USP Reference standards á11ñ
USP Perphenazine RS.
NOTEThroughout the following procedures,protect test or assay specimens,the USP Reference Standard,and solutions containing them,by conducting the procedures without delay,under subdued light,or using low-actinic glassware.
Identification
Add 10mLof water to a volume of Syrup,equivalent to about 4mg of perphenazine,render alkaline by dropwise addition of sodium hydroxide to a pHof 11to 12,and extract with four 5-mLportions of chloroform,combining the extracts through a bed of anhydrous sodium sulfate in a funnel into a beaker.Evaporate the extracts on a steam bath nearly to dryness,and dissolve the residue in 4mLof methanol:the solution so obtained responds to the
Identificationtest under
Perphenazine Injection.
Assay
Acid-alcohol solutionand Palladium chloride solution
Prepare as directed in the
Assayunder
Perphenazine Injection.
Standard preparation
Dissolve an accurately weighed quantity of
USP Perphenazine RSin
Acid-alcohol solutionto obtain a solution having a known concentration of about 160µg per mL.
Assay preparation
Transfer an accurately measured volume of Syrup,equivalent to about 6mg of perphenazine,to a 25-mLvolumetric flask,dilute with water to volume,and mix.Transfer 10mLto a 125-mLseparator,add 25mLof water,adjust with ammonium hydroxide to a pHof 10to 11,and extract with four 20-mLportions of chloroform,filtering the extracts through anhydrous sodium sulfate.Evaporate the combined extracts on a steam bath with the aid of a stream of nitrogen to about 5mL.Complete the evaporation without application of heat,and dissolve the residue in 15.0mLof Acid-alcohol solution,filtering if necessary.
Procedure
Mix 10.0mLeach of the
Assay preparationand the
Standard preparationwith 15.0mLof
Palladium chloride solution,filter if necessary,and concomitantly determine the absorbances of these solutions,against a reagent blank,in 1-cm cells at the wavelength of maximum absorbance at about 480nm,with a suitable spectrophotometer.Calculate the quantity,in mg,of perphenazine (C
21H
26ClN
3OS)in each mLof the Syrup taken by the formula:
0.0375(C/V)(AU/AS),
in which
Cis the concentration,in µg per mL,of
USP Perphenazine RSin the
Standard preparation;Vis the volume,in mL,of Syrup taken;and
AUand
ASare the absorbances of the solutions from the
Assay preparationand the
Standard preparation,respectively.