Identification
A:
Infrared Absorption á197Kñ.
C:
Heat 0.5mLof a saturated solution of chromium trioxide in sulfuric acid in a water bath for 5minutes:the solution wets the sides of the tube readily and there is no greasiness.Add 2or 3mg of Flurbiprofen and heat in a water bath for 5minutes:the solution does not wet the sides of the tube and does not pour easily.
Related compounds
Diluent
Prepare a mixture of water and acetonitrile (11:9).
Mobile phase
Prepare a filtered and degassed mixture of water,acetonitrile,and glacial acetic acid (12:7:1).Make adjustments if necessary (see
System Suitabilityunder
Chromatography á621ñ).
System suitability solution
Pipet 2.0mLof
Standard stock solutioninto a 10-mLvolumetric flask,add about 20mg of
USP Flurbiprofen RS,dilute with
Diluentto volume,and mix.
Standard solution
Transfer 2.0mLofStandard stock solutionto a 10.0-mLvolumetric flask,dilute withDiluentto volume,and mix.
Test solution
Prepare a solution of Flurbiprofen inDiluentcontaining 2.0mg per mL.
Chromatographic system(see Chromatography á621ñ)
The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm ×15-cm column that contains 4-µm packing L1.The flow rate is about 1mLper minute.Chromatograph the
System suitability solution,and record the peak responses as directed for
Procedure:the relative retention times are about 0.9for flurbiprofen related compound Aand 1.0for flurbiprofen;and the relative standard deviation for replicate injections is not more than 1.0%.
Procedure
Separately inject equal volumes (about 20µL)of the
Standard solutionand the
Test solutioninto the chromatograph,record the chromatograms,and measure the areas for the major peaks.Calculate the percentage of flurbiprofen related compound Ain the portion of Flurbiprofen taken by the formula:
100(CS/CU)(rU/rS),
in which
CSis the concentration,in µg per mL,of
USP Flurbiprofen Related Compound A RSin the
Standard solution;CUis the concentration,in µg per mL,of Flurbiprofen in the
Test solution;and
rUand
rSare the peak responses for flurbiprofen related compound Aobtained from the
Test solutionand the
Standard solution,respectively:not more than 0.5%of flurbiprofen related compound Ais found.Calculate the percentage of each impurity in the portion of Flurbiprofen taken by the formula:
100(ri/rs),
in which
riis the peak response for each impurity obtained from the
Test solution;and
rsis the sum of the responses of all the peaks obtained from the
Test solution:the sum of all impurities is not more than 1.0%.