Phenylephrine Hydrochloride Injection
»Phenylephrine Hydrochloride Injection is a sterile solution of Phenylephrine Hydrochloride in Water for Injection.It contains not less than 90.0percent and not more than 115.0percent of the labeled amount of C9H13NO2·HCl.
Packaging and storage— Preserve in single-dose or multiple-dose containers,preferably of Type Iglass,protected from light.
Identification— Concentrate or dilute,if necessary,a suitable volume of Injection to a concentration of about 10mg per mL.Apply 2µLof this solution and of a Standard solution of USP Phenylephrine Hydrochloride RS,containing about 10mg per mL,at points about 2.5cm from the bottom edge of a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel.Dry the spots in a current of warm air,and develop the chromatogram in a suitable chromatographic chamber with a mixture of methanol,water,and ammonium hydroxide (72:25:3)until the solvent front has moved about 12cm.Dry the plate in warm air,and spray it with alcoholic potassium hydroxide TS.Dry at 60for 15minutes,and spray the plate with p-nitroaniline TS:the reddish orange spot obtained from the test solution corresponds in color,size,and intensity to that obtained from the Standard solution.
Bacterial endotoxins á85ñ— It contains not more than 25.0USP Endotoxin Units per mg of phenylephrine hydrochloride.
pHá791ñ: between 3.0and 6.5.
Other requirements— It meets the requirements under Injections á1ñ.
Assay—
Mobile phase— Prepare and filter a mixture of methanol and water (1:1)containing 1.1g of sodium 1-octanesulfonate per liter,adjusted with 3Mphosphoric acid to a pHof 3.0.Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Dilution solvent— Prepare a mixture of methanol and water (1:1),adjusted with 3Mphosphoric acid to a pHof 3.0.
System suitability solution— Dissolve about 50mg each of USP Phenylephrine Hydrochloride RSand USP Epinephrine Bitartrate RSin 5mLof water,dilute with Dilution solventto 25.0mL,and mix.Further dilute 5.0mLof the resulting solution with Dilution solventto 25.0mL,and mix to obtain a solution having a concentration of about 0.4mg of phenylephrine hydrochloride and 0.4mg of epinephrine bitartrate per mL.
Standard preparation— Dissolve about 50mg of USP Phenylephrine Hydrochloride RS,accurately weighed,in 10mLof water,dilute with Dilution solventto 25.0mL,and mix.Further dilute 5.0mLof the resulting solution with Dilution solvent to 25.0mL,and mix to obtain a solution having a known concentration of about 0.4mg per mL.
Assay preparation— Transfer an accurately measured volume of Injection,equivalent to about 10mg of phenylephrine hydrochloride,to a 25-mLvolumetric flask.Dilute with Dilution solventto volume,and mix.
Chromatographic system (see Chromatography á621ñ)—The liquid chromatograph is equipped with a 280-nm detector and a 4.6-mm ×25-cm column that contains packing L1.The flow rate is about 1mLper minute.Chromatograph the System suitability solution,and record the responses for the major peaks:the resolution,R,between epinephrine and phenylephrine is not less than 1.0.Chromatograph replicate injections of the Standard preparation,and record the peak responses as directed for Procedure:the relative standard deviation is not more than 2.0%.
Procedure— Separately inject equal volumes (about 20µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the quantity,in mg,of C9H13NO2·HCl in each mLof the Injection taken by the formula:
(25C/V)(rU/rS),
in which Cis the concentration,in mg per mL,of USP Phenylephrine Hydrochloride RSin the Standard preparation,Vis the volume,in mL,of Injection taken,and rUand rSare the peak responses obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Daniel K.Bempong,Ph.D.,Scientist
Expert Committee:(PA2)Pharmaceutical Analysis 2
USP28–NF23Page 1541
Phone Number:1-301-816-8143