Assay
0.005M Monobasic sodium phosphate solution
Dissolve monobasic sodium phosphate in water to obtain a solution containing 690µg per mL.
Mobile phase
Prepare a mixture of
0.005M Monobasic sodium phosphate solution,acetonitrile,and tetrahydrofuran (62:37:1),filter through a 0.45-µm solvent-resistant filter,and degas.Make adjustments if necessary (see
System Suitabilityunder
Chromatography á621ñ).
Standard preparation
Dissolve an accurately weighed quantity of
USP Triamcinolone Diacetate RSin
Mobile phase,and dilute quantitatively with
Mobile phaseto obtain a solution having a known concentration of about 40µg per mL.
Assay preparation
Transfer about 50mg of Triamcinolone Diacetate,accurately weighed,to a 50-mLvolumetric flask,dissolve in Mobile phase,dilute with Mobile phaseto volume,and mix.Pipet 2mLof this solution into a second 50-mLvolumetric flask,dilute with Mobile phaseto volume,and mix.
System suitability preparation
Dissolve suitable quantities of
USP Triamcinolone Diacetate RSand propylparaben in
Mobile phaseto obtain a solution containing about 40µg per mLand 15µg per mL,respectively.
Chromatographic system
(see
Chromatography á621ñ)The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm ×30-cm column that contains packing L1.The flow rate is about 1mLper minute.Chromatograph the
System suitability preparation,and record the peak responses as directed for
Procedure:the relative retention times are 1.0for triamcinolone diacetate and about 1.1for propylparaben,the resolution,
R,between the triamcinolone diacetate and propylparaben peaks is not less than 1.7,and the tailing factor,
T,for the analyte peak is not more than 1.5.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 10µL)of the
Standard preparationand the
Assay preparationinto the chromatograph,and measure the area responses for the major peaks.Calculate the quantity,in mg,of C
25H
31FO
8in the portion of Triamcinolone Diacetate taken by the formula:
1.25C(rU/rS),
in which
Cis the concentration,in µg per mL,of
USP Triamcinolone Diacetate RSin the
Standard preparation,and
rUand
rSare the peak area responses obtained from the
Assay preparationand the
Standard preparation,respectively.