Tranylcypromine Tablets
DEFINITION
Tranylcypromine Tablets contain an amount of tranylcypromine sulfate equivalent to NLT 90.0% and NMT 110.0% of the labeled amount of tranylcypromine (C9H11N).
IDENTIFICATION
•  The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
•  Procedure
Buffer:  Transfer 3.4 g of monobasic ammonium phosphate into a 1-L volumetric flask containing about 900 mL of water. Adjust the pH of the solution with phosphoric acid to 2.2 ± 0.1. Dilute with water to volume, and mix well.
Mobile phase:  Methanol and Buffer (3:7)
0.05 N sulfuric acid:  Cautiously add 1.3 mL of sulfuric acid to 100 mL of water, cool to room temperature, and dilute to 1000 mL.
Diluent:  Methanol, water, and 0.05 N sulfuric acid (1:3:1)
Standard stock solution:  Dissolve USP Tranylcypromine Sulfate RS in a 50:50 mixture of methanol and 0.05 N sulfuric acid (about 60% of the final volume), using a sonicator, and dilute with Diluent to obtain a 0.4 mg/mL solution of USP Tranylcypromine Sulfate RS.
Standard solution:  0.04 mg/mL of USP Tranylcypromine Sulfate RS in Diluent, from the Standard stock solution
Sample stock solution:  Transfer a number of Tablets of tranylcypromine, equivalent to about 100 mg based on the label claim, to a 200-mL volumetric flask; add 60 mL of 0.05 N sulfuric acid; and sonicate for 10 min with intermittent shaking. Add 60 mL of methanol, and sonicate for 10 min with intermittent shaking. Shake by mechanical means for 30 min, dilute with Diluent to volume, and mix to obtain a solution containing the equivalent of 0.5 mg/mL of tranylcypromine. Centrifuge a portion of the solution, and pass the supernatant through a filter of 0.45-µm pore size, discarding the first 2 mL.
Sample solution:  0.03 mg/mL of tranylcypromine in Diluent, from the Sample stock solution filtrate
Chromatographic system 
Mode:  LC
Detector:  UV 220 nm
Column:  4.6-mm × 25-cm; 4-µm packing L11
Column temperature:  30
Flow rate:  1 mL/min
Injection size:  20 µL
System suitability 
Sample:  Standard solution
Suitability requirements 
Tailing factor:  NMT 2.0
Relative standard deviation:  NMT 2.0%
Analysis 
Samples:  Standard solution and Sample solution
Calculate the percentage of C9H11N in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × (M × Mr1/Mr2) × 100
rU== peak response from the Sample solution
rS== peak response from the Standard solution
CS== concentration of USP Tranylcypromine Sulfate RS in the Standard solution (mg/mL)
CU== concentration of tranylcypromine in the Sample solution (mg/mL)
M== number of moles of tranylcypromine/mole of tranylcypromine sulfate, 2
Mr1== molecular weight of tranylcypromine, 133.19
Mr2== molecular weight of tranylcypromine sulfate, 364.46
Acceptance criteria:  90.0%–110.0%
PERFORMANCE TESTS
•  Dissolution 711
Medium:  0.1 N hydrochloric acid; 500 mL, deaerated
Apparatus 1:  100 rpm
Time:  45 min
Buffer:  Transfer 6.94 g of sodium perchlorate monohydrate to a 1000-mL volumetric flask containing 900 mL of water, and mix until dissolved. Adjust with perchloric acid to a pH of 2.50, and dilute with water to volume.
Mobile phase:  Acetonitrile and Buffer (3:17)
Standard stock solution:  0.54 mg/mL of USP Tranylcypromine Sulfate RS in water. [Note—Sonicate as needed. ]
Standard solution:  0.027 mg/mL of USP Tranylcypromine Sulfate RS in Medium, from the Standard stock solution
Sample solution:  Pass a portion of the solution under test through a suitable filter of 0.45-µm pore size.
