for about 2 min, and mix. (IRA 1-May-2023)

Sample solution: 0.129 mg/mL of Phenelzine Sulfate prepared as follows. (IRA 1-May-2023) Transfer about 25.8 mg of Phenelzine Sulfate to a 200-mL volumetric flask, add about 50 mL of methanol, and sonicate to dissolve. Add 0.7 mL of ammonium hydroxide and shake. Add 0.5 mL of salicylaldehyde and shake by mechanical means for about 5 min. Dilute with methanol to volume, sonicate for about 2 min, and mix.

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 340 nm

Column: 4.6-mm × 25-cm; 5-µm packing L1

Flow rate: 1.5 mL/min (IRA 1-May-2023)

Injection volume: 50 µL

Run time: NLT 1.4 times the retention time of hydrazine derivative (salazine) (IRA 1-May-2023)

System suitability

Samples: System suitability solution (IRA 1-May-2023) and Standard solution

[NOTE-The relative retention times for salicylaldehyde, phenelzine (IRA 1-May-2023) derivative, and hydrazine derivative (salazine) (IRA 1-May-2023) are about 0.16, 0.56. (IRA 1-May-2023) and 1.0, respectively.]

Suitability requirements

Resolution: NLT 1.25 between phenelzine derivative (IRA 1-May-2023) and hydrazine derivative (salazine), System suitability solution (IRA 1-May-2023)

Relative standard deviation: NMT 7%, Standard solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of hydrazine (N₂H₄) (IRA 1-May-2023) in the portion of Phenelzine Sulfate taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of hydrazine derivative (salazine) (IRA 1-May-2023) from the Sample solution

r_S = peak response of hydrazine derivative (salazine) (IRA 1-May-2023) from the Standard solution

C_S = concentration of hydrazine (IRA 1-May-2023) in the Standard solution (mg/mL)

C_U = concentration of Phenelzine Sulfate in the Sample solution (mg/mL)

Acceptance criteria: NMT 0.1%

5 SPECIFIC TESTS

5.1 LOSS ON DRYING (731)

Analysis: Dry at 80° for 2 h over silica gel, at a pressure not exceeding 5 mm of mercury.

Acceptance criteria: NMT 1.0%

5.2 PH (791)

Sample solution: 10 mg/mL of Phenelzine Sulfate in water

Acceptance criteria: 1.4-1.9

5.3 MELTING RANGE OR TEMPERATURE (741)

Acceptance criteria: 164°-168°

6 ADDITIONAL REQUIREMENTS

6.1 PACKAGING AND STORAGE

Preserve in tight containers. Protect from heat and light.

6.2 USP REFERENCE STANDARDS (11)

USP Phenelzine Sulfate RS