Pregna-1,4-diene-3,20-dione, 16,21-bis(acetyloxy)-9-fluoro-11,17-dihydroxy-, (11,16)-.
9-Fluoro-11,16,17,21-tetrahydroxypregna-1,4-diene-3,20-dione 16,21-diacetate [67-78-7].
» Triamcinolone Diacetate contains not less than 97.0 percent and not more than 103.0 percent of C25H31FO8, calculated on the anhydrous basis.
Packaging and storage Preserve in well-closed containers.
B: Ultraviolet Absorption 197U
Solution: 20 µg per mL.
Medium: dehydrated alcohol.
Absorptivities at 238 nm, calculated on the anhydrous basis, do not differ by more than 3.0%.
Specific rotation 781S: between +39 and +45.
Test solution: 5 mg per mL, in dimethylformamide.
Water, Method I 921: not more than 6.0%.
Residue on ignition 281: not more than 0.5%.
Heavy metals, Method II 231: 0.0025%.
0.005 M Monobasic sodium phosphate solution Dissolve monobasic sodium phosphate in water to obtain a solution containing 690 µg per mL.
Mobile phase Prepare a mixture of 0.005 M 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 Suitability under Chromatography 621).
Standard preparation Dissolve an accurately weighed quantity of USP Triamcinolone Diacetate RS in Mobile phase, and dilute quantitatively with Mobile phase to obtain a solution having a known concentration of about 40 µg per mL.
Assay preparation Transfer about 50 mg of Triamcinolone Diacetate, accurately weighed, to a 50-mL volumetric flask, dissolve in Mobile phase, dilute with Mobile phase to volume, and mix. Pipet 2 mL of this solution into a second 50-mL volumetric flask, dilute with Mobile phase to volume, and mix.
System suitability preparation Dissolve suitable quantities of USP Triamcinolone Diacetate RS and propylparaben in Mobile phase to obtain a solution containing about 40 µg per mL and 15 µg per mL, respectively.
Chromatographic system (see Chromatography 621)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 1 mL per minute. Chromatograph the System suitability preparation, and record the peak responses as directed for Procedure: the relative retention times are 1.0 for triamcinolone diacetate and about 1.1 for 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 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, and measure the area responses for the major peaks. Calculate the quantity, in mg, of C25H31FO8 in the portion of Triamcinolone Diacetate taken by the formula:
1.25C(rU / rS)in which C is the concentration, in µg per mL, of USP Triamcinolone Diacetate RS in the Standard preparation, and rU and rS are the peak area responses obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information Please check for your question in the FAQs before contacting USP.Chromatographic Column
USP32NF27 Page 3785Pharmacopeial Forum: Volume No. 32(4) Page 1120
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.