Chromatographic system 
Mode:  LC
Detector:  UV 220 nm
Column:  3.9-mm × 15-cm; 5-µm packing L1
Column temperature:  35
Flow rate:  1 mL/min
Injection size:  50 µL
System suitability 
Sample:  Standard solution
Suitability requirements 
Tailing factor:  NMT 2.0
Column efficiency:  NLT 2000
Capacity factor:  NLT 2.0
Relative standard deviation:  NMT 2.0%
Analysis 
Samples:  Standard solution and Sample solution
Calculate the quantity dissolved as a percentage of the labeled amount of tranylcypromine:
Result = (rU/rS) × (CS × V) × (M × Mr1/Mr2) × (100/L)
rU== peak response from the Sample solution
rS== peak response from the Standard solution
CS== concentration of USP Tranylcypromine Sulfate RS in the Standard solution (mg/mL)
V== volume of Medium, 500 mL
M== number of moles of tranylcypromine/mole of tranylcypromine sulfate, 2
Mr1== molecular weight of tranylcypromine, 133.19
Mr2== molecular weight of tranylcypromine sulfate, 364.46
L== label claim (mg/Tablet)
Tolerances:  NLT 75% (Q) of the labeled amount of tranylcypromine is dissolved.
•  Uniformity of Dosage Units 905: Meet the requirements
IMPURITIES
Organic Impurities 
•  Procedure
Buffer, 0.05 N sulfuric acid, and Diluent:  Prepare as directed in the Assay.
Solution A:  Methanol and Buffer (3:17)
Solution B:  Methanol and Buffer (3:7)
Mobile phase:  See the gradient table below.
Time
(min)
Solution A
(%)
Solution B
(%)
0 100 0
20 100 0
25 0 100
37 0 100
39 100 0
45 100 0
Standard stock solution:  70 µg/mL of USP Tranylcypromine Sulfate RS and 280 µg/mL of USP Tranylcypromine Related Compound A RS in Diluent. [Note—Sonicate as needed. ]
Standard solution:  Transfer 2 mL of Standard stock solution to a 200-mL volumetric flask, add 60 mL each of 0.05 N sulfuric acid and methanol, and dilute with Diluent to obtain a solution containing 0.7 µg/mL of USP Tranylcypromine RS and 2.8 µg/mL of USP Tranylcypromine Related Compound A RS.
Sample solution:  Use the Sample stock solution in the Assay.
Chromatographic system  
Mode:  LC
Detector:  UV 220 nm
Column:  4.6-mm × 15-cm; 3-µm packing L1
Column temperature:  35
Flow rate:  1.2 mL/min
Injection size:  25 µL
System suitability 
Sample:  Standard solution
Suitability requirements 
Resolution:  NLT 2.0 between tranylcypromine and tranylcypromine related compound A
Tailing factor:  NMT 2.0
Relative standard deviation:  NMT 6.0%
Analysis 
Samples:   Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × (M × Mr1/Mr2) × 100
rU== peak response of the impurity from the Sample solution
rS== peak response from the Standard solution
CS== concentration of USP Tranylcypromine Sulfate RS in the Standard solution (mg/mL)
CU== concentration of tranylcypromine in the Sample solution (mg/mL)
M== number of moles of tranylcypromine/mole of tranylcypromine sulfate, 2
Mr1== molecular weight of tranylcypromine, 133.19
Mr2== molecular weight of tranylcypromine sulfate, 364.46
Acceptance criteria 
Individual impurities:  NMT 0.2%
Total impurities:  NMT 1.2%
ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Preserve in well-closed containers, and store at controlled room temperature.
•  USP Reference Standards 11
USP Tranylcypromine Sulfate RS Click to View Structure
USP Tranylcypromine Related Compound A RS
(±)-cis-2-Phenylcyclopropanamine hydrochloride; cis-tranylcypromine hydrochloride.
    C9H11N·HCl        169.65
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USP35–NF30 Page 4913
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