Phenethylhydrazine sulfate (1:1). [156-51-4].
»Phenelzine Sulfate contains not less than 98.0percent and not more than 102.0percent of C8H12N2·H2SO4,calculated on the dried basis.
Packaging and storage Preserve in tight containers,protected from heat and light.
A: Infrared Absorption á197Kñ.
B: Dissolve 100mg in 5mLof water,render the solution alkaline with 1Nsodium hydroxide,and add 1mLof alkaline cupric tartrate TS:a red to yellow-red precipitate is formed.
C: Asolution (1in 10)meets the requirements of the tests for Sulfate á191ñ.
Melting range á741ñ: between 164and 168.
pHá791ñ: between 1.4and 1.9,in a solution (1in 100).
Loss on drying á731ñ Dry it at a pressure not exceeding 5mm of mercury over silica gel at 80for 2hours:it loses not more than 1.0%of its weight.
Heavy metals,Method Iá231ñ: 0.002%.
Limit of hydrazine
Mobile phase Prepare a filtered and degassed mixture of methanol and 1%monobasic ammonium phosphate solution (75:25).Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Standard solution Transfer an accurately weighed quantity of about 42.0mg of hydrazine sulfate,equivalent to about 10mg of hydrazine,to a 100-mLvolumetric flask.Dissolve in water,sonicate for about 5minutes,dilute with methanol to volume,and mix.Dilute an accurately measured volume of this solution quantitatively and stepwise with methanol to obtain a solution having a known concentration of 5.0µg of hydrazine per mL.Transfer 5.0mLof this solution to a 200-mLvolumetric flask,add 50mLof methanol and 0.7mLof ammonium hydroxide,and shake to mix.Add 0.5mLof salicylaldehyde,shake by mechanical means for about 5minutes,dilute with methanol to volume,sonicate for about 2minutes,and mix.
Test solution Transfer about 25.8mg of Phenelzine Sulfate,accurately weighed,to a 200-mLvolumetric flask,dissolve in about 50mLof methanol,and sonicate.Add 0.7mLof ammonium hydroxide,shake to mix,add 0.5mLof salicylaldehyde,shake by mechanical means for about 5minutes,dilute with methanol to volume,sonicate for about 2minutes,and mix.
Chromatographic system (see Chromatography á621ñ) The liquid chromatograph is equipped with a 340-nm detector and a 4.6-mm ×25-cm column that contains 5-µm packing L1.Chromatograph the Standard solution,and record the peak areas as directed for Procedure:the relative retention times for salicylaldehyde,phenelzine sulfate derivative,and hydrazine sulfate derivative are about 0.21,0.47,and 1.0,respectively;the column efficiency determined from the analyte peak is not less than 4500theoretical plates;the resolution,R,between phenelzine and salazine (derivatized hydrazine)is not less than 1.25;and the relative standard deviation for replicate injections is not more than 7%.
Procedure Separately inject equal volumes (about 50µL)of the Standard solutionand the Test solutioninto the chromatograph,record the chromatograms,and measure the peak areas for salazine (derivatized hydrazine).Calculate the percentage of hydrazine in the portion of Phenelzine Sulfate taken by the formula:
20(C/W)(rU/rS),in which Cis the concentration,in µg per mL,of hydrazine base in the Standard solution;Wis the weight,in mg,of Phenelzine Sulfate taken to prepare the Test solution;and rUand rSare the salazine peak areas obtained from the Test solutionand the Standard solution,respectively:not more than 0.1%is found.
Ordinary impurities á466ñ
Test solution: a mixture of methanol and water (1:1).
Standard solution: a mixture of methanol and water (1:1).
Eluant: acetone.[NOTEPrewash the plate with Eluant,and dry.]
Organic volatile impurities,Method Iá467ñ: meets the requirements.
Ion-pair solution,Mobile phase,Standard preparation,andChromatographic system Proceed as directed in the Assayunder Phenelzine Sulfate Tablets.
Assay preparation Transfer about 26mg of Phenelzine Sulfate,accurately weighed,to a 100-mLvolumetric flask,dissolve in and dilute with Mobile phaseto volume,and mix.
Procedure Separately inject equal volumes (about 20µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the peak responses.Calculate the quantity,in mg,of C8H12N2·H2SO4in the portion of Phenelzine Sulfate taken by the formula:
100C(rU/rS),in which Cis the concentration,in mg per mL,of USP Phenelzine Sulfate RSin the Standard preparation;and rUand rSare the peak responses obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information Staff Liaison:Ravi Ravichandran,Ph.D.,Senior Scientist
Expert Committee:(PA3)Pharmaceutical Analysis 3
USP28NF23Page 1527Pharmacopeial Forum:Volume No.27(1)Page 1814